Exposure of black soldier fly larvae to microplastics of various sizes and shapes: Ingestion and egestion dynamics and kinetics

Our Library never stops expanding. What are the most recent contributions to LabRulezGCMS Library in the week of 5th January 2026? Check out new documents from the field of the gas phase, especially GC and GC/MS techniques!<blockquote>👉 <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library">SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT GCMS AND RELATED TECHNIQUES</a></blockquote><blockquote>👉 Need info about different analytical techniques? Peek into <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library">LabRulezLCMS</a> or <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library">LabRulezICPMS</a> libraries.</blockquote>This week we bring you application notes by Agilent Technologies, EST Analytical and Shimadzu!<h3>1. Agilent Technologies: Ultrasensitive and Powerful GC/MS/MS for Analyzing Multipesticides in Black Pepper and Dried Tea</h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_gcms_ms_black_pepper_5994_8783en_agilent_4b1cc85920.pdf">Full PDF for download</a></li></ul>Pesticides play a vital role in safeguarding crops and are indispensable in most farming settings to secure high yields.1 Regulatory authorities, including the Codex Alimentarius and the European Commission mandate the monitoring and reporting of pesticide residues found in or on food product.2 The analysis of pesticides in food faces several major challenges, such as the variety of pesticide classes, the complexity of different food matrices, the effects of these matrices, and the detection of target analytes at low&nbsp;concentrations.3&nbsp;According to the EU's SANTE/11312/2021 guidelines, black pepper and dried tea are considered among the difficult or unique commodity matrices for multiresidue pesticide analysis.4 The matrix interferences are complex and diverse, including carbohydrates, fats, piperine, terpenoids (for black pepper)5 , and caffeine (in dried tea). "For dried tea, matrix interferences include polyphenols, pigments, polysaccharides, alkaloids, free amino acids, high caffeine levels, and&nbsp;catechins".6&nbsp;In addition to affecting the analyte signals, matrix interferences can cause the system to become contaminated more quickly. This leads to a rapid decline in the sensitivity of the analytical instrument, and necessitates frequent maintenance, significantly reducing laboratory productivity. These are the current challenges faced by laboratories when analyzing pesticides in difficult and complex matrices.&nbsp;To overcome these challenges, Agilent offers a robust solution with its backflush and JetClean self-cleaning ion source technologies integrated into the high-sensitivity 7010B GC/TQ system. Backflush technology prevents high‑boiling contaminants from reaching the detector, reducing the need for frequent maintenance and extending column life.7 This ensures consistent performance and minimizes downtime, thereby enhancing laboratory productivity.&nbsp;With JetClean technology, your lab can significantly increase instrument uptime, as fewer manual cleanings are needed, maximizing productivity. This technology helps maintain data quality by ensuring a clean ion source, which guarantees run-to-run reproducibility. Additionally, JetClean enhances operator convenience through automated cleaning, requiring virtually no user intervention.8 Combined with the ultrasensitivity of the 7010B GC/TQ system, these technologies provide precise and reliable analysis of pesticides in complex matrices such as black pepper and dried tea. Agilent’s comprehensive approach effectively mitigates matrix interferences, preserves instrument sensitivity, and significantly boosts overall efficiency in pesticide analysis.This application note describes a detailed approach for the simultaneous quantification of 284 pesticides in black pepper and dried tea samples. Agilent's solution for complex matrices demonstrates the sensitivity of the 8890 GC/7010B GC/TQ and confirms its robustness when using backflush and JetClean techniques.&nbsp;<h4>Experimental and chemicals</h4><h5>GC/TQ parameters&nbsp;</h5>The <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=8890">8890 GC</a>/<a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=7010B">7010B GC/TQ systems</a> (Figure 1) were optimized for wide calibration range performance. Equipped with an Agilent <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=7693A">7693A automatic liquid sampler </a>and a 150-position tray, the GC operated in temperature‑programmed splitless injection mode with a multimode inlet. Detailed instrument parameters can be found in Table 1. Data acquisition was in dynamic MRM (dMRM) mode, enabling analysis of 284 pesticides with 1233 MRM transitions and up to 74 concurrent MRMs (see Figure 2). Retention time was synchronized with the Agilent Pesticides and Environmental Pollutants (P&amp;EP) 4.0 MRM Database, streamlining method&nbsp;setup.<h4>Conclusion&nbsp;</h4>This application note describes an approach for the analysis of multipesticides in complex and distinctive matrices, including black pepper and dried tea using the Agilent 8890 GC/7010B GC/TQ. The comprehensive solution successfully addresses the challenges encountered when analyzing multipesticides in difficult matrices such as black pepper and dried tea. The high sensitivity of the 7010B GC/TQ enables the application of deep dilution methods. Additionally, the use of backflush technology combined with the Agilent JetClean self-cleaning ion source ensures system stability and robustness, enhancing the operational efficiency of testing laboratories and reducing equipment downtime during&nbsp;maintenance.<h3>2. EST Analytical: Static Headspace Sampling of Volatile Organic Compounds</h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/Flex_8260_by_Static_Headspace_7ddf2e4157.pdf">Full PDF for download</a></li></ul><h4>Discussion</h4>Purge and trap sampling involves purging the VOCs out of the matrix and trapping the analytes onto an analytical trap, the trap is then desorbed to the GC/MS. This process has a number of pros and cons. On the positive side, purge and trap is more sensitive. It is also the recommended sampling technique for USEPA Methods. Furthermore, the advent of autosampling systems has simplified sample preparation. However, purge and trap does have some negatives, including active sites, worries about foaming samples, and trap degradation.Static headspace sampling, on the other hand, is much simpler than purge and trap sampling. For this sampling technique, the sample is brought to equilibrium and a portion of the headspace is transferred to the GC/MS for separation and analysis. The simplicity of this technique is a definite pro. Moreover, this sampling process does not develop active sites, has no need for an analytical trap and the linear calibration range can be much higher than that of purge and trap sampling. Conversely, samples need to be manually prepped thus, losing their sample integrity. Additionally, the detection limits are higher for a number of compounds. Finally, some of the analytes do not partition into the headspace well enough and need method optimization.&nbsp;In recent years, GC/MS systems have become much more sensitive. The advent of SIM/Scan acquisition techniques has made low level detection a much simpler proposition. This analysis will focus on the headspace sampling and analysis of over 50 volatile organic compounds.&nbsp;<h4>Experimental</h4>The sampling system used for this analysis was the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/2162">EST Analytical FLEX autosampler</a> fitted with a 2.5ml headspace syringe. An <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=7890+GC">Agilent 7890 GC</a> and <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=5975">5975 MS</a> were used for separation and analysis. The GC was configured with a Restek Rxi 624 Sil MS 30m x 250mm x 1.4µm column and a SKY 2mm x 6.5 x 78.5 splitless inlet liner. The MS was run in SIM/Scan mode. Refer to Tables 1 and 2 for the analysis and sampling parameters.<h4>Conclusions</h4>Static headspace sampling in conjunction with SIM/Scan acquisition proved to be a good alternative to purge and trap sampling for a number of USEPA Method 8260 compounds. The curve %RSD results showed the linearity of the curve to meet the USEPA Method 8260 requirement of 15% or better. The method detection limits of all the compounds tested also passed method requirements. Lastly, the precision and accuracy of the autosampling and analysis system was excellent, with the average precision at less than 6% RSD and the average %recovery at just over 101%.<h3>3. Shimadzu: Aromatic Component Analysis of Gasoline According to ASTM D5580 Using the Brevis GC- 2050 Gas Chromatograph</h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_01_01024_en_039b304288.pdf">Full PDF for download</a></li></ul>Aromatics, such as toluene and xylene, are sometimes added to gasoline to improve the octane number. Measuring the levels of these aromatics is essential for quality control in gasoline production. It is also important for environmental protection, in particular, for reducing emissions of benzene, a hazardous substance, as well as for sustainable energy use that reduces the environmental impact of gasoline while maintaining its performance.ASTM D55801) is a standard test method that uses gas chromatography to measure aromatics in gasoline. Gasoline aromatics can be separated more effectively by switching between two gas chromatography columns of different polarities and venting non-aromatic components from the system. This Application News describes using the Brevis GC2050 gas chromatograph to determine aromatics in gasoline by applying ASTM D5580.<h4>Equipment Configuration and Analytical Conditions&nbsp;</h4>The system comprises a <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=1&amp;search=Brevis+GC-2050">Brevis GC-2050 gas chromatograph</a>, an <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=1&amp;search=AOC-30">AOC-30</a> for sample injection, and a VB-30-S heated valve box. Aromatics were determined using two sets of Analysis Conditions that were tailored to measure different components (Table 1). Note that the timing of the flow path switching and other conditions needs to be adjusted according to the columns being used and the operating environment.<h4>Determining Aromatics in Gasoline&nbsp;</h4>A gasoline sample was prepared by adding 2 to 10 wt% aromatics and 10 wt% of an internal standard (2-hexanone) and then analyzed under Analysis Conditions A and Analysis Conditions B. Fig. 2 shows the chromatograms obtained under each set of Analysis Conditions. Despite gasoline containing large amounts of hydrocarbons, oxygenates, and other impurities, these impurities did not appear as peaks in the chromatograms, and only the aromatics added to the gasoline were detected. These results verify the utility of using flow path switching to effectively utilize the characteristics of two different columns.<h4>Conclusion&nbsp;</h4>A flow path switching valve was installed on a Brevis GC-2050 gas chromatograph to enable the determination of gasoline aromatics (benzene, toluene, ethylbenzene, p/m-xylene, oxylene, and C9+ aromatics) according to ASTM D5580.&nbsp;This system can switch between different columns during analysis to determine specific aromatics from among the many compounds present in gasoline. Analysis was performed under two sets of conditions, each using different flow path switching times. This method met the requirements for linearity and reproducibility described in ASTM D5580. The timing of flow path switching can also be adjusted to allow the targeted determination of oxygenates in gasoline. The ability to perform multiple analyses on a single system means the Brevis GC-2050 offers even greater functionality as a compact gas chromatograph.

