Our Library never stops expanding. What are the most recent contributions to LabRulezGCMS Library in the week of 15th December 2025? 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: Increased Thermal Stability of the DB‑5Q GC Column</h3>Increased signal-to-noise for trace level concentrations of controlled substances<ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_stability_gc_column_5994_8658en_agilent_4c52ae52cf.pdf">Full PDF for download</a></li></ul>The analysis of controlled substances by gas chromatography/mass spectrometry (GC/MS) requires a high level of confidence and thus requires a method that provides optimal data quality. Identification of controlled substances relies heavily on comparison of mass spectra to commercially available spectral libraries, and increased column bleed can cause spectral interference at high temperatures. These interferences can lead to poor library matching probabilities.1-3 The <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=J%26W+5Q">Agilent J&amp;W 5Q series</a> of gas chromatography columns provide the most thermally stable columns available, which helps to decrease spectral interference due to column bleed and improves data accuracy.&nbsp;Poor thermal stability will cause an increase in the slope of the baseline as the oven temperature is increased, leading to difficult peak integrations and inaccurate quantitation. Additionally, sloped or elevated baselines can lead to a decreased response and a loss of sensitivity for analytes eluting during the oven ramp or at the method’s upper temperature limits. Several commercially available 5ms type columns were compared to the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=J%26W+DB-5Q">Agilent J&amp;W DB-5Q GC column</a> to examine the impact thermal stability has on response at upper temperature limits.&nbsp;<h4>Experimental&nbsp;</h4>An <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=8890+GC">Agilent 8890 GC system</a> coupled with an <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=5977B">Agilent 5977B mass selective detector (GC/MSD)</a> with an inert extractor ion source was used for acquisition of data and MassHunter 10.0 Quantitative and Qualitative Analysis software was used for data analysis.&nbsp;A representative toxicology mixture, the Agilent GC/MS forensic toxicology checkout mixture (part number 5190-0471) was used to monitor analytical performance. Calibration standards were prepared in methanol (MeOH) at concentrations ranging from 0.1 to 3.0&nbsp;μg/mL. An internal standard mix was prepared at 10&nbsp;μg/mL from individual stocks of methamphetamine-d3, diazepam-d5, and hydrocodone-d6 all purchased from Millipore Sigma (St.&nbsp;Louis, MO).<h4>Results and discussion&nbsp;</h4>The testing evaluated the Agilent J&amp;W DB-5Q GC column for the analysis of controlled substances by GC/MS. The increased thermal stability of the DB-5Q is seen in the decreased baseline at higher temperatures, as seen in Figure&nbsp;1, and also provides a decrease in the slope during the oven ramping program.&nbsp;An increase in the slope of the baseline will also decrease the signal-to-noise ratio (S/N) of an analyte but will also make integration more difficult and lead to less accurate quantitative results. Figure 2 demonstrates the comparison of the DB-5Q and the commercially available 5ms type G column, and the impact to chromatography during the oven ramp. The S/N for the analytes on the oven ramp slope are a factor of ten or greater for the DB-5Q in comparison to the 5ms type G column.<h4>Conclusion&nbsp;</h4>The increased thermal stability of the Agilent J&amp;W DB-5Q GC column demonstrated in this application note provides a decreased baseline at higher temperatures, which allows for an increased response for later eluting compounds at trace level concentrations. The baseline of the DB-5Q remains more consistent as the temperature is increased. This consistency allows for more accurate integration and quantitation for analytes eluting during oven ramping, in comparison to other commercially available 5ms-type columns. The robust DB-5Q column phase maintained peak shape for trace level basic compounds even when stressed with a heavy matrix and is an excellent choice for the analysis of controlled substance&nbsp;analysis.<h3>2. Shimadzu: Quantitative Analysis of Anti-Degradant Additive (6PPD) in Tire Rubber Using Pyrolysis-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_01_00952_en_b95b2348e5.pdf">Full PDF for download</a></li></ul><h5>User Benefits</h5><ul><li>The simple analysis procedure required just cutting off a sample fragment and placing it in a sample cup without pretreatment.