Enhancing Paper’s Mechanical Strength and Antibacterial Properties through a Biopolymer-Based Coating

<p><strong>Our Library never stops expanding. What are the most recent contributions to LabRulezGCMS Library in the week of 22nd September 2025? Check out new documents from the field of the gas phase, especially GC and GC/MS techniques!</strong></p><blockquote><p><span style="font-size:20px;">👉 </span><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library"><span style="font-size:20px;"><strong>SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT GCMS AND RELATED TECHNIQUES</strong></span></a></p></blockquote><blockquote><p><strong>👉 Need info about different analytical techniques?</strong> Peek into <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library"><strong>LabRulezLCMS</strong></a> or <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library"><strong>LabRulezICPMS</strong></a> libraries.</p></blockquote><p>This week we bring you application notes by <strong>Agilent Technologies, EST Analytical, Shimadzu </strong>and <strong>Thermo Fisher Scientific!</strong></p><h3><strong>1. Agilent Technologies: A Chemometric Approach for Ambient Air Monitoring Using Thermal Desorption GC/MS</strong></h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_voc_8890_chemometric_ambient_air_monitoring_5994_8451en_agilent_fef7d171bb.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Monitoring VOCs is crucial for assessing air quality in industrial and urban settings. These compounds, which include propene, hexachlorobutadiene, and naphthalene, vary in volatility and encompass both polar and nonpolar chemicals. Recognizing the importance of standardized monitoring, the Bureau of Indian Standards (BIS) has developed specific methodologies for these compounds under the IS 5182 series.&nbsp;</p><p>IS 5182-27 focuses on the measurement of vapor-phase organic chemicals such as vinyl chloride and nC22 hydrocarbons in air and gaseous emissions. This method employs diffusive (passive) sampling onto sorbent tubes or cartridges, followed by TD (see Figure 1) and capillary GC analysis. The passive sampling approach offers advantages in terms of ease of deployment and cost-effectiveness, making it suitable for widespread monitoring applications.</p><p>To reveal relevant patterns and sources of variation in these large environmental datasets according to the IS-5182 guidance, this application note proposes chemometric analysis using the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=6&amp;search=TD100-xr"><strong>Markes TD100-xr automated thermal desorber</strong></a> (Figure 2) and the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=8890+gc"><strong>Agilent 8890 GC system</strong></a> with <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=5977c"><strong>5977C GC/MSD</strong></a> (Figure 3). Chemometrics is a discipline that uses mathematics, statistics, and formal logic to design or select optimal experimental procedures. Chemometric techniques commonly used for clustering are the hierarchical agglomerative cluster analysis and PCA with factor analysis.</p><h4><strong>Conclusion&nbsp;</strong></h4><p>This application note highlights the comparison of different air sampling strategies and shows their effect on qualitative and quantitative analysis of VOCs. Active (pumped) sampling helped with faster analysis, which is required for controlled and sensitive real-time monitoring of ambient air. Chromatograms of air sampled at various locations showed the presence of VOCs such as benzene, toluene, ethyl benzene, and xylenes. Many common and unique compounds were found at each location. The intensity of these compounds showed variations at different locations. Fewer compounds with lower intensities were observed in air samples from a residential area, whereas more compounds with higher intensities were observed in air samples from a traffic area.&nbsp;</p><p>Passive sampling was a comparatively cost‑effective and long-term approach and provided consistent replicate results. The chromatographic overlays of different sampling times indicated an increasing trend in peak intensities with respect to time. There was a considerable rise in peak intensities for the 1-week sampling period, as compared to 24-hour sampling. There was a slight rise in peak intensities for the 2-week sampling period, as compared to 1-week sampling. The PCA plot suggested the peak distribution obtained in each dataset. One-week sampling results showed consistent replicate results. Use of the chemometrics software Agilent Mass Profiler Professional added value by providing data visualization for interpretation.</p><h3><strong>2. EST Analytical: USEPA 524.2 Method Validation Using the Evolution Purge and Trap Concentrator and the Centurion WS Autosampler</strong></h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/Purge_and_Trap_524_2_Application_Note_2d327854f2.pdf"><strong>Full PDF for download</strong></a></li></ul><p>USEPA Method 524.2 calls for purge and trap sampling coupled with a Gas Chromatograph (GC) and Mass Spectrometer (MS) for separation and analysis. It has an extensive list of compounds and requires lower detection limits due to its use in drinking water testing. A 20% relative standard deviation for compound response factors is required across the calibration curve while the calibration check standard analytes have to be within 30% of the expected concentration.&nbsp;</p><p>Currently, this method calls for a 5mL or 25mL purge volume and a four minute desorb time. These method requirements can pose a challenge for the analyst due to the amount of moisture that is created. The negative effects of the increased water vapor include instability of the chromatography, band eluting and poor peak shape to name a few. A side effect of this instability is sample re-runs and lost laboratory productivity. In addition, a common practice for mitigating moisture is increasing the GC inlet split rate. This poses yet another difficulty as the increased split rate can result in reduced sensitivity. EST Analytical’s eight port valve in the Evolution purge and trap concentrator aids in limiting the water exposure because the water management of the system is not part of the desorb pathway. This feature also enables laboratories to use a smaller split ratio at the GC inlet thus increasing sensitivity.</p><h4><strong>Experimental</strong></h4><p>The sampling system used for this study was the<a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/2160"><strong> EST Analytical Evolution purge and trap concentrator </strong></a>and the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/2159"><strong>Centurion WS autosampler</strong></a>. The concentrator was affixed with a Vocarb 3000 trap and connected to an <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=1&amp;search=7890A"><strong>Agilent 7890A GC</strong></a> and <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=1&amp;search=5975C"><strong>5975C inert XL MS</strong></a>. The GC was configured with a <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=9&amp;search=Rxi-624+Sil+MS"><strong>Restek Rxi-624 Sil</strong></a> MS 30m x 0.25mm x 1.4µm column. Sampling parameters are listed in Table 1 while Table 2 enumerates the GC/MS parameters.