News from LabRulezGCMS Library - Week 02, 2026

News from LabRulezLCMS Library - Week 02, 2026

Our Library never stops expanding. What are the most recent contributions to LabRulezICPMS Library in the week of 5th January 2026? Check out new documents from the field of spectroscopy/spectrometry and related techniques!<blockquote>👉 <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library">SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT SPECTROSCOPY/SPECTROMETRY RELATED TECHNIQUES</a></blockquote><blockquote>👉 Need info about different analytical techniques? Peek into <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library">LabRulezLCMS</a> or <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library">LabRulezGCMS</a> libraries.</blockquote>This week we bring you application notes by Agilent Technologies, Metrohm and Waters Corporation!<h3>1. Agilent Technologies: Multi-Elemental Analysis of Lithium Aluminum Titanium Phosphate by Automated ICP-OES</h3>Assay of all-solid-state Li-ion battery electrolytes by <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library?mainauthorItems=10&amp;search=5800+ICP-OES">Agilent 5800 ICP-OES</a> with ADS 2 autodilutor<ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_solid_state_battery_LATP_5800_icp_oes_5994_8814en_agilent_e06fd80560.pdf">Full PDF for download</a></li></ul>Rising global electricity demand and the shift away from fossil fuels are driving developments in the cleaner energy and energy storage sectors. Among the emerging energy storage technologies, all-solid-state batteries (ASSBs) are attracting attention due to their enhanced safety, higher energy density, and improved performance relative to conventional lithium-ion batteries (LIBs). Current research is largely focused on optimizing the electrolyte composition of ASSBs, which use a solid electrolyte in place of the liquid or gel electrolyte found in conventional LIBs.&nbsp;Various properties of lithium aluminum titanium phosphate (LATP) make it suitable as a solid electrolyte material for use in ASSBs.1 It has high ionic conductivity (reaching 10–⁴ to 10–³ S/cm at room temperature, close to or exceeding some liquid electrolytes), which improves battery charging and discharging efficiency.&nbsp;Compared to sulfide-based solid electrolytes, LATP is more chemically stable in air and water, minimizing the requirement for an inert atmosphere during processing. This property simplifies manufacturing and reduces costs of storage and transportation. LATP is compatible with high-potential (5 V) cathode materials such as LiNiCoMnO2 (NMC), improving cell energy density. It also offers excellent mechanical strength and ease of processing, allowing it to be shaped into thin films that support miniaturization and robust battery design. The accurate determination of major, doping, and trace elements in materials such as LATP is important at all stages of development, from R&amp;D to pilot-scale production and full-scale manufacturing. The ratio of major elements to doping elements significantly affects the ionic conductivity and stability of lithium (Li) ions, while trace impurities can compromise stability and mechanical strength. Elemental impurities can accumulate during battery charging/ discharging cycles, leading to battery performance degradation, such as shortened cycle life, reduced efficiency, or potential safety risks. Multi-elemental analysis of battery precursors like LATP is therefore vital for ensuring the overall quality of ASSBs.2&nbsp;Battery scientists also require methods to analyze the elemental composition of spent electrolytes to investigate changes that occur during charge and discharge cycles. These analyses support the production of consistent and reliable materials, promoting technological advancement and enabling the industrial implementation of ASSBs.&nbsp;Inductively coupled plasma-optical emission spectroscopy (ICP-OES) is widely used for the simultaneous measurement of multiple elements in complex samples, due to its speed, stability, and tolerance to high total dissolved solids (TDS). Samples with elevated concentrations of matrix elements are classified as high TDS. These samples can pose several analytical challenges for ICP-OES, including spectral interferences from overlapping emission lines, plasma instability, signal drift, and increased maintenance. However, these challenges can be managed or avoided using fieldproven instrumentation. The Agilent 5800 Vertical Dual View (VDV) and 5900 Synchronous Vertical Dual View (SVDV) ICP-OES instruments have seen widespread adoption throughout the LIB value chain, effectively addressing the diverse analytical requirements of the industry.3&nbsp;In a recent study, the 5800 VDV ICP-OES was used for the quantitative analysis of the matrix elements in a Lithium Lanthanum Zirconate Tantalum sample, another all-solidstate electrolyte material.4 The 5800, which uses a robust vertical torch, SSRF generator, Cooled Cone Interface, and is engineered without moving optical components, ensured excellent stability and no maintenance-related interruptions during the analysis.5<h4>Experimental</h4><h5>Instrumentation&nbsp;</h5>The Agilent ICP-OES Automation System was used for the analysis of the LATP sample digests (Figure 1). The <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library?mainauthorItems=10&amp;search=5800+ICP-OES">Agilent 5800 VDV ICP-OES</a> was equipped with a MiraMist nebulizer, inert spray chamber, and a fully demountable torch assembly with a 1.8 mm id injector. The Agilent ADS 2 in-line autodilutor was used for the automatic preparation of calibration standards and autodilution of samples. Details of the operation and capabilities of the ADS 2 can be found elsewhere.10 Following preparation, the standards and samples were delivered to the ICP-OES by the Agilent SPS 4 autosampler.<h4>Conclusion&nbsp;</h4>A highly automated ICP-OES method was developed for the simultaneous measurement of four major elements and 16 minor and trace elements in lithium aluminum titanium phosphate (LATP) solid electrolyte samples. The samples were acid digested using microwave-assisted digestion and then analyzed using an Agilent ICP-OES Automation System. The automated system comprised an Agilent 5800 VDV ICP-OES with integrated AVS 7 switching valve coupled to an ADS 2 intelligent dilution system, all controlled by Agilent ICP Expert Pro software.&nbsp;The ADS 2 automatically prepared the calibration standards from two stock solutions, accelerating the preparation process, reducing analyst workload, and minimizing labware usage. Calibration curves with correlation coefficients above 0.999 for all elements were autogenerated.&nbsp;MDLs below 1 mg/kg were achieved for most of the trace elements in the sample. Recoveries of all 16 trace elements spiked at both 0.2 mg/L (1.0 mg/L for Mg) were between 91 and 107%, confirming the accuracy of the method. The instrument displayed excellent stability during the analysis of the four matrix elements in the actual LATP samples over two hours, with data fluctuation below 1%.&nbsp;The automated quantitative ICP-OES method supports R&amp;D and QA/QC by detecting impurities like Fe, Mg, and Na, while also measuring Li, Al, Ti, and P in the same run. Ensuring the quality of LIB-electrolyte materials is important to meet desired performance targets, enhance safety, and extend the longevity of solid-state batteries.<h3>2. Metrohm: Quality control of honey with NIR spectroscopy</h3>Simultaneous determination of color and glucose, fructose, sucrose, maltose, and turanose content with results in seconds&nbsp;<ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_nir_135_download_157810ae7b.pdf">Full PDF for download</a></li></ul>Honey is mainly comprised of the sugars glucose and fructose, which make up to 85% of its total weight. It additionally contains sucrose, a disaccharide composed of fructose and glucose, and other disaccharides such as maltose and turanose—present in concentrations from 0.5 to 3.5% [1]. The sugar content of honey is usually measured with high performance liquid chromatography (HPLC). Honey's color is a quality attribute evaluated by consumers and is an important sensory property in the beekeeping market. Internationally, different types of honey are classified using the Pfund color scale. All of these honey quality parameters can be measured simultaneously in just a few seconds without any sample preparation using near-infrared spectroscopy (NIRS).<h4>EXPERIMENTAL EQUIPMENT&nbsp;</h4>Pure honey samples were measured with an <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library?mainauthorItems=220&amp;search=OMNIS+NIR">OMNIS NIR Analyzer Solid </a>(Figure 1). All measurements were performed in transflection mode (1000–2250 nm) using a 2 mm gap size reflector and 28 mm disposable vials. <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library?mainauthorItems=220&amp;search=OMNIS+software">OMNIS Software</a> was used for all data acquisition and prediction model development. HPLC was the reference method used to measure the concentration of glucose, fructose, sucrose, maltose, and turanose in honey. Color was measured using a Pfund colorimeter and the Pfund scale, which ranges from 0 to 140 mm (from very light-colored honey up to the darkest honey).<h4>RESULT</h4>The obtained NIR spectra of honey samples (Figure 2) were used to create prediction models for quantification of glucose, fructose, sucrose, maltose, and turanose content, as well as color. The quality of the prediction models was evaluated using correlation diagrams (Figures 3–8) which display a very high correlation between the NIR prediction and the reference values. The respective figures of merit (FOM) display the expected precision of a prediction during routine analysis<h4>CONCLUSION</h4>This Application Note displays the benefits of using near-infrared spectroscopy for quality control of honey. Color, along with glucose, fructose, sucrose, maltose, and turanose content can be measured simultaneously in only a few seconds. Measurements performed with NIR spectroscopy do not need any sample preparation nor solvents, saving users time and money. By using NIRS, only one analytical technology is required for sample measurement, compared to other conventional methods (Table 1). Finally, NIRS does not require skilled technical operators to perform the measurements, unlike HPLC.<h3>3. Waters Corporation: High-Throughput Measurement of Compound Solubility and Physical Form with BMI</h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/labrulez-bucket-strapi-h3hsga3/720009139_en_40f2d10920.pdf">Full PDF for download</a></li></ul>Aqueous solubility of small molecule compounds is an essential parameter during the hit-to-lead stage of drug discovery as well as during lead optimization and formulation. Low solubility can impact biological assays in a number of ways, including underestimated potency and toxicity, inaccurate structure-activity relationships (SAR), and difficult to interpret results. Poor bioavailability and underestimated toxicity directly impact downstream formulation and manufacturability of dosage forms – increasing development costs and reducing the chances of a drug candidate’s success.1–3&nbsp;In this application note, we introduce backgrounded membrane imaging (BMI) on the <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library?mainauthorItems=5&amp;search=HORIZON">HORIZON® system</a> as a rapid and sensitive high-throughput method for compound solubility measurement. Particle analysis with BMI is easy to perform, requires as little as 25 of sample, and is unaffected by solvents or other media components. In addition, highly resolved images and shape distribution data provide valuable information on morphology of precipitated solids for more comprehensive solubility characterization.<h3>Results and Discussion&nbsp;</h3><h4>BMI Overcomes Limitations of Other Solubility Screening Methods&nbsp;</h4>Despite its critical importance at early stages, current methods for solubility measurement have limitations that affect reliability and/or time to results (Figure 1). In the more cumbersome multi-step methods, precipitates are removed by filtration or centrifugation, and concentration of compound remaining in solution is measured by various detection technologies such as UV absorbance or mass spectrometry coupled with HPLC. These methods are not only time consuming and inefficient, but can be affected by compound sticking to filters, incomplete removal of low-density aggregates by centrifugation, and interference by solvents and matrix impurities.<h4>How BMI Works&nbsp;</h4>The HORIZON® system system uses sophisticated image-processing techniques coupled with a simple workflow to acquire and analyze particle data. First, the HORIZON® membrane plate wells are measured to generate a background image (Figure 2a). Samples are then pipetted directly onto the membrane wells and filtered through by vacuum, capturing insoluble particles on the surface. The same wells are re-imaged in the HORIZON® instrument. After measuring, the software aligns and processes background and sample images pixel by pixel so that background texture is eliminated, and particles can be viewed in high contrast with minimal interference from membrane surface imperfections (Figure 2b).<h4>Conclusion&nbsp;</h4>Here, we have demonstrated how high-throughput membrane imaging with BMI on the HORIZON® system offers reliable, informed solubility assessment of small molecule compounds. In addition, imaging provides valuable information on solid state morphology for better interpretation of solubility results. Whether used as a primary solubility screening method, an orthogonal technique, or as a check to eliminate problematic candidates prior to in-depth characterization, implementing BMI technology can accelerate drug discovery and early ADME workflows - providing more complete information with less time and less material than traditional methods.