</li><li>Utilizing a calibration standard that includes a resin solution allows for analysis under conditions that closely resemble those of samples, which improves the reliability of quantitative measurements.</li><li>With Shimadzu’s Polymer Additive Library, it is possible to acquire information on the additives of identified compounds.</li></ul>6PPD (N-(1,3-dimethylbutyl)-N'-phenyl-p-phenylenediamine) is an anti-degradant (anti-oxidant) additive that is used in many rubber products. Its chemical structure is shown in Fig. 1. It plays an important role in tires by preventing degradation and extending its lifespan. However, when 6PPD reacts with ozone in the atmosphere, it forms a highly toxic substance called 6PPD-quinone (6PPD-Q).&nbsp;As an automotive tire wears, microscopic particles are released from the tire into the environment. These particles, tire road wear particles (TRWP), contain 6PPD-Q along with many other chemical substances. On rainy days, these particles are washed into rivers and other bodies of water, where they accumulate in the environment as microplastics.&nbsp;There are serious concerns about the negative effects these microplastics have on ecosystems and the environment. 6PPDQ has been shown to induce acute mortality in Salmonidae fish, specifically coho salmon. 1)&nbsp;Currently, there is no commercial alternative that can maintain tire stability and performance with minimal impact on the environment. Research into alternatives requires accurately assessing 6PPD levels in rubber products and objectively determining whether alternative compounds offer equivalent stability and performance while having a reduced impact on the environment.&nbsp;This article describes using a pyrolysis gas chromatograph mass spectrometer (Py-GC-MS) system to measure 6PPD levels in tire rubber.<h4>Analysis Process&nbsp;</h4>ISO/TS 21396describes a method for determining the mass concentration of TRWP in soil and sediment that uses Py-GC-MS. Similar to this method, Py-GC-MS was used for the analysis; however, this article employs optimized analytical conditions. A schematic diagram of the analysis processisshown in Fig. 2. For more information on the analysis conditions and results from the evolved gas analysis (EGA-MS, <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=42&amp;search=EGA%2FPY-3030D">EGA/PY-3030D Multi-Shot Pyrolyzer AS-1020E Auto-Shot Sampler</a>, Frontier Laboratories Ltd.) method described in Fig. 2, please see Application News No. 01-00901. The analysis conditions for the thermal desorption (TD)-GC/MS (<a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=1&amp;search=GCMS-QP2020+NX">GCMS-QP2020 NX</a>) method used in this article are shown in Table 1. The thermal desorption temperature was chosen based on results obtained by the EGA-MS method.<h4>Qualitative Analysis of Additive&nbsp;</h4>The total ion current (TIC) chromatogram obtained from analyzing the tire rubber is shown in Fig. 4. A spectral library search was also performed using NIST-23 and Shimadzu’s Polymer Additives Library. The library search results for the peak that eluted at around 10.43 minutes are shown in Fig. 5. Based on the results from Shimadzu’s Polymer Additives Library, the peak was estimated to be the anti-degradant Nocrac 6C (a trade name for the chemical 6PPD).<h4>Conclusion&nbsp;</h4>This article presents an analysis of the additive 6PPD in tire rubber utilizing Py-GC-MS. Good results were obtained for calibration curve linearity, calibration standard repeatability, limit of quantification, and limit of detection. Shimadzu’s Polymer Additives Library was used to identify the additive.<h3>3. Thermo Fisher Scientific: Gas chromatography analyzers for the oil &amp; gas industry: upstream to downstream</h3><ul><li>Brochure</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/br_003966_gc_analyzers_trace_1610_industrial_br003966_na_en_44ad1327c6.pdf">Full PDF for download</a></li></ul>Gas chromatography (GC) plays a central role in the oil and gas industry, providing high-accuracy, high-speed analysis of complex hydrocarbon mixtures from upstream exploration through midstream transport to downstream refining and distribution. Across this value chain, GC supports regulatory compliance, product quality control, custody transfer, and process optimization. As the industry adapts to decarbonization goals and stricter environmental regulations, robust and automated analytical solutions have become essential for monitoring hydrocarbons, impurities, and trace components under demanding 24/7 operational conditions.Thermo Scientific™ GC analyzers are engineered to meet these challenges, with the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/486">TRACE™ 1610 GC</a> platform forming