</p><h4><strong>Conclusions</strong></h4><p>This study demonstrated the effectiveness of the Evolution/Centurion purge and trap sampling system. The results passed all of the USEPA Method 524.2 criteria for both linearity and detection limits. Since the Evolution bypasses the water management trap during the four minute desorb process, the amount of water effecting the experiments was limited. Furthermore, the forty to one split ratio at the GC inlet provided excellent detection limits as the system was more sensitive to the low level standard requirements of the method. The lower split rate has an added benefit of reducing laboratory helium consumption when setting it against other system’s higher split ratios. Finally, the precision and percent recovery results showed the reliability of the system in producing accurate experimental findings.</p><h3><strong>3. Shimadzu: Dual-Column Analysis of Blood AlcoholContent (BAC) Using Nitrogen Carrier Gas with </strong><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=1&amp;search=Brevis+GC-2050"><strong>Brevis GC-2050</strong></a></h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_01_00899_en_af0d9bafe7.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Analysis of blood alcohol content (BAC) and other volatile organic compounds (VOCs) is essential for law enforcement agencies to determine alcohol intoxication and its role in traffic accidents, assaults, and injuries, as well as to identify the causes of certain criminal behaviors, poisonings, and so on.&nbsp;</p><p>Typically, this analysis is performed by a gas chromatograph (GC) that is combined with a headspace sampler (HS) and a flame ionization detector (FID). Since accurate results are essential with BAC analysis, 2 columns can be used with different separation characteristics so that cross-checking can be performed. By using an integrated HS-GC system equipped with 2 FIDs connecting to a dual-column configuration, crosschecking can be performed in a single analysis. In this system, the columns are directly connected to the transfer line using a 2-hole ferrule, which minimizes sample losses due to adsorption.&nbsp;</p><p>In addition to the high-end <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=1&amp;search=Nexis+GC-2030"><strong>Nexis GC-2030</strong></a>, Shimadzu also offers the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=1&amp;search=Brevis+GC-2050"><strong>Brevis GC-2050</strong></a> as a compact gas chromatography solution, and in this Application News, it is used with an <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=1&amp;search=HS-20+NX+headspace+sampler"><strong>HS-20 NX headspace sampler </strong></a>(Fig. 1) to perform BAC analysis. Hydrogen was used as the carrier gas in a similar experiment in Application News 01-00570, but in this experiment, nitrogen was used because it is a cheaper alternative carrier gas. Nitrogen generally has an adverse effect on separation, so this experiment also investigated the conditions for separation for 10 types of blood VOCs.</p><h4><strong>Separation of 10 Blood VOCs&nbsp;</strong></h4><p>A solution of 10 VOCs spiked with blood (0.1 mg/mL) was analyzed to determine the separation of methanol, acetaldehyde, ethanol, isopropyl alcohol, acetonitrile, acetone, tert-butanol, 1-propanol, methyl ethyl ketone, and ethyl acetate. The resulting chromatogram is shown in Fig. 6. All peaks were detected within 6.0 minutes in the BAC PLUS1 column and within 3.5 minutes in the BAC PLUS2 column, indicating good separation. The elution sequence of the 10 blood VOCs differed significantly between the columns, which enhanced the system’s qualitative capability. Table 4 shows the retention time of each compound and the repeatability (n=5) of the peak area ratio for the tert-butanol internal standard.</p><h4><strong>Conclusion&nbsp;</strong></h4><p>This experiment involved dual-column analysis of blood alcohol content (BAC) by the compact Brevis GC-2050 and the HS-20 NX. Dual-column configuration enables cross-checking in a single analysis. In addition, nitrogen was used as the carrier gas instead of helium. While hydrogen enables high-speed analysis, it also requires careful handling, so from the perspective of safety, installation of various optional tools such as hydrogen sensor and stop valve have been recommended. Nitrogen gas is relatively inexpensive and easy to handle, and this experiment demonstrated that it also provides reliable results while maintaining good separation.</p><h3><strong>4. Thermo Fisher Scientific: Routine analysis of 7N high purity gallium phosphide by Glow Discharge Mass Spectrometry</strong></h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_003578_ioms_gd_ms_element_gd_plus_gallium_an003578_em_en_1666255eb4.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Gallium phosphide (GaP) is a semiconductor material used in electronic and optoelectronic devices, including light-emitting Diodes (LEDs), solar cells as well as high-frequency and high-power electronics<sup>1-5</sup>. GaP wafers offer several advances over traditional silicon wafers, including high efficiency, high-speed operation, and highpower handling capabilities<sup>4-5</sup>.&nbsp;</p><p>This application note describes the direct analysis of impurities in high purity gallium phosphide with sub-ppb detection limits using the Thermo Scientific <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/products/1690"><strong>Element GD PLUS GD Mass Spectrometer</strong></a>.&nbsp;</p><h4><strong>Experiment&nbsp;</strong></h4><p>The flat samples are analyzed directly, with no digestion required. Instrumental conditions for the analysis with the Element GD PLUS GD-MS are shown in Table 1. Potential sample surface contaminations were removed by short presputtering within the instrument.&nbsp;</p><h4><strong>Method development&nbsp;</strong></h4><p>The developed method ensures a reliable separation of interferences from the analyte ions. The interferences PO, POH and GaGa could potentially lead to falsely high Ti, Ba and Ce results. The formation of these interferences is low in the fast-flow source of the Element GD PLUS GD-MS: 69Ga69Ga/69Ga ≈ 1 ppm and ( 31P16O1 H + 31P17O)/31P ≈ 10 ppm. They can easily be resolved at Medium Mass Resolution (R = M / Δm = 4000). This is visualized in the mass scans shown in Figures 1 and 2 with much wider mass windows than later being used for quantification. Therefore, the Medium Mass Resolution of the Element GD PLUS GD-MS enables interference free measurements of Ti, Ba and Ce in GaP matrix.</p><h4><strong>Conclusions&nbsp;</strong></h4><p>Trace contaminations in 7N high purity gallium phosphide can be determined reliably and routinely with the Element GD PLUS GD-MS without prior digestion.&nbsp;</p><p>While most analytes like Ti, Ba and La are resolved from interferences in medium mass resolution (R = 4000), high mass resolution (R = 10000) is required for Ag because of the GaAr interference. Sub-ppb detection limits, even for elements like Sb and Ge, are achieved by neglectable formation of triatomic interferences and reduced abundance sensitivity. That is enabled by the fast-flow source design and the reverse Nier-Johnson geometry.</p><p>Semiquantitative quantification of element concentrations can be performed without standard reference materials using the standard RSF factor approach. The high sensitivity of the instrument, the reliable separation of interferences in medium and high mass resolution, the outstanding peak stability, the low formation of interferences and the low abundance sensitivity enable limits of detection of 0.05 to 1 ppb for most elements.&nbsp;</p><p>The sum of all impurities in the GaP sample was below 50 ppb, implying that a purity of 7N GaP can be assessed with the instrument.</p>