News from LabRulezICPMS Library - Week 02, 2026

Are We Ready for It? A Review of Forensic Applications and Readiness for Comprehensive Two-Dimensional Gas Chromatography in Routine Forensic Analysis

A furan-based glycidyl amine epoxy resin was synthesized using furfuryl amine and epichlorohydrin and monitored during synthesis by GPC and FTIR. Two major products, furan diepoxy (FDE) and α-chlorohydrin FDE, formed concurrently, with α-chlorohydrin FDE becoming dominant at longer reaction times.Both products were purified and cured with an amine to study network formation using DSC, FTIR, and NMR. Thermomechanical properties measured by DMA showed that α-chlorohydrin FDE exhibited significantly higher stiffness and glass transition temperature than purified FDE. These enhanced properties were attributed to additional cross-linking through furan ring-opening, establishing a clear structure–property relationship.<blockquote><h4>The original article</h4><h4><a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/10.1021/acsomega.5c05822">Synthesis, Processing, and Performance of a Furan-Based Glycidyl Amine Epoxy Resin</a></h4>Amy Honnig Bassett, Emre Kinaci, and Giuseppe R. Palmese*ACS Omega 2025, 10, 46, 55432–55445<a target="_blank" rel="noopener noreferrer" href="https://doi.org/10.1021/acsomega.5c05822">https://doi.org/10.1021/acsomega.5c05822</a><h6>licensed under <a target="_blank" rel="noopener noreferrer" href="https://creativecommons.org/licenses/by/4.0/">CC-BY 4.0</a></h6></blockquote>Selected sections from the article follow. Formats and hyperlinks were adapted from the original.Epoxy resins are conventionally bisphenol A (BPA) based, with the diglycidyl ether of BPA (DGEBA) making up about 70% of the epoxy usage. <a href="javascript:void(0);">(1,2)</a> BPA is a petroleum-based resource and a known human endocrine disruptor. <a href="javascript:void(0);">(3,4)</a> With a growing focus on a more sustainable future, researchers have sought BPA alternatives. Literature has shown furan to be a promising candidate as a phenolic alternative because of its aromaticity and availability. <a href="javascript:void(0);">(5,6)</a>Furan is a heterocyclic, five-membered ring extracted from polysaccharides found in biomass wastes. <a href="javascript:void(0);">(5)</a> Furan-based compounds can possess a wide variety of functionality, including carboxyl, hydroxyl, amino, and vinyl moieties, leading to ease of use in multiple chemistries. <a href="javascript:void(0);">(6)</a> Epoxy-amine chemistry using furan-based compounds has been explored in numerous studies. Hu et al. successfully synthesized the furan-based epoxy monomer, 2,5-bis[(2-oxiranylmethoxy)-methyl]-furan (BOF) from 2,5-bis(hydroxymethyl) furan (BHMF). BOF cured with conventional aliphatic and aromatic amines had an increased room temperature storage modulus (E’) compared to benzene-based analogs. The improved property was hypothesized to result from potential hydrogen bonding associated with the oxygen atom in the furan ring. <a href="javascript:void(0);">(7)</a> A fully furan-based epoxy-amine system was also synthesized and cured. BOF was cured with difuran diamine (DFDA), synthesized from furfuryl amine. BOF/DFDA had a further increased Tg and room temperature E’ compared to BOF cured with a conventional aliphatic amine. The reasoning was again attributed to the potential hydrogen bonding of the oxygen in the furan ring with hydroxyl groups resulting from the epoxy-amine ring opening reaction. Additionally, the fully furan-based system also had increased thermal stability with a char yield in nitrogen at 750 °C of 40 wt %. <a href="javascript:void(0);">(8)</a> Other investigators found similar results when using 2,5-furan dicarboxylic acid (FDCA) as the starting furan material. The epoxy monomer based on FDCA cured with 3, 3′-diamino diphenyl-sulfone (33DDS) and 4, 4′-diamino diphenyl-sulfone (44DDS) had excellent E’ and Tg compared to nonfuran-based systems. <a href="javascript:void(0);">(9)</a> Potential hydrogen bonding and increased chain packing were attributed to the improved properties. The researchers proposed similar ideas for why furan increased viscoelastic properties, but did not provide fundamental evidence. The above-mentioned furan-based molecules require relatively complicated synthesis and purification processes to obtain thermosetting materials and have limited commercial availability. However, some furan-based molecules, such as furfuryl amine, are commercially available and can be readily functionalized to create thermoset materials. This investigation seeks to fundamentally understand the influence of the furan ring on (1) epoxy monomer synthesis, (2) epoxy-amine thermoset processing, and (3) polymer performance characteristics. The outcomes of this work will provide evidence for the role furan plays in improving the viscoelastic properties and promote the use of furan in thermosetting systems.Epoxidizing furfuryl amine creates glycidyl amines instead of the glycidyl ethers shown in literature with BPA-based systems. Glycidyl ethers are characterized by an oxygen atom connected to the oxirane group and are the most widely used epoxy resins. Due to their popularity, extensive research has been done to fundamentally understand the synthesis and curing procedures to obtain the best properties with these materials. <a href="javascript:void(0);">(10,11)</a> Glycidyl amines, however, are less common, leading to a more limited fundamental understanding of these systems for achieving the best properties. Glycidyl amines are characterized by a nitrogen atom connected to the oxirane group. Generally, epoxies are synthesized using epichlorohydrin and an acidic hydroxyl group for glycidyl ethers or an amine-containing compound for glycidyl amines. <a href="javascript:void(0);">(11,12)</a> Despite similar synthetic routes, glycidyl amines present a unique challenge because of the formation of a tertiary amine upon complete glycidation. Tertiary amines are known to catalyze an epoxy’s ring opening, leading to homopolymerization and potentially creating unwanted side products during synthesis or cure. <a href="javascript:void(0);">(10,12)</a>Limited foundational work has been done on glycidyl amine synthesis or cure. In the 1990s, a series of papers was published analyzing the impurities formed during the synthesis of glycidyl amines, the kinetics of intramolecular cyclization, and shelf life analysis. <a href="javascript:void(0);">(13−17)</a> A review was also published focused on the kinetics and mechanisms of cure of glycidyl amines. <a href="javascript:void(0);">(18)</a> Since the publication of these papers, there has been limited research on glycidyl amines. Additionally, the published papers focused on aniline-based molecules. Incorporating furan into a glycidyl amine will introduce further complications because of the structural differences between furan and benzene rings. To the best of our knowledge, there is no published work on understanding the interaction of the furan ring during the synthesis and cure of glycidyl amine.This work has three aims: (1) to investigate the effect of synthetic conditions on glycidyl amine monomer formation, (2) to determine the interaction of the furan ring with glycidyl amine products during polymerization, and (3) to evaluate how the synthetic and polymerization conditions impact the final polymer properties of a furan-based glycidyl amine. The outcomes of this work will provide evidence for the unique ability of the furan ring to interact with synthetic products that are specific to glycidyl amine chemistry and how this can be tailored to impact the final polymer properties.<h4>Experimental Section</h4><h5>Resin Characterization</h5>All FDE and FGE resins were characterized using gel permeation chromatography (GPC). A <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/194">Waters AQUITY Advanced Polymer Chromatography </a>unit with an AQUITY refractive index detector was used. Tetrahydrofuran (THF) Optima was used as the eluent with a flow rate of 0.6 mL min–1. A series of 4.6 × 150 mm <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/1950">AQUITY APC columns</a> (XT 450 2.5 μm, XT 125 2.5 μm, and XT 45 1.7 μm) was used and maintained at 40 °C. Polystyrene standards were used to calibrate the instrument (PSS ReadyCal Kit, range: 474–2,500,000 g mol–1; maximum Đ: 1.15). Samples were prepared by mixing 10–12 mg of resin into 2 mL of THF. The number-average molecular weight (Mn) and areas under the curve were determined. The hydrolyzable chlorine content was measured for Flashed-FDE and 52 h.-FDE following ASTM D1726–11 using Test Method A. <a href="javascript:void(0);">(19)</a> Test method A is used for 1 wt % or less hydrolyzable chlorine content.The epoxy equivalent weight (EEW) was measured for Flashed-FDE and 52 h.