the backbone of a comprehensive portfolio of preconfigured and customizable systems. Its modular “Instant Connect” design enables rapid configuration of injectors, detectors, and valves, reducing downtime and simplifying maintenance. The platform supports multi-detector configurations—including FID, TCD, FPD, PDD, MS, and VUV—allowing a single analyzer to address a broad range of applications, from natural gas composition and BTU determination to sulfur species, fixed gases, and detailed hydrocarbon analysis .Dedicated GC analyzer configurations are available for specific industry needs, including natural gas and natural gas liquids (NGA/NGL), refinery gas analysis (RGA), light hydrocarbons (LPG), oxygenates, aromatics (BTEX), permanent gases, and high-purity gas streams. Advanced techniques such as GC-VUV further simplify complex analyses like PIONA group-type characterization of gasoline, delivering comprehensive compositional data in a single run while reducing calibration effort and cost per sample. These systems are designed to comply with major ASTM, ISO, GPA, DIN, EN, and UOP standards, ensuring global regulatory alignment .Complementing the hardware, <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/76">Thermo Scientific™ Chromeleon™ Chromatography Data System (CDS)</a> provides an integrated informatics backbone for method control, data processing, reporting, and connectivity to LIMS platforms. This unified approach enhances data integrity, improves workflow efficiency, and enables real-time decision-making across refinery and gas processing operations. Together, Thermo Scientific GC analyzers and integrated software solutions deliver reliable, scalable, and future-ready analytics for the evolving oil and gas industry.

News from LabRulezGCMS Library - Week 51, 2025

News from LabRulezLCMS Library - Week 51, 2025

Our Library never stops expanding. What are the most recent contributions to LabRulezICPMS Library in the week of 15th December 2025? 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 Shimadzu!<h3>1. Agilent Technologies: Measurement of Bidirectional Transmittance Distribution Function</h3>Using the <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library?mainauthorItems=10&amp;search=Cary+7000">Agilent Cary 7000</a> universal measurement spectrophotometer<ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_btdf_cary_7000_ums_5994_8679en_agilent_c2ced43759.pdf">Full PDF for download</a></li></ul>The bidirectional transmittance distribution function (BTDF) is a fundamental concept in optical metrology, describing how light is transmitted through a material in various directions. Understanding BTDF is essential for characterizing the optical properties of materials.&nbsp;To address BTDF, it is important to first understand the bidirectional scattering distribution function (BSDF). BSDF encompasses both the bidirectional reflectance distribution function (BRDF) and BTDF. While BRDF measures how light is reflected off a surface, BTDF focuses on the transmission of light through a material. Together, these functions provide a comprehensive picture of how light interacts with materials, enabling precise characterization of their optical&nbsp;behavior.1,3&nbsp;BTDF measurements are used in diverse fields to understand how light is transmitted through materials. In computer graphics, BTDF data enables realistic rendering of materials, enhancing visual simulations and animations with lifelike quality.4 Remote sensing relies on BTDF to calibrate satellite sensors, improving the accuracy of earth observation data necessary for monitoring environmental changes and weather patterns.5 Optical device design benefits from BTDF measurements by optimizing the performance of lenses, diffusers, and light-emitting devices, ensuring efficient light transmission.4 In materials science, BTDF characterizes the optical properties of new materials, aiding in the development of advanced composites and coatings.6 The food industry uses BTDF to assess the quality and consistency of products through their optical characteristics, which is vital for quality control.6 The solar industry uses BTDF to enhance the efficiency of solar panels and photovoltaic devices by understanding light transmission properties.6 Additionally, the aerospace sector uses BTDF to evaluate the optical properties of materials used in satellites and other space applications, ensuring reliable performance under various&nbsp;conditions.4&nbsp;The focus of this work is to demonstrate that BTDF measurements in the visible and near-infrared (NIR) spectral range can be easily performed using the Agilent&nbsp;Cary 7000 universal measurement spectrophotometer (UMS), Figure 1. Alternatively, the Agilent Cary 5000 and 6000i instruments equipped with the universal measurement accessory (UMA) may also be used for BTDF measurements. These instruments offer automated control over detector position, sample rotation, and polarization, making BTDF measurements straightforward and&nbsp;reliable.