News from LabRulezGCMS Library - Week 39, 2025

<p><strong>Our Library never stops expanding. What are the most recent contributions to LabRulezLCMS Library in the week of 22nd September 2025? Check out new documents from the field of liquid phase, especially HPLC and LC/MS techniques!</strong></p><blockquote><p><span style="font-size:20px;">👉 </span><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library"><span style="font-size:20px;"><strong>SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT LCMS AND RELATED TECHNIQUES</strong></span></a></p></blockquote><blockquote><p><strong>👉 Need info about different analytical techniques?</strong> Peek into <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library"><strong>LabRulezGCMS</strong></a> or <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library"><strong>LabRulezICPMS</strong></a> libraries.</p></blockquote><p>This week we bring you application notes by <strong>Agilent Technologies, Shimadzu </strong>and <strong>Waters Corporation </strong>and<strong> </strong>poster by <strong>Thermo Fisher Scientific / HPLC Symposium!</strong></p><h3><strong>1. Agilent Technologies: Quantitation of N-Nitroso Nebivolol in Nebivolol Tablet Formulation</strong></h3><p><strong>Using an </strong><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=10&amp;search=6495D+triple+quadrupole"><strong>Agilent 6495D triple quadrupole LC/MS system</strong></a></p><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_nebivolol_tablet_formulation_6495_qqq_lc_ms_system_5994_8053en_agilent_e7f21eb12f.pdf"><strong>Full PDF for download</strong></a></li></ul><p>N-Nitroso Nebivolol is a NDSRI of Nebivolol, a beta-1 adrenergic receptor antagonist commonly used in the treatment of hypertension and heart failure. In the carcinogenic potency categorization published by the FDA, N-Nitroso Nebivolol has been categorized as Class 4, indicating the maximum allowable intake limit for the impurity to be 1,500 ng/day. Nebivolol has maximum daily dosage limit of 40&nbsp;mg for adults.</p><p>Considering a maximum daily dose of 40&nbsp;mg and allowable intake of 1,500&nbsp;ng/day for the nitrosamine impurity in the formulation under study, the specification limit of N-Nitroso Nebivolol has been calculated as 22.5 ng/mL for the 0.6 mg/mL test concentration used during this study.&nbsp;</p><p>This application note demonstrates a highly specific, sensitive, and reproducible method for the quantitation of N-Nitroso Nebivolol in a 20 mg Nebivolol tablet formulation. The method uses a 1290 Infinity II LC coupled to a 6495D triple quadrupole LC/MS/MS. The multiple reaction monitoring (MRM) conditions and ion source parameters were automatically optimized using the optimizer tool available with MassHunter Acquisition software to maximize the sensitivity of the target analyte. The API peaks were diverted to waste with the help of an integrated, software-controlled diverter valve during quantitation of the&nbsp;impurity.</p><h4><strong>Experimental</strong></h4><h5><strong>Equipment&nbsp;</strong></h5><p>The analysis was performed on a <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=10&amp;search=1290+Infinity+II+LC"><strong>1290 Infinity II LC system</strong></a> coupled to a <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=10&amp;search=6495D+triple+quadrupole"><strong>6495D triple quadrupole LC/MS/ MS</strong></a>. The LC system was equipped with the following&nbsp;modules: – Agilent 1290 Infinity II high-speed pump (G7120A) – Agilent 1290 Infinity II multisampler (G7167B) – Agilent 1290 Infinity II multicolumn thermostat (G7116B) – Agilent 1290 Infinity II diode array detector (G7117A)</p><h4><strong>Conclusion&nbsp;</strong></h4><p>A highly sensitive and robust MRM method was developed for the quantitation of N-Nitroso Nebivolol in 20&nbsp;mg Nebivolol tablet formulation using an Agilent 6495D triple quadrupole LC/MS system. The chromatographic method developed provided good separation between the analyte and the API. The method showed LOD and LOQ of 2 and 5 pg/mL, respectively. The minimum signal-to-noise ratio at the LOQ level was found to be more than 50:1 (Peak to Peak). The calibration curve from 5 pg/mL to 50&nbsp;ng/mL was found to be linear, with 1/x weighting. R and R2 values were 0.999 and 0.997, respectively. Spike recovery analysis showed the efficiency of sample extraction with a recovery percentage of 116.8% in API, 108.3% in placebo, and 111.8% in tablet formulation at the spiking level of 200 pg/mL. The method was found to be highly reproducible at the LOQ level, while the %RSD value for the area response of seven replicate injections was approximately 3.1%.</p><h3><strong>2. Shimadzu: Efficient Method Development for Synthetic Peptide and Related Impurities</strong></h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_01_00780_en_4d0aa014ea.pdf"><strong>Full PDF for download</strong></a></li></ul><h5><strong>User Benefits</strong></h5><ul><li>LabSolutions MD improves the efficiency of the entire workflow for method development of synthetic peptide and impurities.&nbsp;</li><li>Screening for multiple mobile phases and columns can be automated using mobile phase and column switching valves.&nbsp;</li><li>Molecular weights of peptides and related impurities can be estimated and accurately tracked with LCMS-2050, a single quadrupole mass spectrometer.</li></ul><p>Peptide therapeutics, characterized by specific amino acid sequences crucial to their function, can be synthesized chemically, similar to small molecule drugs. The production of synthetic peptides involves multiple steps, including deprotection, activation, coupling, and the cleavage of the final sequence from the solid support. Impurities, such as those resulting from premature chain termination or missing amino acids, can affect the safety and efficacy of the final product. Therefore, these impurities must be separated by liquid chromatography (LC). In LC analysis, selecting the appropriate mobile phase and column across a wide range of combinations is critical for achieving optimal separation, as it significantly impacts the separation. However, since the separation pattern varies depending on the peptide chain lengths, amino acid compositions, and presence of modifications, optimizing separation for each peptide sequence is time-intensive. This study describes how to efficiently find the best separation conditions for peptides and related impurities utilizing LabSolutions MD, a dedicated software for supporting method development, through both screening and optimization phases.</p><h4><strong>Experimental</strong></h4><ul><li><strong>LC System: </strong><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=1&amp;search=Nexera+X3"><strong>Nexera X3</strong></a> (Method Scouting System)</li><li><strong>MS System: </strong><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=1&amp;search=LCMS-2050"><strong>LCMS-2050</strong></a></li></ul><h4><strong>Automated Peak Tracking by LCMS-2050&nbsp;</strong></h4><p>LC chromatograms obtained with a gradient time of 5 min, flow rate of 0.6 mL/min, and initial concentration of 5 % and 15 %, along with molecular weights for FLP and impurities, are shown in Fig. 18. The UV spectra for each impurity are displayed in Fig. 19. The similarity between UV spectra of Met(O2), p.A1del, p.A1_E2del, p.A1_K3del, and p.A1_D5del is greater than 0.99, suggesting that peak tracking based on UV spectra would be challenging. In contrast, LabSolutions MD enables peak tracking based on molecular weights acquired by LCMS-2050, facilitating accurate identification of compounds with similar UV spectra (Fig. 18). The estimated molecular weights for each compound show small mass errors compared to the theoretical values (Table 3), which can be used to confirm the molecular weights of known compounds as well as to approximate the molecular weights of unknown impurities.</p><h4><strong>Conclusion</strong></h4><p>The separation patterns of synthetic peptides vary depending on mobile phase composition, column type, and various LC parameters, such as gradient conditions, column oven temperature, and flow rate. Separation behavior can also differ based on peptide structure, including length, amino acid composition, and the presence of modifications. Therefore, it is necessary to optimize the separation for each peptide sequence individually. However, optimizing analytical conditions through numerous analyses and data processing can be time-consuming. LabSolutions MD automates the entire workflow, including generating analysis schedules, preparing mobile phases, and processing the data, thanks to functionalities such as automated peak tracking, ranking of chromatograms, and design space visualization. This article introduced a case where the optimal separation conditions for synthetic peptides were efficiently identified through screening and optimization phases. LabSolutions MD also offers fully automated gradient optimization by AI algorithm to meet user-defined criteria. For more details, please refer to the application news, “Automatic Optimization of Gradient Conditions by AI Algorithm on Synthetic Peptide and Impurities: 01-00814”.