-FDE. The EEW was measured following ASTM D1652–19 using the manual titration method. <a href="javascript:void(0);">(20)</a> However, it was found that for monosubstituted furan epoxies, the furan ring interacted with the perchloric acid used in the titration. A new titration method was developed to obtain an accurate EEW for monosubstituted furan epoxies based on methacrylation and acid number titration. Complete details on the EEW method are found in the <a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/suppl/10.1021/acsomega.5c05822/suppl_file/ao5c05822_si_001.pdf">SI</a>.Samples were also characterized by 1H- and 13C{1H}-NMR (24 °C in CDCl3) using a Bruker Avance Neo 400 MHz NMR Spectrometer. 1H NMR spectra with peak assignments are found in <a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/suppl/10.1021/acsomega.5c05822/suppl_file/ao5c05822_si_001.pdf">Figures S2–S4</a>. Full 13C{1H}-NMR spectra are found in <a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/suppl/10.1021/acsomega.5c05822/suppl_file/ao5c05822_si_001.pdf">Figures S5–S7</a>. The 1H NMR chemical shifts, number of protons represented by the signal, peak multiplicity, and coupling constants are listed below for the two pure products of Flashed-FDE and 52 h.-FDE. Additionally, the 13C{1H}-NMR chemical shifts are denoted below for Flashed-FDE and 52 h.-FDE.<h5>Reaction Kinetics for S-FDE and 1:10-FDE</h5>A Thermo Scientific Nicolet iS50 FTIR spectrometer was used in transmission mode in the near-IR range (4000–8000 cm–1) to track the formation of the epoxy-amine adduct over time. The reaction mixtures of 1:2.1 and 1:10 furfuryl amine: epichlorohydrin were mixed at room temperature and put into the FTIR cell setup. The cell setup was a sealed 1.5 mm outer diameter glass tube. A spectrum was taken every 30 min for 52 h, and each spectrum was 32 scans with a 4 cm–1 resolution. The peak height of 5987 cm–1 was used as a reference. The conversion of epoxy (EP, 6080 cm–1), secondary amine (SA, 6545 cm–1), and primary amine (PA, 4945 cm–1) were calculated using <a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/10.1021/acsomega.5c05822#eq1">eqs 1</a>–<a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/10.1021/acsomega.5c05822#eq3">3</a>, where I(t = 0) and I(t) are the designated peak intensities before and during cure: <a href="javascript:void(0);">(21−23)</a><h4>Results and Discussion</h4><h5>Investigating the Effect of Reaction Conditions on FDE Resin Synthesis</h5><a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/10.1021/acsomega.5c05822#fig2">Figure 2</a> includes the GPC traces for S-FDE and Flashed-FDE. The S-FDE trace had three peaks, suggesting the presence of high-molecular-weight oligomers in addition to pure FDE. Comparing the GPC traces of S-FDE and Flashed-FDE shows the location of the pure FDE peak, as Flashed-FDE has one peak at 8.56 min with an Mn value of 209 Da based on polystyrene standards. The molecular weight of FDE is 210 Da. Flash chromatography successfully removed oligomers and unreacted epichlorohydrin.<img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/ACS_Omega_2025_10_46_55432_55445_Figure_2_GPC_trace_for_S_FDE_1_10_FDE_and_Flashed_FDE_23cd341c27.jpg" alt="ACS Omega 2025, 10, 46, 55432–55445: Figure 2. GPC trace for S-FDE, 1:10-FDE, and Flashed-FDE" srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_ACS_Omega_2025_10_46_55432_55445_Figure_2_GPC_trace_for_S_FDE_1_10_FDE_and_Flashed_FDE_23cd341c27.jpg 151w," sizes="100vw" width="617" height="637">The GPC peak areas were used to calculate the percentage of pure FDE formed in S-FDE. By this method, S-FDE contained about 44% pure FDE, with the remaining being high-molecular-weight oligomers.Using excess epichlorohydrin well above the stoichiometric value in the epoxidation of bisphenols and other alcohols yields products with limited oligomerization wherein the amount of n = 0 monomers can be more than 85%. <a href="javascript:void(0);">(12)</a> In an attempt to eliminate both the oligomers formed and the need for flash chromatography to purify the epoxidation products of furfuryl amine, a higher molar ratio of furfuryl amine to epichlorohydrin (1:10 mol) was used. <a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/10.1021/acsomega.5c05822#fig2">Figure 2</a> also shows the GPC trace for the epoxidation products of 1:10-FDE.1H NMR spectroscopy was used to characterize the products formed during synthesis. The 52-h product, though similar to Flashed-FDE, particularly with respect to the monosubstituted furan ring (<a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/suppl/10.1021/acsomega.5c05822/suppl_file/ao5c05822_si_001.pdf">Figures S2–S4</a>), had noticeable differences in the epoxy hydrogen peaks and the hydrogens on the carbon bridge between the furan and the nitrogen. In both regions, there was peak broadening, suggesting the formation of a product containing additional chemical groups.13C{1H}-NMR spectroscopy was used instead to characterize the products formed during the synthesis because the spectra had more apparent differences. <a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/10.1021/acsomega.5c05822#fig5">Figure 5</a> shows 13C NMR spectra (A) showing the furan ring carbon region, and (B) showing the carbons between the epoxy ring and furan. The full spectra are found in <a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/suppl/10.1021/acsomega.5c05822/suppl_file/ao5c05822_si_001.pdf">Figures S5–S7</a>.<img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/ACS_Omega_2025_10_46_55432_55445_Figure_5_13_C_1_H_NMR_for_increasing_reaction_time_42b517715b.jpg" alt="ACS Omega 2025, 10, 46, 55432–55445: Figure 5. 13C{1H}-NMR for increasing reaction time of 1:10-FDE compared to Flashed-FDE with spectra offset for clarity. (A) Furan ring carbons with all carbons in the FDE structure labeled for all regions. Inserts are zoomed-in portions of the spectra. (B) Epoxy and chlorinated product carbons." srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_ACS_Omega_2025_10_46_55432_55445_Figure_5_13_C_1_H_NMR_for_increasing_reaction_time_42b517715b.jpg 225w," sizes="100vw" width="1817" height="1263"><h5>Model Study of 52 h.-FDE Cured with Furfuryl Amine</h5>1H- and 13C{1H}-NMR techniques are better suited than FTIR for elucidating the bonds forming after furan ring opening. However, polymers that can be dissolved in solvents are required to use these techniques. Therefore, 52 h.-FDE was cured with furfuryl amine, a monoamine, to control network formation and allow the samples to be soluble in NMR solvent. <a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/10.1021/acsomega.5c05822#fig8">Figure 8</a> shows reaction information for 52 h.-FDE cured with furfuryl amine, including A) a general reaction scheme, B) FTIR data, C) 13C{1H}-NMR data, and D) 1H NMR data for unreacted and cured samples.<img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/ACS_Omega_2025_10_46_55432_55445_Figure_8_52_h_FDE_cured_with_furfuryl_amine_up_to_160_C_0e3ac8f3c8.jpg" alt="ACS Omega 2025, 10, 46, 55432–55445: Figure 8. 52 h.-FDE cured with furfuryl amine up to 160 °C. A) General reaction scheme. B) FTIR spectra before and after cure. C) 13C{1H}-NMR at room temperature and 160 °C after 2 h. D) 1H NMR at room temperature and 160 °C after 2 h." srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_ACS_Omega_2025_10_46_55432_55445_Figure_8_52_h_FDE_cured_with_furfuryl_amine_up_to_160_C_0e3ac8f3c8.jpg 182w," sizes="100vw" width="1500" height="1288"><h4>Conclusions</h4>In this study, the synthesis, polymerization, and physical properties of the epoxidation of furfuryl amine with epichlorohydrin to create FDE were investigated. First, the synthesis and isolation of FDE were studied by varying the reaction conditions, including epichlorohydrin concentration and epoxy adduct formation time. When furfuryl amine was epoxidized with excess epichlorohydrin, a chlorinated side product formed in addition to the desired FDE monomer. The chlorinated side product was α-chlorohydrin FDE, referred to as 52 h.-FDE in this work.The next step was to evaluate the effect of structural variations on epoxy-amine polymerization by comparing the polymerization of Flashed-FDE and 52 h.-FDE cured with PACM. Curing 52 h.-FDE with PACM promoted the formation of additional cross-linking reactions. A reaction pathway was proposed for the formation of additional cross-links. The hydrolyzable chlorine on 52 h.-FDE accelerated the epoxy-amine polymerization but also promoted the ring opening of furan. Furan is commonly accepted as a nonreactive group, but under specific conditions, it will act as a functional group to participate in network formation.Finally, the increased cross-links were confirmed using cross-link density measurements, and the effect of additional cross-links on physical properties was evaluated. The experimental ve for 52 h.-FDE/PACM was greater than the experimental ve for Flashed-FDE/PACM, as well as the theoretical ve values. The increase ve supported the findings from the second step. The additional cross-linking resulted in an E′ of 4.4 GPa and Tg of 129 °C for 52 h.-FDE/PACM. Epoxy resins containing both a furan ring and hydrolyzable chlorine have the potential to increase the final properties due to the additional cross-linking reactions the furan ring can participate in.