<h4>Setup for the <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library?mainauthorItems=10&amp;search=Cary+7000">Cary 7000 UMS&nbsp;</a></h4>The Cary 7000 UMS was used for measurements of directional and bidirectional transmittance with in-plane geometries ranging from −85° to 85° viewing angles. The instrument is easily configured using Agilent Cary WinUV software, as shown in Figures 4 and 5, and method parameters are summarized in Table 1. The source system included a quartz tungsten-halogen lamp and a deuterium arc lamp for UV illumination, coupled with a Littrow out-of-plane DMC. The DMC output slit provided a 4 nm bandwidth for the illuminating beam. The optics directed the beam onto a chopper, forming a double-beam photometric configuration. The reference beam monitored the illumination source for any drift in intensity, while the sample beam was shaped by vertical and horizontal slits to control convergence, resulting in an approximately 5.0 × 4.5 mm beam spot on the sample.&nbsp;The detection system included a set of turntables regulated by an optical encoder wheel with an angular resolution of 0.02°. The sample holder and detector turntables set the incident and viewing zenith angles within ± 85°. If BRDF were to be performed, excluded angles would be between ± 10° due to shadowing by the detector. The detector setup featured a calibrated aperture with an 18.00 mm diameter and a sample-to-detector-aperture distance of 129 mm, resulting in a solid angle of 0.0153 sr. The scattered light was collected by an off‑axis mirror onto a dual-band Si/InGaAs photodetector for the visible and NIR wavelength range.<h4>Results and discussion</h4><h5>BTDF measurement by the Cary 7000&nbsp;UMS&nbsp;</h5>The Cary 7000 UMS was used to measure the spectral BTDF of two samples: fused synthetic silica (HOD‑500) and porous polytetrafluoroethylene (PTFE). Measurements were conducted across the wavelength range of 450 to 1,650 nm in 50 nm intervals, and viewing zenith angles from –35° to 35° in 5° steps. Figures 6 and 7 illustrate the BTDF results for both samples. Figure 6A shows the BTDF of the HOD‑500 sample, while Figure 6B presents the BTDF of the PTFE sample. Both samples exhibited near-Lambertian characteristics and a smooth increase in BTDF as a function of wavelength.<h4>Conclusion&nbsp;</h4>The Cary 7000 universal measurement spectrophotometer (UMS) is an effective and user-friendly instrument for assessing the bidirectional transmittance distribution function (BTDF) across visible and near-infrared wavelengths. Its automated features, including detector positioning, sample rotation, and polarization control, streamline the measurement process, ensuring simplicity and reliability. The Cary 7000 UMS consistently delivers precise results with acceptable levels of uncertainty, making it ideal for routine BTDF assessments. Its intuitive interface and seamless integration with Cary WinUV software make it versatile for various optical metrology applications, offering a practical solution for both researchers and industry professionals.<h3>2. Metrohm: Online zinc/nickel plating bath analysis with X-ray fluorescence</h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_pan_1069_download_66948900d9.pdf">Full PDF for download</a></li></ul>Electroplating is a technique that uses electrical current to apply a thin coating of one material, such as nickel or zinc, onto the surface of another material, such as copper. Zinc and zinc-based alloys, such as zinc-nickel (Zn/Ni), are commonly used to protect steel from corrosion. Zn-Ni alloys are especially popular, as they offer a corrosion resistance that is greater than that of pure zinc [2,3].&nbsp;Both alkaline and acidic Zn/Ni baths are commonly used for electroplating (Figure 1). Each bath type offers unique advantages depending on the application [4]. Alkaline Zn/Ni baths are known for producing highly uniform coatings with good throwing power, making them ideal for complexshaped components. On the other hand, acidic Zn/Ni baths offer higher deposition rates and can deliver smooth, bright finishes that are often preferred for aesthetic applications [4].Electroplating baths are sensitive to various processrelated fluctuations that significantly impact metal deposition and influence the final coating thickness and quality. These variations can arise due to changes in temperature, plating tank metal concentration levels, or contamination. Analyzing the bath solution frequently is crucial to maintain stable plating conditions and minimize material waste. Continuous monitoring of the plating solutions helps ensure that the concentration of metals remains within the optimal range.