</p><h3><strong>3. Thermo Fisher Scientific / HPLC Symposium: Sensitive cationic lipids impurities analysis with quantitation by charged aerosol detection and simultaneous mass confirmation by MS</strong></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/po_sensitive_cationic_lipids_impurities_analysis_quantitation_po_en_3dacf61554.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Cationic lipid is a critical component in lipid nanoparticle formulations for delivering nucleic acids such as mRNA, siRNA, antisense oligonucleotides etc. [2] Cationic lipids are amphiphilic molecules that possess a hydrophilic region, a hydrophobic region, and a linker structure connecting the two. [1] Charged aerosol detector (CAD) and evaporative light scattering detectors (ELSD) are preferred for characterizing lipid nanoparticle components, with CAD being the better choice for impurity quantification due to its higher sensitivity [3]. In a previous study, an inverse gradient method was developed to quantify impurities in cationic lipids raw materials.[1] To demonstrate the inverse gradient method on CAD HP, the same cationic lipids -- R-DOTAP, DLin-KC2- DMA and ALC-0315 -- were measured to this experiment as in Application note 003384 [1]. New diverter valve and software features were showcased, along with method’s sensitivity and repeatability.</p><h4><strong>Materials and methods</strong></h4><p>Using the inverse gradient method from Application note 003384 [1], to demonstrate impurity analysis in cationic lipids on the <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/2176"><strong>Thermo Scientific Vanquish Charged Aerosol Detector HP (CAD HP)</strong></a> integrated in the <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/743"><strong>Thermo Scientific Vanquish Flex Inverse Gradient UHPLC System</strong></a>, with parallel mass confirmation by the <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/413"><strong>Thermo Scientific ISQ EM Single Quadrupole Mass Spectrometer</strong></a>.&nbsp;</p><p><strong>Methods:</strong> The workflow uses a <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/743"><strong>Vanquish Flex Inverse Gradient LC system</strong></a> with Vanquish CAD HP and <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/1970"><strong>Thermo Scientific Hypersil GOLD C8 column</strong></a>.</p><h5><strong>Data Analysis&nbsp;</strong></h5><p><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/76"><strong>Thermo Scientific Chromeleon Chromatography Data System (CDS)</strong></a> 7.2.10 was used for data acquisition and analysis.</p><h4><strong>Conclusions&nbsp;</strong></h4><p>The CAD HP integrates perfectly into the Vanquish Inverse Gradient LC system and offers high sensitivity and excellent repeatability for quantitative cationic lipid impurity analysis, while the ISQ EM MS provides straightforward mass confirmation with high repeatability, all under compliance-ready conditions.</p><h3><strong>4. Waters Corporation: Quantitative Analysis of Four Long-Chain Lysophosphatidylcholines (LPCs) in Dried Blood Spot using Liquid Chromatography Tandem Mass Spectrometry for Clinical Research</strong></h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/720008826_en_dc154872b6.pdf"><strong>Full PDF for download</strong></a></li></ul><h5><strong>Benefits</strong></h5><ul><li>Good chromatographic resolution of all forms</li><li>Short extraction time compared to traditional methods for lipid extraction</li><li>Short analysis injection-to-injection 7 minutes</li></ul><p>Historically, very long chain fatty acids have been quantified using direct transesterification and gas chromatography methods which involve time-consuming and labor-intensive sample preparation and analysis. Consequently, simpler LC-MS/MS methods have been reported for the measurement of long-chain LPCs (LPCs generic chemical structure, Figure 1) in DBS. Interferences have been reported using positive ESI, thus researchers have developed methodologies utilizing negative ESI to circumvent isobaric interferences when there is lack of chromatographic resolution. Here a UHPLC-MS/MS method is described using acetate adducts for the reliable analysis of four long-chain LPCs in DBS for clinical research.&nbsp;</p><p>A UHPLC-MS/MS method for quantifying a panel of LPCs (C20:0, C22:0, C24:0, and C26:0-LPCs) was developed. The mobile phase composition consisted of a mixture of water, acetonitrile, and isopropanol with 5 mM ammonium acetate as a modifier. The DBS sample extraction used a working solution prepared with the deuterated LPC internal standards in methanol. The method was developed with an ACQUITY UPLC I-Class PLUS System (Fixed Loop) using an ACQUITY Premier CSH C18 Column, which provided baseline resolution of endogenous isobaric interferences for the saturated forms of the targeted LPCs. The detector was a Xevo TQ-S micro Mass Spectrometer operated in negative ESI mode. This methodology resulted in a total analysis time (injection-to-injection) of 7 minutes.</p><h5><strong>LC Conditions&nbsp;</strong></h5><ul><li><strong>LC system: </strong><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/199"><strong>ACQUITY UPLC I-Class PLUS FL&nbsp;</strong></a></li><li><strong>System Detection: </strong><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/209"><strong>Xevo TQ-S micro Mass Spectrometer&nbsp;</strong></a></li><li><strong>Plate:</strong> Waters 96-well Sample Collection Plate, 350 µL&nbsp;</li><li><strong>Column(s): </strong><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/1952"><strong>ACQUITY Premier CSH C18 Column</strong></a>, 2.1 mm x 50 mm, 1.7 µm (p/n: 186009460)</li></ul><h5><strong>MS Conditions&nbsp;</strong></h5><ul><li><strong>MS system:</strong> Xevo TQ-S micro Mass Spectrometer</li></ul><h5><strong>Data Management&nbsp;</strong></h5><ul><li><strong>MS software: </strong><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/635"><strong>MassLynx™ v4.2 Software SCN 1045&nbsp;</strong></a></li><li><strong>Informatics: </strong>TargetLynx™ XS v4.2 Software SCN1045 and QUAN Review</li></ul><h4><strong>Results and Discussion&nbsp;</strong></h4><p>During method development, different types of column chemistry, mobile phase composition, and ESI polarity modes were assessed to optimize chromatographic peak shape, analytical sensitivity and manage interferences. In positive mode, ammonium formate favored the formation of m/z 184 and m/z 104 as daughter ions for all the LPCs. The m/z 184 ion lacks specificity because most phospholipids share this moiety, so the ion m/z 104 was selected as quantifier. Having evaluated conditions in positive mode for the analysis of the four saturated LPCs, it was observed that some existing interferences were not only affecting the parent masses of the analytes but their corresponding internal standard parent ion masses too. Hence, negative ionization using ammonium acetate as modifier was assessed for the detection of LPCs. Acetate adducts [M+CH3COO]- were the most abundant parent ion masses, generated under these conditions for each LPC. The acyl-chain product ions generated in negative ionization reduce the detection of interferences coming from other phosphocholine headgroups. The latter detection conditions were used for the validation of the method presented herein.</p><h4><strong>Conclusion&nbsp;</strong></h4><p>An LC-MS/MS clinical research method for measuring C20:0, C22:0, C24:0, and C26:0 LPCs with the ACQUITY UPLC I-Class PLUS FL System, and the Xevo TQ-S micro Mass Spectrometer that:</p><ul><li>Demonstrates good linearity, with no significant carryover, or matrix effects</li><li>Offers good precision with a total reproducibility and repeatability <span>≤</span>10% CV</li><li>Offers reliability in the identification of LPCs from interfering isobaric compounds Provides good selectivity and analytical sensitivity in negative mode and is relatively fast as approximately 220 samples can be analyzed in 24 hours</li></ul>