Synthesis, Processing, and Performance of a Furan-Based Glycidyl Amine Epoxy Resin

Bacillus species produce diverse bioactive lipopeptides that contribute to their ecological and biocontrol functions, yet some families remain poorly characterized. This study focuses on kurstakins, a lipopeptide family associated with biocontrol activity, using metabolomic, structural, and multiomics approaches.Metabolomic analysis of a Bacillus cereus extract revealed approximately 50 kurstakin analogs with diverse linear and branched lipid tails. Two new analogs were isolated and fully characterized by NMR, providing the first experimental determination of absolute configuration within this family. Integration of public genomic and MS data further demonstrated the broad chemical diversity and global distribution of kurstakins, highlighting their potential ecological significance in Bacillus-based biocontrol systems.<blockquote><h4>The original article</h4><h4><a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/10.1021/acs.jnatprod.5c01212">Structural Characterization and Multiomics Analysis Reveal Extensive Diversity and Global Distribution of Kurstakin Lipopeptides</a></h4>Rose Campbell, and Emily Mevers*J. Nat. Prod. 2025, 88, 12, 2960–2967<a target="_blank" rel="noopener noreferrer" href="https://doi.org/10.1021/acs.jnatprod.5c01212">https://doi.org/10.1021/acs.jnatprod.5c01212</a><h6>licensed under <a target="_blank" rel="noopener noreferrer" href="https://creativecommons.org/licenses/by/4.0/">CC-BY 4.0</a></h6></blockquote>Selected sections from the article follow. Formats and hyperlinks were adapted from the original.Lipopeptides are a well-known family of microbial natural products that possess a range of applications, including their potential medicinal uses and as crop biocontrol agents. <a href="javascript:void(0);">(1)</a> Several lipopeptides or synthetic analogs are FDA-approved for the treatment of infectious diseases, including as antibiotics (e.g., polymyxin B, oritavancin, telavancin, and daptomycin) and antifungals (e.g., rezafungin and micafungin), with many others in various stages of clinical trials. <a href="javascript:void(0);">(2,3)</a> Their bioactive properties arise from their amphiphilic structures, which consist of a fatty acid tail (lipid) and a polar peptide. The lipopeptide antibiotics are known to bind to cell membranes, forming pores that lead to depolarization. <a href="javascript:void(0);">(4)</a> Lipopeptides are commonly produced by a diverse range of microorganisms, including bacteria, fungi, and cyanobacteria; however, Bacilli are particularly well-known for their ability to produce structurally diverse bioactive lipopeptides. This includes the widespread production of surfactins, iturins, fengycins, polypeptins, and octapeptins. <a href="javascript:void(0);">(2,5)</a> This biosynthetic capability has led to their wide use as biocontrol agents in agricultural settings, such as Bacillus thuringiensis being leveraged for insect and disease control and Bacillus velezensis for controlling plant pathogens. <a href="javascript:void(0);">(6,7)</a> The diverse lipopeptides produced by these strains have been shown to work synergistically as antifungals, biofilm formation regulators, and plant defense modulators. <a href="javascript:void(0);">(5,8)</a>Although many lipopeptides have been well characterized from Bacilli, this does not represent their full biosynthetic potential. <a href="javascript:void(0);">(9)</a> In addition, many lipopeptide families have been mentioned in the literature, but lack appropriate analytical data to confirm their planar and secondary structures and the diversity of the family. <a href="javascript:void(0);">(2)</a> This includes the kurstakins, gavaserin, and saltavalin, which have all been implicated to play a critical role in the biocontrol properties of the producing organisms. <a href="javascript:void(0);">(10)</a> The kurstakins were first discovered to be produced by B. thuringiensis, and have been considered a biomarker for Bacillus cereus group species. <a href="javascript:void(0);">(11,12)</a> However, they have since been isolated from a range of bacteria, including non-cereus group Bacillus species (e.g., B. subtilis, B. licheniformis) <a href="javascript:void(0);">(13,14)</a> and more distantly related bacteria (e.g., Enterobacter cloacae, and Citrobacter sp.). <a href="javascript:void(0);">(15,16)</a> Several of the producing strains have been studied extensively for their potential use as a biocontrol agent, due to their antimicrobial activity and ability to swarm and produce protective biofilms, <a href="javascript:void(0);">(12,17,18)</a> which has been attributed in part to the kurstakins. <a href="javascript:void(0);">(19−22)</a> Four cyclic analogs, kurstakins 1–4 (1–4), were elucidated through tandem mass spectrometry (MSMS) analyses and chemical derivatization. <a href="javascript:void(0);">(12)</a> There have been reports of many additional analogs, but these reports are primarily based on MS analyses. <a href="javascript:void(0);">(23−25)</a> The studies indicate that all analogs contain the same peptide core, but incorporate diverse lipid tails. Additionally, amino acid configurations were deduced through bioinformatic analyses alone, <a href="javascript:void(0);">(17)</a> which can only predict the configuration of the α-position. Therefore, chemical analyses are needed to unequivocally determine the amino acid configurations, particularly of the β-hydroxyl in the threonine residue. Herein, we leveraged our metabolomic data set from marine bacteria to characterize the kurstakins, including the first NMR analysis, report of two new analogs, kurstakins 5 and 6 (5–6), deduction of the absolute configuration, and analysis of the true chemical diversity and distribution of the kurstakins.<h4>Results and Discussion</h4>Analysis of a Global Natural Product Social (GNPS) molecular network representing the chemical potential of diverse marine bacteria from our internal library revealed that it contained a rather large spectral family, with masses ranging from 850 to 940 m/z (<a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/10.1021/acs.jnatprod.5c01212#fig1">Figure 1</a>A). <a href="javascript:void(0);">(26)</a> A subset of these nodes were identified as 1–4 based on their exact mass and key fragment ions (<a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/10.1021/acs.jnatprod.5c01212#fig1">Figure 1</a>B). A peak at 110.1 m/z, which putatively represents a decarboxylated histidine, was abundant in all MSMS spectra and became a key identifying fragment (<a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/10.1021/acs.jnatprod.5c01212#notes-2">Figure S1</a>). Other nodes matched masses of reported kurstakin analogs with hypothetical structures, <a href="javascript:void(0);">(15,19,23,27)</a> as well as new analogs. Based on key MS fragments, this spectral family represents both cyclic and linear core peptide sequences that have incorporated various lipid tails (e.g., C9–C14 with and without hydroxylation; <a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/10.1021/acs.jnatprod.5c01212#notes-2">Figure S2–S3</a>).<img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/J_Nat_Prod_2025_88_12_2960_2967_Figure_1_A_Molecular_family_of_kurstakins_found_in_the_marine_isolates_library_8818fa75c4.jpg" alt="J. Nat. Prod. 2025, 88, 12, 2960–2967: Figure 1. (A) Molecular family of kurstakins found in the marine isolates library, showing structural diversity in tail structure and peptide linearity. (B) Key common fragments of each core peptide used to identify the kurstakins. Fragments not including histidine were rarely observed. (C) Overlaid EICs of all kurstakin masses observed in an enriched semipure fraction, 850–996 m/z, representing a large diversity of cyclic (aqua), linear (blue), and hydroxyl-tail (red) analogs." srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_J_Nat_Prod_2025_88_12_2960_2967_Figure_1_A_Molecular_family_of_kurstakins_found_in_the_marine_isolates_library_8818fa75c4.jpg 245w," sizes="100vw" width="1600" height="889">To characterize the structural breadth of the kurstakin family, the producing strain, B. cereus EM195W, was grown in large-scale (8 L) liquid media containing hydrophobic resins (HP-20, XAD4, and XAD7) to capture the secreted small molecules. After 9 days, the resin was extracted with organic solvents to generate a crude extract. The crude extract was first subjected to reverse-phase (RP) flash chromatography to yield eight refined fractions. MS analysis revealed that the kurstakins were present in the nonpolar fractions, which were combined and processed through normal-phase (NP) flash chromatography, generating an additional 13 fractions. Fractions that were highly enriched with the kurstakins were reanalyzed by high-resolution liquid chromatography-MS (HR-LCMS), revealing the presence of many more analogs than previously detected in the original GNPS analysis. Manual interpretation of the MS data indicated that there is significantly more tail variation than previously thought, which was likely overlooked due to the isobaric nature of many of the analogs and low relative abundance of several analogs (<a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/10.1021/acs.jnatprod.5c01212#fig1">Figure 1</a>C). In total, 31 masses ranging from 850–996 m/z were detected, representing approximately 50 distinct analogs (<a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/10.1021/acs.jnatprod.5c01212#notes-2">Table S1, Figure S4</a>). The breadth of these analogs spanned tail lengths ranging from C9–C17, most of which appeared as all possible combinations of linear- or cyclic-peptide core with and without hydroxylated tails, and represented many previously undescribed compounds.To discover the breadth of tail diversity, we turned to gas chromatography-MS (GC-MS) analysis. A portion of one of the semipurified NP fractions was treated with HCl (aq) to liberate the free acid, which was subsequently methylated with TMS-diazomethane. The methylated fatty acids were analyzed by GC-MS, comparing the retention times and fragmentation patterns with authentic standards of linear, iso-branched, and anteiso-branched fatty acid methyl esters (LCFA, iBCFA, and aBCFA, respectively). <a href="javascript:void(0);">(34)</a> Comparing the derivatized natural material to the LCFA standards revealed the presence of linear fatty acid tails ranging in length from C9–C18 (<a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/10.1021/acs.jnatprod.5c01212#fig2">Figure 2</a>A). This agreed with the masses found on the HR-LCMS, but with the addition of the C18 LCFA.<img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/J_Nat_Prod_2025_88_12_2960_2967_Figure_2_Chemical_characterization_of_the_family_of_kurstakins_405ad6222e.jpg" alt="J. Nat. Prod. 2025, 88, 12, 2960–2967: Figure 2. Chemical characterization of the family of kurstakins. (A) GC-MS traces (EIC of common 74.1 m/z fragment) of the semipure B. cereus EM195W fraction (purple) compared to the LCFA (blue) and iBCFA (aqua) standards. (B) Summary of all fatty acid tails identified in kurstakins produced by EM195W." srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_J_Nat_Prod_2025_88_12_2960_2967_Figure_2_Chemical_characterization_of_the_family_of_kurstakins_405ad6222e.jpg 245w," sizes="100vw" width="1300" height="673"><h4>Experimental Section</h4><h5>General Experimental Procedures</h5>Optical rotation data were recorded on a JASCO P-2000 polarimeter. NMR spectra were recorded in d6-DMSO with the residual solvent peak as an internal standard (δC 39.5, δH 2.50) on a Bruker Avance III 600 MHz instrument equipped with a triple resonance inverse (CP-TCI) Prodigy N2 cooled CryoProbe (1H 600 MHz; 13C 150 MHz) or a Bruker Avance II 500 MHz instrument equipped with a CPBBO Prodigy N2 cooled CryoProbe (1H 500 MHz; 13C 125 MHz). TFA fuming was monitored on a JEOL ECZ 400 MHz instrument equipped with a Royal HFX probe (1H 400 MHz). GC-MS data were obtained using an <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=5975C">Agilent 5975C VL MSD GC-MS</a>. LR-LCMS data were obtained using an <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=10&amp;search=1200">Agilent 1200 series HPLC system</a> equipped with a photodiode array detector and a Thermo LTQ mass spectrometer. HR-ESIMS and HR-MSMS were carried out using an <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=10&amp;search=6530">Agilent 6530 Q-TOF</a> equipped with a <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=10&amp;search=1290+Infinity+II">1290 Infinity II UPLC system</a> or a <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/403">Thermo Orbitrap Exploris 120 mass spectrometer</a>. Reverse-phase flash chromatography purification was carried out with a Biotage Selekt automated flash chromatography system. HPLC purifications were carried out using a <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=10&amp;search=1260+Infinity+II">1260 Infinity II HPLC system</a> equipped with a photodiode array detector. All solvents were of HPLC quality.

Structural Characterization and Multiomics Analysis Reveal Extensive Diversity and Global Distribution of Kurstakin Lipopeptides