&nbsp;The metal content in electroplating baths is often measured manually in on-site laboratories. Classical wet chemistry techniques, AAS, and ICP-OES are commonly used for this purpose. While these methods are effective, they can be time consuming, require skilled personnel, and may not provide realtime data. This potentially leads to delayed corrections and material inefficiencies. Modern process analytical technologies (PAT) are increasingly being adopted in electroplating operations to automate and optimize the monitoring of plating baths. These systems continuously analyze critical bath parameters such as metal concentration, pH, temperature, and conductivity in real time. All these factors directly influence the quality and uniformity of the deposited metal coating.The <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library?mainauthorItems=220&amp;search=2060+XRF+Process+Analyzer">2060 XRF Process Analyzer</a> from Metrohm Process Analytics (Figure 2) offers an effective solution to continuously monitor electroplating baths. By providing real-time measurements of metal concentrations such as Zn and Ni, this process analyzer helps maintain the ideal bath composition required for consistent and high-quality coatings.<h4>Conclusion</h4>The 2060 XRF Process Analyzer is a reliable solution for the metal finishing industry, offering real-time monitoring of zinc and nickel concentrations in electroplating baths. Its ability to continuously measure these key bath parameters ensures consistent coating quality, reduces material waste, and improves process efficiency.<h3>3. Shimadzu: Determination of Elemental Impurities in Petroleum Distillates Using ICP-MS ~ASTM D8110-17~</h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_01_00922_en_0b99a9bc9e.pdf">Full PDF for download</a></li></ul><h4>User Benefits</h4><ul><li>&nbsp;Enables the analysis of elemental impurities in various kinds of petroleum distillates (light and middle distillates) with the sample preparation method that involves only dilution with organic solvents.</li><li>Metal elements in petroleum distillates (light and middle distillates) can be accurately analyzed over a long period of time.</li><li>Solvent-resistant peristaltic pump tubing enables the addition of internal standard elements in-line, even for organic solvent analysis, thereby eliminating the need for manual addition.</li></ul>The concentration of metal elements in petroleum products needs to be controlled due to concerns that they can act as catalyst poisons and affect product quality. Additionally, it is important to measure the concentration of heavy metals to reduce environmental impact during emissions. Traditionally, analytical methods using ICP Optical Emission Spectrometry (ICPOES), such as ASTM D7111-161), have been employed to determine metal elements in petroleum products. However, in recent years, there has been a demand for more sensitive analytical methods using ICP mass spectrometry (ICP-MS), such as ASTM D8110-172), to detecttrace amounts of metal elements.&nbsp;ASTM D8110-17 is the test method for the analysis of elements in petroleum distillates (light and middle distillates) using ICP-MS. Since this method involves diluting the sample with organic solvents, it is necessary to introduce organic solvent samples into the ICP-MS.&nbsp;In this Application News, various light and middle distillates were diluted with organic solvents in accordance with ASTM D8110-17 and trace elements were analyzed using the <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library?mainauthorItems=1&amp;search=ICPMS-2050">ICPMS-2050</a> (Fig. 1). The validity of the analytical results was confirmed through spike recovery tests and the analysis of reference material for residual fuel oil. Additionally, the stability of the analysis over long periods of time was evaluated.