News from LabRulezLCMS Library - Week 39, 2025

<p><strong>Our Library never stops expanding. What are the most recent contributions to LabRulezICPMS Library in the week of 22nd September 2025? Check out new documents from the field of spectroscopy/spectrometry and related techniques!</strong></p><blockquote><p><span style="font-size:20px;">👉 </span><a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library"><span style="font-size:20px;"><strong>SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT SPECTROSCOPY/SPECTROMETRY RELATED TECHNIQUES</strong></span></a></p></blockquote><blockquote><p><strong>👉 Need info about different analytical techniques?</strong> Peek into <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library"><strong>LabRulezLCMS</strong></a> or <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library"><strong>LabRulezGCMS</strong></a> libraries.</p></blockquote><p>This week we bring you application notes by <strong>Agilent Technologies</strong> and <strong>Shimadzu</strong> and<strong> </strong>poster by <strong>Thermo Fisher Scientific!</strong></p><h3><strong>1. Agilent Technologies: Protein Glycosylation Analysis Using the </strong><a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library?mainauthorItems=10&amp;search=Cary+630+FTIR"><strong>Agilent Cary 630 FTIR</strong></a><strong> Spectrometer</strong></h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_ftir_glycosylation_cary_630_5994_8540en_agilent_614efd9fb4.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Protein glycosylation is a crucial post-translational modification (PTM) impacting the efficacy, stability, and integrity of therapeutic proteins, including monoclonal antibodies (mAbs) and other biopharmaceuticals. This process involves attaching sugar molecules, or glycans, to specific amino acid residues on proteins. Glycosylation is classified as a critical quality attribute (CQA) and has important functions in biological processes, impacting protein structure, solubility, and ability to resist proteolytic degradation.1 Therefore, monitoring and controlling glycosylation is essential in developing and producing therapeutic proteins.</p><p>Various analytical techniques are employed to monitor glycosylation in biopharmaceutical production. These techniques include FTIR spectroscopy, mass spectrometry, high-performance liquid chromatography, capillary electrophoresis, nuclear magnetic resonance spectroscopy, and lectin arrays. However, most of these techniques require time-consuming complex sample preparation steps. Alternatively, FTIR is a robust analytical technique that provides a fast and easy tool for protein research. It is a nondestructive technique used to study protein molecules under different experimental conditions. The building blocks of glycans (monosaccharide/sugars), amide groups of protein, and water molecules produce distinguishable fingerprint absorption bands in FTIR. It has also been used to monitor the carbohydrate content and glycosylation profiles in&nbsp;glycoproteins.2,3&nbsp;</p><p>In this study, we used an Agilent Cary 630 FTIR spectrometer to demonstrate an FTIR spectroscopy method for protein glycosylation analysis. The results show that FTIR spectra of glycoproteins provide an FTIR signal corresponding to the glycosylation profile, allowing a rapid, nondestructive analysis method with minimal sample preparation.</p><h4><strong>Experimental&nbsp;</strong></h4><h5><strong>Instrumentation&nbsp;</strong></h5><p>The <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library?mainauthorItems=10&amp;search=Cary+630+FTIR"><strong>Cary 630 FTIR spectrometer </strong></a>was fitted with a single reflection diamond attenuated total reflection (ATR) module. Data acquisition was carried out with an Agilent MicroLab software using the parameters shown in Table 1.</p><h4><strong>Results and discussion&nbsp;</strong></h4><p>Proteins exhibit characteristic amide absorption bands in FTIR spectroscopy, which are related to secondary structure and confirmation. The amide I band (1,600 to 1,800 cm–1) and amide II band (1,470 to 1,570 cm–1) result from the absorption of the carbonyl and N-H group.&nbsp;</p><p>Glycosylation is one of the common PTMs that occur in biopharmaceuticals. Carbohydrates linked to glycoproteins have an absorption band distinct from the protein amide region. The infrared (IR) absorption of glycan spans broadly in the 1,200 to 950 cm–1 region where proteins have very low signal intensity. It has been demonstrated that the amount of carbohydrates in the glycoprotein correlates with the intensity of these spectral bands.3&nbsp;</p><p>In this study, various glycosylated proteins with different levels of glycosylation were selected to evaluate the FTIR method. The formulated mAbs contain excipients that can exhibit absorption bands, and these signals may interfere with glycan analysis in the 1,200 to 950 cm–1 region. Therefore, mAb samples were buffer-exchanged with water using spin columns. Figure 3 shows the comparison of FTIR spectra of formulated and buffer-exchanged mAbs. The desalting step is necessary to eliminate buffer interference with the glycosylation measurement.</p><h4><strong>Conclusion&nbsp;</strong></h4><p>This application note demonstrates the simplicity and usability of glycosylation analysis using an Agilent Cary 630 FTIR spectrometer. The FTIR method provides a spectral variation related to the global glycosylation level of protein, removing the necessity for extensive sample preparation or labeling. It provides a signal corresponding to the glycan profile that allows the identification of glycoproteins and enables rapid comparative glycosylation analysis between innovator and biosimilar therapeutic proteins. The user‑friendly Agilent MicroLab Expert software streamlines data processing and shortens time to results. The technique may be used to verify batch consistency and product quality during the protein production process. Its capability for quick glycosylation estimation makes it an excellent fit for protein quality control workflows. In summary, the FTIR approach provides numerous advantages, including minimal sample preparation, reduced analysis time, and the capacity to analyze intact glycoproteins</p><h3><strong>2. Shimadzu: Peel Test for Cathode Materials of Lithium-Ion Batteries in a Thermostatic Chamber</strong></h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_01_00944_en_88bbab3581.pdf"><strong>Full PDF for download</strong></a></li></ul><h5><strong>User Benefits</strong></h5><ul><li>A thermostatic chamber makes it possible to measure the adhesion force of cathode materials in actual temperature environments.&nbsp;</li><li>A copper foil peeling test device enables to conduct peel tests while maintaining a 90° angle in a thermostatic chamber.&nbsp;</li><li>By using a load cell with a wider accuracy guarantee range than a conventional one, it is possible to conduct high-accuracy tests even with small test forces.</li></ul><p>Lithium-ion batteries play an important role in various electronic devices due to their high energy density and excellent charging efficiency. To improve battery performance, materials and processing methods are actively being developed, and strength measurement is one of the essential evaluation methods. This Application News focuses on the adhesion strength of the electrode sheets used as battery electrodes. Fig. 1 shows the structure of an electrode sheet. An electrode sheet consists of an electrode material that adheres to a current collector, through which electrons move. The electrode material is composed of a cathode active material such as lithium iron phosphate and an insulating material known as a binder. When the adhesion between the electrode material and the current collector is weak, the electrode material may delaminate from the current collector, preventing electrons from moving in the electrode sheet and increasing the electrical resistance. Therefore, evaluating the adhesion strength is important for improving battery performance. In this application, test equipment, test conditions, and results of the peel test for battery cathode materials are described. The temperature dependence of the adhesion strength of the electrode materialsis also described.</p><ul><li><strong>Testing Machine: </strong><a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library?mainauthorItems=1&amp;search=AGS-V"><strong>Precision Universal Testing Machine AGS-V</strong></a></li></ul><h4><strong>Conclusion&nbsp;</strong></h4><p>Peel tests in a thermostatic chamber were conducted using an AGS-V and TCE-N300A for Lithium iron phosphate used as cathode sheet of lithium-ion batteries. From the test results, it was confirmed that the adhesion force between the cathode active material and the aluminum foil increased as the temperature increased. This measurement can easily evaluate the temperature dependence of mechanical characteristics of battery cathodes. This method is expected to be applied to solve problems for improving battery performance.</p><h3><strong>3. Thermo Fisher Scientific: Assessing the level and distribution of trace elements in individual cells using single cell ICP-MS analysis</strong></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/labrulez-bucket-strapi-h3hsga3/po_001851_tea_cells_icp_ms_ewcps_po001851_em_en_826dff968d.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Trace elements play a key role in many processes involved in living beings. Some elements are found as constituent elements in biopolymers, such as phosphorous as part of the DNA backbone, or sulfur, as part of the key amino acids methionine and cysteine involved in the formation of proteins covering a wide variety of functions. Other elements (in particular, the transition elements copper, iron, and zinc) are involved in specific functions, such as acting as co-factors in enzymes. However, the distribution of trace elements cannot be assumed to be homogeneous across a cell cohort, even under ideal conditions. Ultimately, cell-tocell variability of the metal content may be an important factor in understanding biological diversity. The analysis of specific biomarkers at the single cell level has therefore gained significant interest in recent years.&nbsp;</p><p>The analysis of the content of a given metal at the single cell level has remained a challenge. While inductively coupled plasma mass spectrometry (ICP-MS) is well known as a powerful and element-selective detection system, it is only recently that its capacity for analyzing individual cells has been recognized.</p><h4><strong>Methods</strong></h4><p>A <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/products/1206"><strong>triple quadrupole ICP-MS system</strong></a>, in conjunction with the scQuant plug-in for <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/products/1489"><strong>Thermo Scientific™ Qtegra™ Intelligent Scientific Data Solution software</strong></a> was used for all measurements.</p><h4><strong>Conclusions&nbsp;</strong></h4><p>This poster highlights how ICP-MS operated in the single cell mode can determine the amount of different trace elements in individual cells and can therefore allow not only assessment of the average element mass per cell, but also the element distribution across the cohort.&nbsp;</p><ul><li>Scanning for multiple elements is possible using a sequential approach, in which all the elements of interest are measured for an identical period in a single aspiration of a sample, and the results are summarized in a single data set.&nbsp;</li><li>The scQuant plug-in allows integrated control over sample delivery devices, in this case, a syringe pump, to facilitate a stable sample flow at the required low flow rates.&nbsp;</li><li>Key method parameters, such as detection sensitivity and transport efficiency can be determined as part of the same Qtegra ISDS Software LabBook or can be independently determined (if no suitable standards are available) and applied to a data set.&nbsp;</li><li>The data visualization features of the scQuant plug-in allow raw data and intermediate data (signal distribution) to be comprehensively evaluated, as well as enabling representation of results in either a histogram or a box plot. All results can be exported in a spreadsheet compatible format if required.</li></ul>

News from LabRulezICPMS Library - Week 39, 2025

<p><strong>In the week of September 29, the following webinars await you in the field of gas / solid phase and especially Raman, FTIR, GC and GC/MS.</strong></p><blockquote><h4><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/webinars"><strong>👉 DETAILS AND REGISTRATION IN THE WEBINARS SECTION</strong></a></h4><p><strong>👉 Search and filter in the largest global database</strong> with over <strong>5 000 GC, LC, MS and spectroscopy webinars</strong>.</p></blockquote><h5><strong>1. Thermo Fisher Scientific: Advanced analytical methods in polymer science, Part 1</strong></h5><ul><li>Tu, 30.9.2025 10:00 CEST</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/webinar/5455">Registration</a></li></ul><p>Free webinar on polymer science! Learn how rheology, FTIR, NIR, Raman, XRF, and XRD enhance polymer analysis, quality control, and material design. Live sessions with expert speakers.</p><h5><strong>2. Thermo Fisher Scientific: Advanced analytical methods in polymer science, Part 2</strong></h5><ul><li>We, 1.10.2025 10:00 CEST</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/webinar/5456">Registration</a></li></ul><p>Discover cutting-edge applications in polymer science! Learn about plastic sorting, multilayer analysis, and marine waste extrusion from leading experts.</p><h5><strong>3. Thermo Fisher Scientific: Advanced analytical methods in polymer science, Part 3</strong></h5><ul><li>Th, 2.10.2025 10:00 CEST</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/webinar/5457">Registration</a></li></ul><p>Explore hyphenated techniques in polymer science! Learn Rheo-Raman, Raman-assisted extrusion, and TGA-IR for advanced material analysis in this free webinar.</p>