Our Library never stops expanding. What are the most recent contributions to LabRulezGCMS Library in the week of 12th January 2026? Check out new documents from the field of the gas phase, especially GC and GC/MS techniques!<blockquote>👉 <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library">SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT GCMS AND RELATED TECHNIQUES</a></blockquote><blockquote>👉 Need info about different analytical techniques? Peek into <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library">LabRulezLCMS</a> or <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library">LabRulezICPMS</a> libraries.</blockquote>This week we bring you application notes by Agilent Technologies, Shimadzu and brochure by Thermo Fisher Scientific!<h3>1. Agilent Technologies: Volatile PFAS in Cosmetics Using PAL3 Coupled with Triple Quadrupole GC/MS</h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_pfas_cosmetics_pal3_gc_tq_5994_8752en_agilent_52b56afd36.pdf">Full PDF for download</a></li></ul>Per- and polyfluoroalkyl substances (PFAS) are a large family of synthetic organic chemicals containing carbon chains where most or all the hydrogen atoms are replaced by fluorine. Due to the strength and stability of the carbon‑fluorine bond, PFAS tend to be very stable and chemically inert, which makes them both very useful in various applications and resistant to degradation. This persistence causes environmental contamination and bioaccumulation in humans and wildlife; as a result, PFAS are often labeled "forever chemicals".1&nbsp;In cosmetics, PFAS are valued for their functional properties, including emulsification, stabilization, and water or sweat resistance. Despite these benefits, concerns have grown over their safety due to direct exposure from repeated use through skin, eyes, and mouth. The OECD's 2024 report underscores the risks associated with PFAS in cosmetic formulations, particularly given their potential for long-term health and environmental impacts.2,3 Regulators around the world are taking decisive steps to ban or restrict PFAS in cosmetics. For example, in the EU, various types of PFAS have been regulated under REACH and POPs regulations that span most industries, including cosmetics.4,5 EU Cosmetics Regulation (EC) No. 1223/2009 has listed the five types of PFAS as the substances prohibited.6 A broader EU-wide ban is underway, with France having passed its own ban on PFAS in cosmetics effective 1 January 2026, as part of a larger proposal to ban PFAS in consumer products.7,8 The US has not banned the use of PFAS in cosmetics at the federal level yet. The USFDA has been evaluating the use of PFAS in cosmetics under the authority of the Cosmetic Regulatory Modernization Act (MoCRA), and is expected to release a report on safety and risk by the end of 2025.9 Although the federal government is still on the sidelines, many states in the US have been rapidly enacting or implementing the ban and reporting requirements for PFAS in cosmetics, with effective dates ranging from 2025 to 2032.10-13 Canada has proposed a ban on the use of PFAS in various consumer products, including cosmetics.14 South Korea has added 12 PFAS into a restricted substances list for cosmetic products in 2024.15 The Environmental Protection Authority (EPA) of New Zealand has officially announced a ban on the use of PFAS in cosmetic products, effective from 31 December 2026.16&nbsp;As regulations surrounding PFAS continue to evolve, developing a sensitive and robust analytical method is crucial to meet stringent guidelines. The objective of this study was to demonstrate a fully automated workflow using PAL3&nbsp;Series&nbsp;2 RTC autosampler coupled with an Agilent 7010D triple quadrupole GC/MS to quantify more than 30&nbsp;volatile PFAS analytes in cosmetics. The automation method performance includes sensitivity, accuracy, and precision studies.<h4>Experimental</h4><h5>Instrumentation&nbsp;</h5>An <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=8890+GC">Agilent 8890 GC </a>with a <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=7010D">7010D GC/TQ</a> equipped with HES 2.0 ion source, coupled with a <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=PAL3">PAL3</a> Series 2 RTC autosampler, was used for this analysis. An MMI inlet and splitless liner (part number 5190-2293) were used and chromatographic separation was performed using an <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=J%26W+DB-624">Agilent J&amp;W DB-624</a>, 30 m × 0.25 mm, 1.40 μm column (part number 122-1334UI). The instrument setup is shown in Figure 1. The acquisition method for 34 native PFAS and four ISTDs, including GC condition, TQ parameters were described in a previous application note.17<h4>Sample analysis&nbsp;</h4>Seven cosmetic samples from various brands—including foundations, lipsticks, and mascaras—were analyzed. One liquid foundation was designated as a quality control (QC) sample, while the remaining six were treated as unknowns. According to the OECD report published in 2024, cosmetic products such as shampoo, eye makeup, foundation, facial cleansers, lipsticks, and lip glosses may contain PFAS, which serve functional or performance-enhancing roles.2,19 In this study, several PFAS compounds were detected above the method detection limit (MDL) in the unknown samples, including 10:2 FTOH, MeFHxSA, MeFOSE, EtOSE and 1H,1H‑perfluorooctyl acrylate. The results also demonstrated that the automated workflow is effective for PFAS extraction and quantitation in cosmetic matrices.<h4>Conclusion&nbsp;</h4>An accurate and robust automated workflow was successfully developed using the PAL3 Series 2 RTC autosampler coupled with the Agilent 7010D GC/TQ system for the analysis of volatile PFAS in cosmetic products. Most PFAS targets achieved an LOQ of 50 µg/kg and MDL below 1.5 µg/kg, with recoveries falling within the acceptable range of 60% to 110%. These results demonstrate excellent extraction efficiency and reliability of the automated workflow. Furthermore, automation significantly reduces human error and enhances productivity, while maintaining high sensitivity in PFAS analysis.<h3>2. Shimadzu: Simplifying Multicomponent Quantitative Analysis of Organic Compounds with the Polyarc Microreactor for GC</h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_01_00945_en_9f7adeedc4.pdf">Full PDF for download</a></li></ul><h4>User Benefits&nbsp;</h4><ul><li>The Polyarc system converts organic compounds eluting from the column into methane, enabling sensitivity to be normalized to carbon concentrations.&nbsp;</li><li>Even for compounds containing heteroatoms or unsaturated bonds, which tend to show lower sensitivity with FID, the Polyarc reduces response differences.&nbsp;</li><li>Because the response is normalized, fewer calibration curves are required even for multicomponent sample analysis.</li></ul>The Flame Ionization Detector (FID), the most widely used detector for GC, is used for quantitative analysis across a wide range of fields because it can detect almost all organic compounds. However, FID can exhibit sensitivity differences depending on the compound type, such as compounds containing heteroatoms (e.g., oxygen or nitrogen) or those with unsaturated bonds (for details, refer to Application News No.01-01033-EN). As a result, conventional quantitative methods using calibration curves— including external standard methods— typically require a separate calibration curve for each target analyte. This application introduces a case study analyzing a mixed solution of eleven compounds with different functional groups using the Polyarc, a GC microreactor. While compounds exhibit varying sensitivity with FID detection, the Polyarc system reduces sensitivity differences between compounds and facilitates quantitative analysis through simplified calibration curve creation.<h4>Overview of the Polyarc</h4>The <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?search=Polyarc">Polyarc</a> is a post-column microreactor installed between the column and the FID. The main unit is mounted on the GC’s top panel. A schematic isshown in Fig. 1. Organic compounds introduced into the Polyarc via the column are fully converted to methane in two steps—oxidation followed by reduction (Fig. 2)—and are ultimately detected by FID. Because the FID detects methane, sensitivity is determined by the number of carbons, regardless of the original organic compound’s functional groups. For example, 1 mol of 1- propanol (C3H8O) is detected as 3 mol of methane.<h4>Analytical Conditions&nbsp;</h4>In this application, the sample was prepared by dissolving nheptane, cyclohexane, toluene, o-xylene, methyl ethyl ketone (MEK), tetrahydrofuran (THF), N,N-dimethylformamide (DMF), butyl acetate, propylene glycol monomethyl ether acetate (PMA), pyridine, and 1,2-dichloroethane in methanol so that each compound was 500 ppm (v/v%). Analytical conditions are shown in Table 1. The instrument used was a <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=1&amp;search=Nexis+GC-2030">Nexis GC-2030</a> equipped with the Polyarc Ultra was used.(Fig. 3) Polyarc can be installed on both the Nexis GC-2030 and the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=1&amp;search=Brevis+GC-2050">Brevis GC-2050</a>. Additionally, in this application, N2 was used as the carrier gas for affordability and safety, enabling cost-effective analysis.<h4>Conclusion&nbsp;</h4>Analyzing multicomponent samples with a Polyarc confirmed that sensitivity differences due to functional groups can be reduced. Compounds containing heteroatoms or unsaturated bonds can be analyzed with relative response comparable to hydrocarbons when a Polyarc is used. Peak area reproducibility was excellent, with %RSD &lt; 1. Additionally, it was confirmed that analyzing at least one compound of known concentration enables quantitation of compounds with unknown concentration—i.e., calibration curve preparation can be omitted.Table 5 summarizes the benefits of using a Polyarc system. The Polyarc simplifies multicomponent quantitative analysis and enables high-sensitivity analysis of compounds that are poorly detected by FID. Note that for certain compounds, adsorption in the inlet or similar effects may prevent achieving a relative response equivalent to that of saturated hydrocarbons.<h3>3. Thermo Fisher Scientific: Targeted MS quantitation - Controlled and accessed from anywhere (Thermo Scientific™ Chromeleon™ 7.4 software)</h3><ul><li>Brochure</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/BR_70660_CDS_Chromeleon_BR_70660_EN_a0bf1ab440.pdf">Full PDF for download</a></li></ul><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/76">Thermo Scientific™ Chromeleon™ 7.4 software</a> is presented as a centralized, server-based data system designed to consolidate mass spectrometry laboratories by connecting instruments, users, and data within a single, scalable platform. It enables secure access to data and instruments from anywhere, while centrally managing methods, templates, and reports to streamline daily laboratory operations.The software is fully optimized for targeted MS quantitation workflows, offering native control of Thermo Scientific single and triple quadrupole as well as high-resolution accurate mass (HRAM) MS instruments. Advanced data processing tools support targeted quantitation, screening, intact mass deconvolution, MSⁿ library searching, and customizable reporting, making Chromeleon suitable for biopharma, environmental, and food safety applications.A strong emphasis is placed on compliance and data integrity. Chromeleon 7.4 supports GxP, ISO, and 21 CFR Part 11 requirements through granular user controls, audit trails, electronic signatures, and versioned results. Built-in network failure protection, centralized databases, and secure remote access ensure high availability, resilience, and scalability from small on-premise installations to multi-site or cloud deployments.The brochure also highlights Chromeleon’s role in advanced bioanalysis and environmental workflows, including intact protein characterization, multi-attribute methods (HR-MAM), PFAS analysis, pesticides, dioxins, and PCBs. Integration with complementary Thermo Scientific software further enables end-to-end workflows from compliant data acquisition to targeted processing, reporting, and long-term data management.