<h4>Removal of Interference and Detection Limit&nbsp;</h4>To analyze metal elements with high sensitivity in organic solvents, it is important to eliminate interference caused by carbon from the organic solvent. For example, there are carbonderived polyatomic ion interferences such as 12C12C+ for 24Mg, 12C16O+ for 28Si, and 40Ar12C+ for 52Cr. By using collision mode with helium gas or reaction mode with hydrogen gas, these interferences can be eliminated, enabling sensitive analysis. As an example, Fig. 2 shows the calibration curve for Mg under each condition. In the No Gas mode, the influence of 12C12C+ results in a high background equivalent concentration (BEC), making it challenging to analyze trace amounts of 24Mg. However, in collision mode, the interference from 12C12C+ was reduced, and BEC of 80 ng/g was obtained. Furthermore, in reaction mode, the interference from 12C12C+ was significantly reduced, and BEC of 0.8 ng/g was obtained, which enables trace amounts of 24Mg analysis. Detection limits are shown in Table 4. The detection limit was calculated as the concentration that gives a signal equivalent to three times the standard deviation (σ) of the calibration blank sample (STD0).<h4>Long Term Stability&nbsp;</h4>To evaluate the long-term stability of organic solvent analysis using the <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library?mainauthorItems=1&amp;search=ICPMS-2050">ICPMS-2050</a>, light and middle distillates were analyzed over approximately 6 hours. To confirm the variability of the quantitative results, Check Standards were analyzed before sample analysis, every 10 samples, and at the end of the analysis. The results are shown in Fig. 3. All quantitative results of the Check Standard fell within the range of 90 to 110 % based on the prepared concentrations, which meets the validation requirements of ASTM D8110-17 (red dashed line). Additionally, the change in the intensity of the internal standard elements over approximately 6 hours are shown in Fig. 4. The change in intensity of the internal standard elements were within 90 to 120 %, which also falls within the validation requirements of 50 to 150 % asspecified in ASTM D8110-17 (red dashed line). These results indicate that the ICPMS-2050 has sufficient long term stability for the analysis of organic solvent samples.<h4>Conclusion&nbsp;</h4>In this Application News, the analysis of metal elements in light and middle distillates was performed using the ICPMS-2050 and the organic solvent introduction system. Good results were obtained from spiking recovery tests and the analysis of reference material for residual fuel oil, demonstrating that trace metal elements in light and middle distillates can be accurately quantified with a simple sample preparation method that involves only dilution with organic solvents. Furthermore, the recoveries of the Check Standards and the change in intensity of the internal standard elements also satisfied the validation requirements of ASTM D8110-17, confirming stable analysis over long periods of time. Since it is possible to analyze without the complex procedures required for acid decomposition, the risk of volatilization or contamination of the target elements during the sample preparation process is reduced. Additionally, the use of solventresistant peristaltic pump tubing enables the in-line addition of internal standard elements, further reducing the time required for sample preparation.

News from LabRulezICPMS Library - Week 51, 2025

Insecticide-Induced Perturbations in Sugar Metabolism and Alkaloid Biosynthesis in Coffea arabica (L.) Seedlings

A stability-indicating RP-HPLC method was developed and validated for impurity analysis of the cystic fibrosis drug Elexacaftor using a Quality-by-Design (QbD) approach. The method achieved effective separation of six known impurities with appropriate resolution and peak shape under optimized chromatographic conditions.Validation according to ICH guidelines confirmed the method’s robustness, linearity, accuracy, specificity, and precision. Stress testing under hydrolytic, oxidative, thermal, and photolytic conditions demonstrated suitability for degradation studies, supporting both process development and routine quality control of bulk drug substances.<blockquote><h4>The original article</h4><h4><a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/10.1021/acsomega.4c10834">Quality-by-Design-Driven RP-HPLC Method Development and Validation for Impurity Analysis of Elexacaftor, a Cystic Fibrosis Drug, with LC-MS/MS-Based Degradant Identification</a></h4>Jayaprakash Kanijam Raghupathi, Divya Kumar Vemuri, Syed Mastan Ali, Vishnuvardhana Kishore Polisetti, Rambabu Gundla, Leela Prasad Kowtharapu, Dittakavi Ramachandran*, and Naresh Kumar Katari*ACS Omega 2025, 10, 39, 44885–44894<a target="_blank" rel="noopener noreferrer" href="https://doi.org/10.1021/acsomega.4c10834">https://doi.org/10.1021/acsomega.4c10834</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.Elexacaftor is a drug that is used to treat fibrosis (TCF). When treating patients with cystic fibrosis (CF) who have the F508del mutation or other genetic mutations that react well with these medications, it is specifically used in conjunction with two other medications, ivacaftor and