Webinars LabRulezGCMS Week 40/2025

<p><strong>In the week of September 29, the following webinars await you in the field of liquid phase and especially HPLC and LC/MS.</strong></p><blockquote><h4><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/webinars"><strong>👉 DETAILS AND REGISTRATION IN THE WEBINARS SECTION</strong></a></h4><p><strong>👉 Search and filter in the largest global database</strong> with over <strong>5 000 GC, LC, MS and spectroscopy webinars</strong>.</p></blockquote><h5><strong>1. SelectScience: Part 2: Size exclusion chromatography with light scattering for biopharmaceuticals</strong></h5><ul><li>Mo, 29.9.2025 17:00 CEST</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/webinar/5430">Registration</a></li></ul><p>In Part 2, Dr. Jelle De Vos and Dr. Sonja Schneider share real-world SEC with light scattering applications for antibodies, mRNA-LNPs, AAVs, and VLPs in biopharma analysis.</p><h5><strong>2. Metrohm: Introduction to Localized Electrochemical Techniques</strong></h5><ul><li>Tu, 30.9.2025 10:00 CEST</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/webinar/5431">Registration</a></li></ul><p>Join this webinar to explore localized electrochemical techniques (SECM, SDC, SECCM) with applications in electrocatalysis, corrosion, and sensors.</p><h5><strong>3. Thermo Fisher Scientific: Probing DNA-damage response at the single cell level</strong></h5><ul><li>Tu, 30.9.2025 14:00 CEST</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/webinar/5501">Registration</a></li></ul><p>Learn how single-cell proteomics reveals cellular heterogeneity in DNA repair. Prof. Thalassinos explores 60G-induced damage, repair pathways, and links to cancer and neurodegeneration.</p><h5><strong>4. Agilent Technologies: Inert Separations for Oligo LC-MS Workflows</strong></h5><ul><li>Tu, 30.9.2025 17:00 CEST</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/webinar/5535">Registration</a></li></ul><p>Join Agilent’s webinar to discover next-gen HPLC column technology delivering sharper peaks, faster equilibration, and improved oligonucleotide separations.</p><h5><strong>5. Agilent Technologies: New Software Features for UV Work Station Software</strong></h5><ul><li>Tu, 30.9.2025 21:30 CEST</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/webinar/5521">Registration</a></li></ul><p>New functions of the improved UV Workstation Software will be described and demonstrated.</p><h5><strong>6. Mettler-Toledo: UV/Vis Integration in Laboratory Workflows</strong></h5><ul><li>We, 1.10.2025 09:00 CET</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/webinar/4746">Registration</a></li></ul><p>Join us for an engaging live webinar on integrating UV/Vis spectroscopy into your laboratory workflows.</p><h5><strong>7. Technology Networks: Addressing Evolving Demands in Food Analysis</strong></h5><ul><li>We, 1.10.2025 19:00 CEST</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/webinar/5466">Registration</a></li></ul><p>Learn how the PerkinElmer QSight 500 LC-MS/MS overcomes challenges in detecting PFAS, pesticides, and residues in complex foods with robust, efficient, and reliable workflows.</p><h5><strong>8. Waters Corporation: Managing Method Variability: A Foundation for Risk-Based Change - Session 3</strong></h5><ul><li>We, 1.10.2025 19:00 CET</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/webinar/5369">Registration</a></li></ul><p>Learn from real-world case studies how pharma companies manage analytical method changes, document variability, and ensure compliance with evolving regulatory expectations.</p><h5><strong>9. SCIEX: Streamline your ICH M10 workflows</strong></h5><ul><li>Th, 2.10.2025 11:00 CEST</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/webinar/5536">Registration</a></li></ul><p>Join SCIEX experts to explore ICH M10 guidelines for regulated bioanalysis and see how SCIEX OS software streamlines validation, reporting, and compliance.</p><h5><strong>10. Waters Corporation: Becoming a SEC-MALS &amp; ASTRA Expert: Part 8</strong></h5><ul><li>Th, 2.10.2025 11:00 CEST</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/webinar/5328">Registration</a></li></ul><p>Improve the reliability of your results by understanding error sources and uncertainty in MALS. Learn how to establish meaningful conclusions.</p><h5><strong>11. Thermo Fisher Scientific: Imaging of intact proteoform complexes in tissue</strong></h5><ul><li>Th, 2.10.2025 14:00 CEST</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/webinar/5502">Registration</a></li></ul><p>Discover how Dr. Oliver Hale applies nano-DESI native ambient MS to map proteoforms in tissues, preserving intact complexes and advancing neurodegenerative disease research.</p><h5><strong>12. Waters Corporation: Becoming an ASTRA Expert: Part 7</strong></h5><ul><li>Fr, 3.10.2025 20:00 CEST</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/webinar/5332">Registration</a></li></ul><p>Master the use of dn/dc and extinction coefficients in ASTRA. Understand how these key parameters influence accurate molar mass and concentration results.</p>

Webinars LabRulezLCMS Week 40/2025

<p><strong>In the week from September 29, the following webinars await you in the field of atomic and molecular spectroscopy and spectrometry</strong></p><blockquote><h4><a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/webinars"><strong>👉 DETAILS AND REGISTRATION IN THE WEBINARS SECTION</strong></a></h4><p><strong>👉 Search and filter in the largest global database</strong> with over <strong>5 000 GC, LC, MS and spectroscopy webinars</strong>.</p></blockquote><h5><strong>1. Thermo Fisher Scientific: Accurate Measurement of Elemental Impurities in Industrial Samples by ICP-OES and ICP-MS</strong></h5><ul><li>Mo, 29.9.2025 13:00 CEST</li><li><a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/webinar/4701">Registration</a></li></ul><p>Accurate Measurement of Elemental Impurities in Industrial Samples by ICP-OES and ICP-MS.</p><h5><strong>2. Thermo Fisher Scientific: Advanced analytical methods in polymer science, Part 1</strong></h5><ul><li>Tu, 30.9.2025 10:00 CEST</li><li><a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/webinar/5455">Registration</a></li></ul><p>Free webinar on polymer science! Learn how rheology, FTIR, NIR, Raman, XRF, and XRD enhance polymer analysis, quality control, and material design. Live sessions with expert speakers.</p><h5><strong>3. Metrohm: Introduction to Localized Electrochemical Techniques</strong></h5><ul><li>Tu, 30.9.2025 10:00 CEST</li><li><a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/webinar/5431">Registration</a></li></ul><p>Join this webinar to explore localized electrochemical techniques (SECM, SDC, SECCM) with applications in electrocatalysis, corrosion, and sensors.</p><h5><strong>4. Bruker: Spatially Resolved Geochemistry: micro-XRF Applications in Peer-Reviewed Geoscience</strong></h5><ul><li>Tu, 30.9.2025 17:00 CEST</li><li><a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/webinar/5443">Registration</a></li></ul><p>Discover how micro-XRF drives advances in geoscience. Learn its applications in mineral exploration, trace elements, sedimentation, and planetary samples.</p><h5><strong>5. Agilent Technologies: New Software Features for UV Work Station Software</strong></h5><ul><li>Tu, 30.9.2025 21:30 CEST</li><li><a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/webinar/5521">Registration</a></li></ul><p>New functions of the improved UV Workstation Software will be described and demonstrated.</p><h5><strong>6. Mettler-Toledo: UV/Vis Integration in Laboratory Workflows</strong></h5><ul><li>We, 1.10.2025 09:00 CET</li><li><a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/webinar/4746">Registration</a></li></ul><p>Join us for an engaging live webinar on integrating UV/Vis spectroscopy into your laboratory workflows.</p><h5><strong>7. Thermo Fisher Scientific: Advanced analytical methods in polymer science, Part 2</strong></h5><ul><li>We, 1.10.2025 10:00 CEST</li><li><a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/webinar/5456">Registration</a></li></ul><p>Discover cutting-edge applications in polymer science! Learn about plastic sorting, multilayer analysis, and marine waste extrusion from leading experts.</p><h5><strong>8. Thermo Fisher Scientific: Advanced analytical methods in polymer science, Part 3</strong></h5><ul><li>Th, 2.10.2025 10:00 CEST</li><li><a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/webinar/5457">Registration</a></li></ul><p>Explore hyphenated techniques in polymer science! Learn Rheo-Raman, Raman-assisted extrusion, and TGA-IR for advanced material analysis in this free webinar.</p><h5><strong>9. Anton Paar: Maximize Your XRD Efficiency with the XRDynamic Autosampler</strong></h5><ul><li>Th, 2.10.2025 18:00 CEST</li><li><a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/webinar/5447">Registration</a></li></ul><p>Discover the Anton Paar XRDynamic Autosampler—boosting XRD throughput, flexibility, and automation for up to 105 samples. Streamline routine and advanced materials research.</p><h5><strong>10. Agilent Technologies: Interference Correction using the Agilent 5X00 ICP Systems – FACT Modeling and Comparison with Inter-Element Correction IEC</strong></h5><ul><li>Th, 2.10.2025 20:00 CEST</li><li><a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/webinar/5448">Registration</a></li></ul><p>Learn how to correct spectral interferences in ICP-OES. Discover the advantages of FACT modeling compared to classical IEC correction with Agilent 5X00 ICP systems.</p>