News from LabRulezGCMS Library - Week 03, 2026

Our Library never stops expanding. What are the most recent contributions to LabRulezLCMS Library in the week of 12th January 2026? Check out new documents from the field of liquid phase, especially HPLC and LC/MS techniques!<blockquote>👉 <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library">SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT LCMS AND RELATED TECHNIQUES</a></blockquote><blockquote>👉 Need info about different analytical techniques? Peek into <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library">LabRulezGCMS</a> or <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library">LabRulezICPMS</a> libraries.</blockquote>This week we bring you application notes by Agilent Technologies, Shimadzu, Waters Corporation and poster by Thermo Fisher Scientific / HPLC!<h3>1. Agilent Technologies: B Vitamin Analysis in Dietary Supplements on the Agilent 1290 Infinity III LC System</h3>Using ion-pairing reagent and supported by time‑saving automation of routine tasks using the Agilent InfinityLab Assist<ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_b_vitamin_dietary_supplements_1290_infinityiii_lc_5994_8826en_agilent_56b5eb2fb1.pdf">Full PDF for download</a></li></ul>There is a huge variety of (multi)vitamin supplements on the market, with different vitamin combinations and different concentrations available. To ensure that the claimed vitamin contents are met, analysis of those supplements is&nbsp;necessary.&nbsp;To ensure constant and good analytical performance, preparation of the analytical system is fundamental. There are different approaches to preparing the system for analysis. Purging the solvent lines from bottle to pump removes possible air bubbles, especially after longer breaks between instrument usage or changing eluent to the ion-pairing and buffer-containing eluent after the weekend. Equilibration can either be done by a calculated time (10–20 column volumes)1 , set as a fixed experimentally determined value, or manually monitored. Using a fixed time for equilibration can lead to unnecessary high solvent consumption, as equilibration may already be established and no monitoring was previously done. In contrast, manual monitoring of equilibration can be time-consuming and error-prone. For example, if there are no written rules regarding key points for equilibration of the column, its determination can be subjective (constant&nbsp;pressure and baseline of e.g. UV absorption).&nbsp;As vitamins are grouped according to their water solubility and not their chemical structure, separation behavior can greatly differ as they have different charges at physiological pH. In such cases, ion-pairing reagents such as hexane sulfonic acid can enable the separation of those vitamins while using a reversed phase column. As ion-pairing LC depends on good equilibration to ensure the presence of ion‑pairing reagent within the system, the process of preparing the instrument is an inevitable step. This is essential for good and reproducible analytical results.&nbsp;With the Agilent InfinityLab Assist, making your instrument ready is no longer a time-consuming and unpleasant procedure.1 This application note demonstrates the separation of multiple B vitamins in multivitamin tablets and effervescent tablets using an <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?search=1290+Infinity+III">Agilent 1290 Infinity III LC System</a>. Furthermore, it is shown how the InfinityLab Assist can help users ensure good chromatographic results, save time, and reduce errors by replacing manual tasks with InfinityLab Assist tasks.&nbsp;<h4>Experimental&nbsp;</h4><h5>Equipment&nbsp;</h5><ul><li>Agilent 1290 Infinity III High-Speed Pump (G7120A)&nbsp;</li><li>Agilent 1290 Infinity III Multisampler (G7167B) with Agilent InfinityLab Sample Thermostat (G4761A)&nbsp;</li><li>Agilent 1290 Infinity III Multicolumn Thermostat (G7116B) with Agilent InfinityLab Quick Connect Heat Exchanger (G7116-60015)&nbsp;</li><li>Agilent InfinityLab Level Sensing (G7175A)&nbsp;</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=10&amp;search=InfinityLab+Assist">Agilent InfinityLab Assist</a> (G7180A) with Agilent InfinityLab Assist Control Software, version 2.0&nbsp;</li><li>Agilent 1290 Infinity III Diode Array Detector (G7117B) with Agilent InfinityLab Max-Light Cartridge Cell (10 mm, 1.0 µL, G4212-60008)&nbsp;</li></ul><h5>Software&nbsp;</h5><ul><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=10&amp;search=OpenLab+CDS">Agilent OpenLab CDS,</a> version 2.8, update 7 (or later versions)&nbsp;</li></ul><h5>Column&nbsp;</h5><ul><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=10&amp;search=InfinityLab+Poroshell+120+EC-C18">Agilent InfinityLab Poroshell 120 EC-C18</a>, 2.1&nbsp;mm × 100 mm, 2.7 µm column (p/n 695775-902).</li></ul><h4>Results and discussion&nbsp;</h4><h5>Separation of vitamin B1, B2, B5, B9, and B12&nbsp;</h5>To analyze vitamin B1, B2, B5, B6, B7, B9, and B12 in vitamin supplements, different columns, mobile phases, and gradients were evaluated. The selected chromatographic conditions (Table 1) showed the best separation from peak to peak and additional matrix peaks. Hexane sulfonate was needed as an ion-pairing reagent to ensure good peak shapes, as all vitamins investigated, except vitamin B12, are expected to be charged based on their pKa values.3 The method detects the B vitamins investigated in vitamin tablets and effervescent tablets as demonstrated in Figure 1, showing chromatograms of aqueous standards and real samples. As some vitamins are present at higher doses, such as the 12 mg tablet (vitamin&nbsp;B5) compared to the 2.5 µg tablet (B12) in supplement 3 (Figure 1), parallel analysis is rather difficult, and not all vitamins present were detectable in each&nbsp;supplement.<h4>Conclusion&nbsp;</h4>Using the Agilent 1290 Infinity III LC System setup detection of vitamins B1, B2, B5, B6, B7, B9, and B12 in effervescent tablets and multivitamin supplement matrix, good separation was achieved. Using the Agilent InfinityLab Assist "Make&nbsp;Ready" task, the system was prepared for B vitamin analysis using only one automated task and no manual monitoring. Running this task automatically by scheduling saved more than 20 minutes of working time. Additionally, the time required for medium equilibration monitoring sensitivity was reduced by approximately six minutes, compared to manual equilibration. Furthermore, using the schedulable InfinityLab Assist "Standby" task, the risk of errors regarding instrument standby can be drastically reduced. User-defined settings enable adjustment for different purposes, such as switching of all modules except the sampler thermostat.2 The ability to remove the used buffer and ion-pairing reagent from the flow path for longer storage by scheduling a standby task also greatly helps to prevent salt precipitation in the system without additional effort. Also, the InfinityLab Assist can clearly help to accelerate checking the instrument status while preparing the instrument, as well as during running&nbsp;samples.2<h3>2. Shimadzu: Analysis of Ammonia as an Impurity in Fuel Cell Grade Hydrogen According to ISO 14687 Grade D Using a Gas Generator</h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_01_01070_en_43a535bf87.pdf">Full PDF for download</a></li></ul>Hydrogen is expected to be a new power and heat source to reduce greenhouse gas emissions. Hydrogen is an easily available substance that can be produced from the electrolysis of water in our daily lives. However, when used in fuel cells, it is necessary to control impurities in hydrogen gas because certain impurities introduced during the manufacturing process deteriorate the electrode and electrolyte membrane, reducing the performance of the fuel cell or shortening its life. When ammonia is used as a carrier of hydrogen gas due to its distribution as a chemical, there is a possibility that ammonia may be introduced into hydrogen. This article presents an example of analysis of ammonia in hydrogen using an ion chromatograph (IC) based on the standard values described in ISO 14687 Grade D.1)<h4>Analysis of Ammonium Ion by IC</h4>A <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=1&amp;search=HIC-NS">non-suppressor IC (HIC-NS)</a> was used to analyze NH4. Since the IC can selectively measure ions dissolved in the sample, it is less affected by contaminants than other methods and can measure NH4 with high accuracy. In addition, by using the same device together with a suppressor IC, it is possible to measure inorganic halogens and formic acid, which are other impurities listed in ISO 14687. Table 1 shows the analytical conditions for NH4, Fig. 2 shows the chromatogram of a standard sample at a concentration near the specified value (25 μg/L), and Fig. 3 shows the calibration curve in the range from 2.5 μg/L to 200 μg/L. As shown in Fig. 3, the linearity was greater than 0.9999. Table 2 shows the reproducibility of the sample at 10 μg/L, which is around 1/2 of the specified concentration, repeated 7 times.<h4>Conclusion</h4>Ammonia, an impurity in hydrogen, was analyzed using a nonsuppressor IC, and it was confirmed that the method met the standard value specified by ISO 14687 Grade D. In addition, when ammonia standard gas near the standard value was mixed into hydrogen using a gas generator, a good recovery rate was obtained, which confirmed the validity of the method including the collection flow of pretreatment.<h3>3. Thermo Fisher Scientific / HPLC: High-sensitive multi-attribute analysis of ADCs under native conditions by using an online multiple heart-cut 2D-LC-HRAM mass spectrometry system</h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/po_high_sensitive_multi_attribute_analysis_adcs_native_conditions_po_en_28e7e0b002.pdf">Full PDF for download</a></li></ul>ADCs are a rapidly expanding class of biotherapeutics for cancer treatment. Critical quality attributes such as charge heterogeneity, DAR, and drug distribution are essential for ensuring the safety, stability, and efficacy of ADCs. Strong cation exchange (SCX) and hydrophobic interaction chromatography (HIC) are conventional methods employed for charge variant analysis and DAR determination of ADCs1. However, these methods frequently utilize MS-incompatible salts, limiting their use for MS characterization. Online 2D-LC addresses this by enabling desalting in the second dimension(2D) and offering multi-attribute analysis in one method. Here, multiple heart-cut 2D-LC-HRAM MS methods were developed to achieve high sensitivity for the multi-attribute analysis of polatuzumab vedotin under native conditions.<h4>Methods</h4>A <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/742">Thermo Scientific Vanquish 2D UHPLC system</a>, coupled with a <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/402">Thermo Scientific Orbitrap Exploris 240 mass spectrometer</a> with Biopharma option, were utilized to configure the multiple heart-cut 2D-LC-HRAM MS system. HIC-SEC and SCXSEC methods were developed and optimized for the charge variants, drug-to-antibody ratio (DAR) and drug load distribution (DLD) characterization of ADCs under native conditions.<h4>Conclusions&nbsp;</h4>In this study, an online multiple heart-cut 2D-LC-HRAM MS system was configured and optimized for the multi-attribute analysis of polatuzumab vedotin. This approach provides detailed and comprehensive insights into the charge heterogeneity analysis, DAR, and DLD analysis of polatuzumab vedotin under native conditions.&nbsp;<ul><li>The online multiple heart-cut 2D-LC system enables the direct transfer of SCX and HIC fractions to mass spectrometry analysis by utilizing SEC as a desalting step, thereby overcoming the MS-incompatibility buffer in the LC separation.&nbsp;</li><li>The backflush transfer of fractions was employed to enhance peak shape and sensitivity in the 2D SEC separation.&nbsp;</li><li>The 2D SEC-MS analysis enables the characterization of ADCs under native conditions.&nbsp;</li><li>The high sensitivity of the Orbitrap Exploris 240 MS allows for the identification of fractions with low abundance in the 1D chromatography</li></ul><h3>4. Waters Corporation: Automated Multiple Reaction Monitoring (MRM) Method Development for Peptide Drugs Using waters_connect for Quantitation Software</h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/720009123_en_1f51e50be8.pdf">Full PDF for download</a></li></ul><h5>Benefits&nbsp;</h5><ul><li>Rapid evaluation and optimization of MRM conditions freeing up bioanalysts to perform other valuable tasks</li><li>Interactive graphical review of results facilitating informed decision making.&nbsp;</li><li>Elimination of transcription errors via direct transfer of MRM results to the LC-MS method editor.</li></ul>LC-MS/MS is the technology of choice for the quantification of drugs, metabolites, and biomarkers in biofluids, typically employing tandem quadrupole mass spectrometry (MS) with detection via MRM. MRM method development for classic small molecule drugs involves the selection of the best precursor and product ion followed by optimization of cone voltages and collision energies. This is achieved by infusion or LC injection of the analyte(s) of interest. For small molecule drug compounds, this process is usually straightforward and lends itself to automation as they largely generate singly charged ions. However, in electrospray mass spectrometry, biomolecules such as peptides, oligonucleotides, and proteins normally form several multiply charged precursor ions, e.g., M+3H3+, M+4H4+. This significantly complicates MRM method development, as each charge state can generate multiple fragment ions, all of which need to be compared both within and across each charge state to choose the best transition or transitions for analyte measurement.&nbsp;The MRM Optimization tool with the waters_connect for Quantification Software has been specifically designed to address the challenge of MRM method development for multiply charged biomolecules. The Optimization tool facilitates the automatic acquisition of data from multiple precursor and product ion and collision energy combinations across several charge states, with the results reviewed via an interactive graphical interface. Here, the use of this optimization is illustrated, using the GLP-1 peptide, semaglutide, as an example.<h4>Experimental</h4><h5>Mass Spectrometry</h5>Mass spectrometry was performed on a <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/2100">Waters Xevo™ TQ Absolute XR Mass Spectrometer</a>, operated in positive ion electrospray ionization mode (ESI). Nitrogen was used as the nebulizer gas and argon as the collision gas. The cone voltage, collision energy, and MS/MS transitions were adjusted and evaluated using the waters_connect MRM Optimization tool.<h5>Informatics&nbsp;</h5>The mass spectrometer was controlled and resulting data evaluated using <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/1544">waters_connect for Quantitation</a> Application Manager version 1.9.<h4>Conclusion&nbsp;</h4>The number of candidate biomolecule drugs, peptides, oligonucleotides, and proteins in pharmaceutical discovery and development is steadily increasing. These biomolecules require the development of quantitative LC-MS/MS assays to support discovery, preclinical, and human DMPK studies. Unlike small molecules, these biomolecules form multiply charged ions in the MS source, making MRM method development more challenging, as multiple charge state–product ion combinations must be evaluated and compared. The Optimization tool in waters_connect for Quantitation Software provides an automated, fast platform for the optimization and evaluation of the precursor ion → product ion pairs formed at each charge state, simplifying the process of LCMS/MS method development for biomolecules.