tezacaftor. The cystic fibrosis transmembrane conductance regulator, or CFTR, modulator, is Elexacaftor. Due to genetic abnormalities, people with CF have abnormal CFTR protein function, which is improved by this treatment. Based on clinical research, individuals with CF should expect a much better quality of life, reduced pulmonary exacerbations, and improved lung function when using Elexacaftor, ivacaftor, and tezacaftor together as opposed to prior treatments. After receiving FDA approval, Elexacaftor was marketed in the USA under the brand name Trikafta in October 2019. <a href="javascript:void(0);">(1−5)</a> Since then, it has emerged as a key component of the CF treatment plan, especially for those with specific mutations. It is taken orally as tablets or granules, usually once a day, along with a meal high in fat. Headache, upper respiratory tract infection, abdominal pain, diarrhea, rash, and elevated liver enzymes are among the frequently reported side effects. Generally speaking, these side effects are controllable and can be well watched during therapy.To ensure the quality and safety of ELX, it is required to develop analytical methods for the identification and estimation of impurities. The currently available literature reveals that the ELX drug combination with ivacaftor and tezacaftor is used very effectively. So, most of the analytical methods related to the estimation of three drugs simultaneously quantitatively by using different analytical techniques, i.e., by high-performance liquid chromatography and liquid chromatography–mass spectroscopy. Several liquid chromatography-ultraviolet (LC-UV) methods <a href="javascript:void(0);">(6,7)</a> and liquid chromatography-tandem mass spectrometry (LC-MS/MS) <a href="javascript:void(0);">(8−15)</a> methods are available to simultaneously measure the concentration of different combinations of IVA/TEZ/ELX with metabolites in plasma or other biological fluids. However, we did not find the literature for the analysis of process-related impurities and degradation impurities. The methods available in the literature do not discuss the process-related impurities and the degradation impurities of the ELX drug substance; hence, a stability-indicating LC method was developed for identifying and estimating the process-related impurities and degradation impurities of the ELX drug substance. In this paper, we report on a new analytical method to the estimation of ELX and its six process-related impurities quantitatively by using an HPLC instrument. This new LC method is sensitive enough to detect impurities as low as 0.02%, which ensures there is no harm or risk to the patients from impurities; however, existing methods in the literature do not discuss the sensitivity of the potential impurities, which can harm the patients.The method has been validated according to current international guidelines; this method is specific and rugged for analysis. An experimental design constructed according to Quality by Design (QbD) can identify the individual effects as well as interactions of the critical method variables, such as organic ratio, pH of the buffer or mobile phase, flow rate, column oven temperature, and gradient composition. <a href="javascript:void(0);">(16−18)</a> It is a systematic approach to analytical method development that is risk-based, which helps to create robust and reliable analytical methods. The current robustness method was studied by utilizing the QbD-based Design of Experiments (DoE) with Design-Expert software.<h4>2. Materials and Methods</h4><h5>2.2. Instrumentation and Software</h5><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/210">Waters Alliance e2695 HPLC</a> with a quaternary pump was used for method development and analysis (34 Maple St, Milford, Massachusetts 01757, USA). Empower 3 software (Waters Corporations, USA) was used for data collection and processing. Mettler Toledo microbalance was used, on which weighing was done on an MX5 microbalance (Mettler Toledo, Columbus, Ohio, USA). A SevenMulti pH meter (Mettler Toledo Columbus, Ohio, USA) was used for estimation of the pH.<h5>2.3. HPLC Instrumentation and Conditions</h5>Waters Alliance’s e2695 LC system with the 2998 photodiode array (PDA) detector was used for method development, method validation, and forced degradation investigations. Using Empower software, data were gathered and processed. Using a Waters 2998 PDA detector, the peak homogeneity was investigated.