Webinars LabRulezICPMS Week 40/2025

Synthesis and Identification of 3-Oxazolines in Cocoa

Hydrophilic Interaction Chromatography HRMS with Acrylamide Monolithic Columns: A Novel Approach for Intact Antibody Glycoform Characterization

<p><strong>This study presents a combined microwave-assisted digestion (MAD) and dispersive magnetic solid-phase microextraction (DMSPE) method for determining major (Ca, Cu, Fe, Mn, Mg, Na, Zn) and trace elements (As, Pb, Se) in lignocellulosic biomass by ICP-OES. Maghemite nanoparticles were synthesized and characterized to serve as sorbents, and conditions for both MAD and DMSPE were optimized using a central composite design.</strong></p><p>The method achieved low detection limits (As 0.01, Pb 0.03, Se 0.01 µg g–1) and high enrichment factors (21–42 for trace elements). Validation with certified reference materials confirmed accuracy. Application to five biomass samples provided reliable quantification of major elements, while As, Pb, and Se were below LOQs. This approach offers a robust strategy for elemental profiling of lignocellulosic biomass.</p><blockquote><h4><strong>The original article</strong></h4><h4><a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/10.1021/acsomega.5c02196"><strong>Microwave-Assisted Digestion Method and Dispersive Magnetic Solid-Phase Microextraction for the Determination of Major and Trace Elements in Lignocellulosic Biomass by ICP-OES</strong></a></h4><p>Camilla M. Belmiro, Mikaelle de Carvalho Gomes, Fernanda Nunes Ferreira, Márcia Angelica F. S. Neves, and Jefferson Santos de Gois*</p><p>ACS Omega 2025, 10, 28, 30443–30449</p><p><a target="_blank" rel="noopener noreferrer" href="https://doi.org/10.1021/acsomega.5c02196">https://doi.org/10.1021/acsomega.5c02196</a></p><h6>licensed under <a target="_blank" rel="noopener noreferrer" href="https://creativecommons.org/licenses/by/4.0/"><strong>CC-BY 4.0</strong></a></h6></blockquote><p><strong>Selected sections from the article follow. Formats and hyperlinks were adapted from the original.</strong></p><p>Lignocellulosic biomass consists mainly of cellulose, hemicellulose, and lignin. It can be used as an ecological material for the production of second-generation fuels, such as ethanol from petroleum to replace fossil fuels and their derivatives, and as an energy source (by gasification, pyrolysis, liquefaction, or combustion), with the aim of contributing to the reduction of global CO<sub>2</sub> emissions. <a href="javascript:void(0);">(1−4)</a></p><p>A variety of analytical techniques can be used for the elemental characterization of biomass and biomass-derived ash, such as inductively coupled plasma mass spectrometry (ICP–MS), <a href="javascript:void(0);">(5,6)</a> flame atomic absorption spectrometry (FAAS), <a href="javascript:void(0);">(7)</a> graphite furnace atomic absorption spectrometry (GF AAS), <a href="javascript:void(0);">(3)</a> laser-induced breakdown spectroscopy (LIBS), <a href="javascript:void(0);">(8)</a> and inductively coupled plasma optical emission spectrometry (ICP-OES). <a href="javascript:void(0);">(9−11)</a></p><p>Inductively coupled plasma optical emission is often used for the determination of trace elements due to its low detection limits and multielement capability. However, this technique usually requires at least one sample preparation step to solubilize the analytes in an aqueous medium prior to analysis. Microwave-assisted acid digestion (MAD) in closed vessels is considered the most efficient technique for the decomposition/solubilization of organic sample matrices and the determination of trace elements by spectrometric techniques. <a href="javascript:void(0);">(12)</a> Concentrated acids and their mixtures have been identified for the preparation of biomass samples with MAD, the most commonly used acids are hydrofluoric acid, <a href="javascript:void(0);">(10)</a> nitric acid, and/or hypochlorous acid and their mixtures; <a href="javascript:void(0);">(13)</a> hydrogen peroxide may also be used to recycle oxygen into the aqueous media. <a href="javascript:void(0);">(4,6)</a></p><p>Elements such as As, Pb, and Se usually occur in very low concentrations (ng g<sup>–1</sup>) and therefore require very sensitive analytical techniques for their determination or preconcentration methods, which can provide a cost-effective method for their determination. Dispersive magnetic solid-phase extraction (DMSPE) with magnetic nanoparticles of iron oxide (Fe<sub>3</sub>O<sub>4</sub> and Fe<sub>2</sub>O<sub>3</sub>) is advantageous because they can be quickly obtained by synthesis, can adsorb elements, and can be easily separated from the aqueous medium with a magnet. <a href="javascript:void(0);">(14,15)</a></p><p>Therefore, the aim of this work was to develop a MAD method using diluted HNO<sub>3</sub> for the determination of trace elements (Ca, Cu, Fe, Mn, Mg, Na, Zn), followed by an MSPE preconcentration method for the determination of As, Pb, and Se in lignocellulosic biomass samples by ICP-OES.</p><h4><strong>2. Materials and Methods</strong></h4><h5><strong>2.1. Instrumentation</strong></h5><p>An ICP-OES model <strong>iCAP 6300</strong>, equipped with a Mira Mist nebulizer (Burgener Research Inc., Canada) and a cyclone spray chamber (Thermo Scientific, USA), was used for the multielement determination. The operating parameters used in ICP-OES were plasma gas flow (12 L min<sup>–1</sup>), nebulizer gas flow (0.4 L min<sup>–1</sup>), auxiliary gas flow (1.0 L min<sup>–1</sup>), radio frequency power (1300 W), pump flow rate (5 rpm, 0.2 mL min<sup>–1</sup>), and radial view. The monitored wavelengths were Ca (422.673 nm), Cu (324.754 nm), Fe (259.940 nm), Mn (257.610 nm), Mg (280.270 nm), Na (588.995 nm), Zn (213.856 nm), As (189.042 nm), Pb (220.353 nm), Se (203.985 nm), and Sc (361.384 nm) as internal standards. Argon with a purity of 99.95% (Air Liquide, Brazil) was used as the main, auxiliary, and nebulizer gas. All mass measurements were performed using an analytical balance with an accuracy of 0.1 mg, model M214A (Bel Engineering, Italy). The samples were ground in a mill model MG200 (Black+Decker, Brazil) and sieved with a 200 mesh sieve.</p><p>The microwave-assisted digestion of the samples was carried out in a <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library?mainauthorItems=444&amp;search=Multiwave+PRO"><strong>Multiwave PRO microwave oven</strong></a> (Anton-Paar, Graz) with a 24HVT50 rotor model. The DMSPE experiments were carried out in a horizontal orbital shaker model SK-180-PRO (Scilogex, EUA) and a thermal shaker model Thermo Mixer (Kasvi, Brazil).</p><h5><strong>2.5. Dispersive Magnetic Solid-Phase Microextraction Procedure</strong></h5><h5><strong>2.5.2. Characterization of the γ-Fe2O3 Magnetic Nanoparticles</strong></h5><p>The synthesized magnetic γ-Fe<sub>2</sub>O<sub>3</sub> nanoparticles were characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), field emission scanning electron microscopy (FEG-SEM), and thermogravimetric analysis (TGA). A<strong> Frontier FTIR of the 98737 series</strong> (PerkinElmer, USA) was used for the FTIR analysis. The analysis was performed with a resolution of 4 cm<sup>–1</sup> in the range of 4000 to 400 cm<sup>–1</sup> in KBr pellets. For TGA, an SDT Q600 model (TA Instruments, USA) was used with the following parameters: a temperature range from 30 to 700 °C at a rate of 20 °C min<sup>–1</sup> under a nitrogen atmosphere (150 mL min<sup>–1</sup>). For FEG-SEM, images were taken with an electronic microscope model JSM-7100F (Jeol, Japan) with magnifications of x30 000 and x60,000. The XRD was carried out in an AXS D-5005/Siemens (Bruker, EUA), with an angular step of 0.10°, ranging from 15 to 70°, and with an acquisition time between counts of 1.0 s.