News from LabRulezLCMS Library - Week 03, 2026

Our Library never stops expanding. What are the most recent contributions to LabRulezICPMS Library in the week of 12th January 2026? Check out new documents from the field of spectroscopy/spectrometry and related techniques!<blockquote>👉 <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library">SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT SPECTROSCOPY/SPECTROMETRY RELATED TECHNIQUES</a></blockquote><blockquote>👉 Need info about different analytical techniques? Peek into <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library">LabRulezLCMS</a> or <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library">LabRulezGCMS</a> libraries.</blockquote>This week we bring you application notes by Agilent Technologies, Shimadzu, and Waters Corporation and brochure by Thermo Fisher Scientific!<h3>1. Agilent Technologies: Detecting Spice Adulteration with the <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library?mainauthorItems=10&amp;search=8700+LDIR">Agilent 8700 LDIR</a> Chemical Imaging System</h3>Accelerating adulterant detection in turmeric with IR spectroscopy and imaging&nbsp;<ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_spice_adulteration_8700_ldir_5994_8800en_agilent_235b48c7e6.pdf">Full PDF for download</a></li></ul>Spices are essential components of culinary practices worldwide, valued for their flavor, aroma, and health benefits. However, the intentional or accidental adulteration of spices with cheaper or foreign substances poses significant risks to both food quality and consumer safety. Adulteration practices often aim to increase product volume, enhance visual appeal, or mimic authentic flavors, compromising the integrity of the final product.1Common adulteration practices include substituting genuine plant materials with cheaper or visually similar ones, using inferior plant species or parts, and mixing with fillers such as corn starch, bran, or sawdust. Some products are also adulterated with chemicals to enhance flavor, inorganic substances such as sand, chalk, or red brick powder, or illegal dyes such as Sudan dyes and rhodamine B to intensify&nbsp;color.1–4&nbsp;Current tools for detecting adulteration in herbs and spices face several challenges. Sampling across complex supply chains often lacks consistency, making it difficult to obtain representative samples.5 The chemical and physical complexity of sample matrices, combined with natural variation among species and origins, complicates data interpretation.5&nbsp;In&nbsp;ground or powdered spices, the original plant structures are lost, making it difficult to visually or morphologically identify adulterants, particularly when they are fine or physically similar to the genuine&nbsp;material.6 An <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library?mainauthorItems=10&amp;search=8700+LDIR">Agilent 8700 Laser Direct Infrared (LDIR) chemical imaging system</a> (Figure&nbsp;1) was used in this study to detect spice adulteration through the integration of infrared spectroscopy and&nbsp;microscopy<h4>Experimental&nbsp;</h4>Agilent Clarity software: To evaluate the 8700 LDIR's capability in distinguishing genuine spices from common adulterants, a series of pure and adulterated samples were prepared and analyzed using the system's automated Particle Analysis (PA) workflow.<h4>Results and discussion&nbsp;</h4><h5>Identification of pure spices (turmeric)&nbsp;</h5>To verify the 8700 LDIR and the user&nbsp;generated library in identifying particles of varying sizes, shapes, and counts, the pure turmeric sample was analyzed as an "unknown". Turmeric sample identification demonstrated high spectral matching accuracy. Within the selected analysis area, 74&nbsp;particles were detected and 70&nbsp;particles (94.6%) were matched to the turmeric reference spectra in the custom library. Notably, 64 particles achieved Hit Quality Index (HQI) values exceeding 0.8, indicating strong spectral correlation and high confidence in the identification data (Figure 2).<h4>Conclusion&nbsp;</h4>This study demonstrates the suitability of the Agilent 8700 LDIR chemical imaging system with Agilent Clarity software as an effective tool for detecting adulteration in ground spices. Using the automated Particle Analysis (PA) workflow, the system quickly and reliably distinguished turmeric from both organic (corn starch) and inorganic (sand) adulterants based on their distinct IR spectral signatures.&nbsp;Differentiating between chemically similar spices remains challenging due to overlapping IR profiles. However, the 8700 LDIR system's ability to build custom spectral libraries offers flexibility for targeted authentication, allowing laboratories to adapt the system to their evolving analytical needs.&nbsp;A key advantage of the 8700 LDIR method is the speed and simplicity of sample preparation—dry powders can be analyzed directly on low-e slides without solvents or extraction. By combining the high-throughput automated PA workflow with integrated imaging, the 8700 LDIR provides a practical, time-saving solution for routine analysis in food testing&nbsp;laboratories.<h3>2. Shimadzu: Observation of the Automotive Cylindrical Lithium-Ion Battery “4680” Using a Micro-Focus X-ray CT System</h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_01_01060_en_5e744626ad.pdf">Full PDF for download</a></li></ul><h4>User Benefits</h4><ul><li>The internal structure of the “4680” cylindrical lithium-ion battery for automotive use, which is a market trend, can be observed nondestructively.&nbsp;</li><li>Electrode placement and bonding condition can be verified, which is useful for product quality inspection.</li></ul>In recent years, with the proliferation of electric vehicles (EVs), the development of high-performance, low-cost automotive batteries has become an urgent priority. Among these, the cylindrical lithium-ion battery “4680” has attracted particular attention. Compared with the conventional “2170,” the “4680” is larger, and its energy density per cell is increased, thereby extending vehicle range. In addition, the adoption of a tab-less structure reduces internal resistance, improving charge/discharge efficiency and thermal management performance, while simplification of the manufacturing process is expected to reduce cost. Owing to these characteristics, the “4680” is drawing attention across both industry and academia as a core technology for next-generation EVs. Meanwhile, lithium-ion batteries are always subject to concerns about the risk of ignition and explosion due to internal short circuits or foreign matter inclusion. Because X-ray CT enables nondestructive testing (NDT) with three-dimensional visualization of internal structures, it is possible to detect fine defects such as electrode misalignment, separator damage, and foreign matter inclusion.&nbsp;This article introduces a case study in which the cylindrical lithium-ion battery “4680” for automotive applications was observed using the microfocus <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library?mainauthorItems=1&amp;search=inspeXio+7000">X-ray CT system inspeXio 7000</a> (Fig. 1).<h4>Conclusion</h4>We presented a case study of imaging the cylindrical lithium-ion battery “4680” using a microfocus X-ray CT system. By nondestructively visualizing its three-dimensional structure, it is possible to obtain important information on the battery’s internal structure, such as the arrangement of electrodes and their bonding state. Thus, X-ray CT is shown to be a powerful tool that contributesto the advancement of battery technology.<h3>3. Thermo Fisher Scientific: MarqMetrix All-In-One X Process Raman Analyzer</h3>Enabling accurate, real-time results for process monitoring in hazardous locations<ul><li>Brochure</li><li><a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/labrulez-bucket-strapi-h3hsga3/marqmetrix_all_in_one_x_process_raman_analyzer_ds1339_en_c1739807d2.pdf">Full PDF for download</a></li></ul>The <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/products/2208">Thermo Scientific™ MarqMetrix™ All-In-One X Process Raman Analyzer </a>is a compact, portable spectrometer designed for fast deployment and ease of use. Built for industries where rapid time-to-results is critical, it is designed to be intrinsically and inherently safe for operation within hazardous locations, in such applications as:&nbsp;<ul><li>Midstream and downstream oil &amp; gas operations&nbsp;</li><li>Chemical and polymer applications&nbsp;</li><li>Pharmaceutical development and manufacturing</li></ul><h4>The MarqMetrix All-In-One X Analyzer offers multiple operational advantages:&nbsp;</h4><ul><li>Analysis without sample preparation, delivering Raman spectral results in real time&nbsp;</li><li>Easy setup and deployment by non-spectroscopists&nbsp;</li><li>Intrinsically and inherently safe optical power to robust probes, which can be deployed in hazardous locations: up to ATEX Zone 0 (Europe &amp; Middle East), IECEx (Asia), and Class 1 Div 1 (North America)&nbsp;</li><li>Nondestructive workflows to protect precious samples&nbsp;</li><li>A small footprint for convenient deployment&nbsp;</li><li>Factory calibration for hardware stability and portability&nbsp;</li></ul>The MarqMetrix All-In-One X Process Raman Analyzer is designed for out-of-the-box use, enabling you to be ready in less than 15 minutes to collect highly accurate Raman measurements. Pack this analyzer in a protective case and take it to the point of need; its factory calibration ensures continuous and precise analysis on the go. Easily integrate the MarqMetrix All-In-One X Process Raman Analyzer into your existing process without the need for costly technical expertise. Once implemented, the analyzer enables operators in hazardous locations to make faster, safer, and smarter decisions by delivering real-time compositional insights directly on site.<h3>4. Waters Corporation: Residual Dynabeads Detection with <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/products/2190">Aura+</a></h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/labrulez-bucket-strapi-h3hsga3/720009096_en_aeb7e4288f.pdf">Full PDF for download</a></li></ul>Autologous cell therapies have seen explosive growth as evidenced by the recent landmark FDA approvals of two CAR-T cell therapies, Yescarta® and Kymriah®. 1 Dynabeads™ are commonly used in cell therapy manufacturing process to expand and activate CAR-T cells.2 CD3/CD28 Dynabeads specifically are one of the leading approved GMP expression beads for T cell therapies and are key to achieving the potency required of these novel medicines. Dynabeads are also efficiently removed from the final product to ensure final purity. However, residual CD3/CD28 beads present a significant risk patients’ safety and therefore are generally kept below a widely accepted but not yet regulatory controlled limit of 100 residual beads per 3,000,000 cells.3–4&nbsp;Residual bead analysis is currently performed with manual hemocytometry that uses light microscopy and manual counting. However, manual hemocytometry is prone to human error, which leads to significant bead undercounting because it is incredibly difficult to find and differentiate between Dynabeads and cells in a sample, making residual bead counting one of the most challenging cell therapy lot release assays. Other traditional cell and subvisible analysis tools, including flow cytometers, also undercount beads and cannot differentiate residual Dynabeads from cells and other subvisible particles.&nbsp;In this technical note, we show step-by-step how Aura CL and <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/products/2190">Aura+</a> enable fast, accurate, sensitive, and specific residual Dynabead detection in a concentrated cell therapy product. Powered by backgrounded membrane imaging (BMI) to characterize the entire cell therapy particle population and side illumination membrane imaging (SIMI) to specifically detect Dynabeads, Aura® CL and Aura®+ are the first and only tailored solutions to find and count these hard to detect contaminants.<h4>Conclusion&nbsp;</h4>Analysis of the cell therapy sample on Aura CL or Aura+ begins with the BMI well image, where sharp contrast, high resolution optics provide the landscape to count and size all the particles in your cell therapy product. SIMI imaging, which is run at the same time as BMI, enables the differentiation of biologic vs. non-biologic particles which is essential to this application. Figures 2 and 3 capture how BMI detects all particles present in a cell therapy sample, while SIMI mode selects for particles of higher refractive index contrast. In BMI mode, cells, Dynabeads, and mixtures of the two were all easily visible. However, in SIMI mode, only the residual Dynabeads were detected both in the standard high-throughput 4x mode and in the 10x high magnification mode. This is essential for specific detection of residual Dynabeads given their low abundance in a highly concentrated cell sample as shown in Figure 4. We determined that the limit of quantitation (LOQ) of Dynabeads is &lt;1 bead/well (or 18 beads/mL of sample), well below the hemacytometer residual bead detection rate of 1 bead per 10,000 cells. Additionally, the bead counts in our dilution series exhibited a linear relationship, measuring an R2 of 0.98. Using Aura CL or Aura+ for residual Dynabead detection provides greater accuracy and higher-throughput in counting compared to the cumbersome and error prone currently used methods. Resolving false positive counts can be easily rectified by measuring the particles at higher magnification, where single Dynabeads identity can be confirmed by size. Aura CL and Aura+ deliver the only automated way of measuring single Dynabeads in concentrated cell therapy solutions, while also offering built in orthogonal confirmation through various objectives and light sources.

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