</p><h4><strong>3. Results and Discussion</strong></h4><h5><strong>3.1. Chemical Characterization of the γ-Fe2O3 Magnetic Nanoparticles</strong></h5><p>The X-ray diffractogram of the magnetic γ-Fe<sub>2</sub>O<sub>3</sub> nanoparticles is shown in <a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/10.1021/acsomega.5c02196#fig1">Figure 1</a>A. Diffraction peaks were consistent with the standard structure and indicated the presence of the cubic phase of maghemite. These reflections are assigned to (220), (311), (400), (422), (511), and (440), which correspond to the crystallographic planes that are characteristic reflections of maghemite, indicating that they are consistent with the X-ray diffraction pattern of γ-Fe<sub>2</sub>O<sub>3.</sub> <a href="javascript:void(0);">(17)</a></p><p><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/ACS_Omega_2025_10_28_30443_30449_Figure_1_X_ray_diffraction_A_Fourier_transform_infrared_spectra_B_scanning_electron_microscopy_x60_000_C_and_thermogravimetric_analysis_of_g_Fe2_O3_D_8bb288c909.jpg" alt="ACS Omega 2025, 10, 28, 30443–30449: Figure 1. X-ray diffraction (A), Fourier transform infrared spectra (B), scanning electron microscopy x60,000 (C), and thermogravimetric analysis of γ-Fe2O3 (D)." srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_ACS_Omega_2025_10_28_30443_30449_Figure_1_X_ray_diffraction_A_Fourier_transform_infrared_spectra_B_scanning_electron_microscopy_x60_000_C_and_thermogravimetric_analysis_of_g_Fe2_O3_D_8bb288c909.jpg 238w," sizes="100vw" width="1750" height="1144"></p><p>Fourier transform infrared spectroscopy was used to characterize the functional groups. The FTIR spectra of the γ-Fe<sub>2</sub>O<sub>3</sub> nanoparticles, shown in <a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/10.1021/acsomega.5c02196#fig1">Figure 1</a>B, highlight the bands at 628, 580, and 447 cm<sup>–1</sup>, which correspond to the vibrational mode of stretching and angular deformation characteristic of Fe–O bonding and confirm the formation of γ-Fe<sub>2</sub>O<sub>3</sub>. <a href="javascript:void(0);">(18)</a> The broad stretching band at 3411 cm<sup>–1</sup> corresponds to the OH group and surface H<sub>2</sub>O, and the band at 1630 cm<sup>–1</sup> correlates with the angular deformation mode of H–O–H. The OH groups at the surface are associated with residual or physically adsorbed water. <a href="javascript:void(0);">(14)</a></p><p>The thermal stability of maghemite was investigated using TGA. It was found that the material is thermally stable, as it suffers a slight mass loss with an increase in temperature, as shown in <a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/10.1021/acsomega.5c02196#fig1">Figure 1</a>D. The mass loss at around 100 °C is due to the loss of water, which is physically adsorbed onto the material. <a href="javascript:void(0);">(16)</a> In the range between 550 and 580 °C, a mass loss is observed, which is due to phase transitions from maghemite to hematite. <a href="javascript:void(0);">(15)</a></p><h5><strong>3.2. Microwave-Assisted Digestion of Biomass</strong></h5><p>Microwave-assisted digestion is a powerful technique for decomposition of the organic matrix of a sample and solubilization of inorganic analytes into the aqueous media for analysis. This technique can be used with inorganic acids and H<sub>2</sub>O<sub>2</sub> to increase the efficiency of sample digestion. Microwave-assisted digestion in closed vessels can minimize analyte loss, reduce contamination, and shorten sample preparation time. It also offers high sample decomposition efficiency and high sample throughput. <a href="javascript:void(0);">(19,20)</a> The selection of the type and concentration of inorganic acids, as well as the sample mass, is crucial for sample preparation in microwave-assisted digestion. Therefore, the optimization of these factors was performed, as described in Section <a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/10.1021/acsomega.5c02196#sec2_3">2.3</a>. Nitric acid was selected for sample preparation due to its oxidizing properties and versatility for a variety of organic matrices; furthermore, the nitrates are soluble in aqueous media.</p><p><a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/suppl/10.1021/acsomega.5c02196/suppl_file/ao5c02196_si_001.pdf">Table S3</a> shows the fitted models for each analyte after refinement, where the obtained R-squared ranged from 0.6885 to 0.9989, while the fitted R-squared ranged from 0.6719 to 0.9987, indicating a good fit of the models. According to the Shapiro–Wilk test (α = 0.05), the residuals of the models for Ca, Fe, Mg, Mn, Na, and Zn were found to follow a normal distribution, except for Cu, for which the central limit theorem was considered.</p><p>The desirability function was applied to determine the optimal experimental condition for multiresponse optimization, with values ranging from 0 (undesirable value) to 1 (desirable value). <a href="javascript:void(0);">(21)</a> The surface response of the overall desirability for the microwave-assisted digestion method is shown in <a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/10.1021/acsomega.5c02196#fig2">Figure 2</a>. The optimum experimental condition was achieved at a sample mass of 280 mg, 2.5 mL of HNO<sub>3</sub>, and 2.0 mL of H<sub>2</sub>O<sub>2</sub>, achieving an overall desirability of 0.534, which is an acceptable value, while the individual desirabilities were Ca (0.618), Cu (0.535), Fe (0.428), K (0.388), Mg (0.378), Mn (0.866), Na (0.620), and Zn (0.591).</p><p><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/ACS_Omega_2025_10_28_30443_30449_Figure_2_Overall_desirability_response_surface_for_the_optimization_of_the_microwave_assisted_digestion_of_lignocellulosic_biomass_9dd074f965.jpg" alt="ACS Omega 2025, 10, 28, 30443–30449: Figure 2. Overall desirability response surface for the optimization of the microwave-assisted digestion of lignocellulosic biomass and determination of Ca, Cu, Fe, Mn, Mg, Na, and Zn by ICP-OES." srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_ACS_Omega_2025_10_28_30443_30449_Figure_2_Overall_desirability_response_surface_for_the_optimization_of_the_microwave_assisted_digestion_of_lignocellulosic_biomass_9dd074f965.jpg 245w," sizes="100vw" width="1305" height="420"></p><h4><strong>4. Conclusions</strong></h4><p>A microwave-assisted digestion method and a dispersive magnetic solid-phase microextraction method for trace-element determination in lignocellulosic biomass were successfully obtained. Both methods were optimized using a multivariate approach, which ensured a high efficiency of the methods.</p><p>The developed microwave-assisted digestion achieved good accuracy using a lower concentration of reagents than reported in the literature, while the microextraction method using maghemite nanoparticles provided a simple and reliable alternative for the determination of trace elements in biomass samples. Although only Ca, Cu, Fe, Mn, Mg, Na, Zn, As, Pb, and Se were considered in the validation of the method, we believe that this method can be extended for other analytes after proper validation, especially As, Pb, and Se, since the recovery of the analytes was performed by dissolving the nanomaterial into an aqueous medium. The methods provided good accuracy for all analytes and LOQs suitable for the purpose and proved to be a good alternative for the determination of trace elements in biomass samples from lignocellulose.</p>

Microwave-Assisted Digestion Method and Dispersive Magnetic Solid-Phase Microextraction for the Determination of Major and Trace Elements in Lignocellulosic Biomass by ICP-OES

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Microwave-Assisted Digestion Method and Dispersive Magnetic Solid-Phase Microextraction for the Determination of Major and Trace Elements in Lignocellulosic Biomass by ICP-OES

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