<h5>2.3.1. Chromatographic Method Conditions</h5>The analysis of Elexacaftor employed the <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/1823">XBridge Shield RP18</a>, 150 mm × 4.6 mm, 3.5 μm column with 10 mm KH2PO4 in water, pH adjusted to 3.2 with phosphoric acid buffer, and showed positive and encouraging results. Furthermore, extensive trials were made on an XBridge shield RP column with various flow rate and gradient conditions. The optimum separation of all impurities and ELX was achieved on XBridge Shield RP18, 150 × 4.6 mm, 3.5 μm, with mobile phase A as buffer:methanol (98:2, v/v) and mobile phase B as acetonitrile:2-propanol:water (70:20:10, v/v/v), flow rate 0.7 mL/min; column temperature 27 °C; with binary gradient time (min)/B concentration (%): 0/5, 20/50, 60/85, 80/85, 82/5 and 90/5. All peaks were separated with good resolution and peak shape under these conditions and are shown in <a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/10.1021/acsomega.4c10834#fig2">Figure 2</a>. The diluent was a 40:60 v/v solution of water and acetonitrile that was also used to wash the needles.<h4>3. Results and Discussion</h4><h5>3.2. Optimized Chromatographic Conditions</h5>Based on the method developmental trials, it was found that Elexacaftor and related substances were not retained and separated as per the requirement in any of the screened conditions except the trial with XBridge Shield RP 18, 150 mm × 4.6 mm, 3.5 μm, mobile phase A as buffer:methanol (98:2, v/v) and mobile phase B as acetonitrile:2-propanol:water (70:20:10, v/v/v), flow rate 0.7 mL/min; column temperature 27 °C; with binary gradient time (min)/B conc (%): 0/5, 20/50, 60/85, 80/85, 82/5, and 90/5. All seven peaks were separated with good resolution and peak shape in this condition. The details of the finalized method conditions are mentioned in <a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/10.1021/acsomega.4c10834#tbl2">Table 2</a> for quantitating ELX and its related substances by using HPLC.<img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/ACS_Omega_2025_10_39_44885_44894_Table_2_Analysis_of_Optimized_HPLC_Method_Conditions_for_Elexacaftor_and_Its_Impurities_5fc5c933c5.jpg" alt="ACS Omega 2025, 10, 39, 44885–44894: Table 2. Analysis of Optimized HPLC Method Conditions for Elexacaftor and Its Impurities" srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_ACS_Omega_2025_10_39_44885_44894_Table_2_Analysis_of_Optimized_HPLC_Method_Conditions_for_Elexacaftor_and_Its_Impurities_5fc5c933c5.jpg 225w," sizes="100vw" width="1046" height="726">With the above chromatographic conditions, ELX and its related substances (Imp-A to Imp-F) got separated from each other with a resolution of more than 2.0, as shown in <a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/10.1021/acsomega.4c10834#fig3">Figure 3</a>.<img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/ACS_Omega_2025_10_39_44885_44894_Figure_3_Overlay_chromatogram_of_degradation_studies_b71797ad37.jpg" alt="ACS Omega 2025, 10, 39, 44885–44894: Figure 3. Overlay chromatogram of degradation studies." srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_ACS_Omega_2025_10_39_44885_44894_Figure_3_Overlay_chromatogram_of_degradation_studies_b71797ad37.jpg 245w," sizes="100vw" width="2096" height="790"><h5>3.3. Method Validation Results</h5>According to ICH requirements, <a href="javascript:void(0);">(19−23)</a> the created approach was validated, and the results are shown in <a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/10.1021/acsomega.4c10834#tbl3">Table 3</a>. In the presence of its process contaminants, the devised HPLC technique for ELX’s specificity was assessed. ELX and Imp-A-Imp-F are well separated from one another. Utilizing a photodiode array detector and HPLC, the analysis was completed. All of the peaks of ELX and its impurities were shown to be pure when the peak purity tool was employed on them, indicating the method’s specificity because no additional impurities were detected coeluting at the same retention period.<img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/ACS_Omega_2025_10_39_44885_44894_Table_3_Method_Validation_Summary_of_the_Estimation_of_Elexacaftor_and_Its_Impurities_Part_1_ffb1d7d057.jpg" alt="ACS Omega 2025, 10, 39, 44885–44894: Table 3. Method Validation Summary of the Estimation of Elexacaftor and Its Impurities_Part 1" srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_ACS_Omega_2025_10_39_44885_44894_Table_3_Method_Validation_Summary_of_the_Estimation_of_Elexacaftor_and_Its_Impurities_Part_1_ffb1d7d057.jpg 168w," sizes="100vw" width="1042" height="969"><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/ACS_Omega_2025_10_39_44885_44894_Table_3_Method_Validation_Summary_of_the_Estimation_of_Elexacaftor_and_Its_Impurities_Part_2_75f03ca18f.jpg" alt="ACS Omega 2025, 10, 39, 44885–44894: Table 3. Method Validation Summary of the Estimation of Elexacaftor and Its Impurities_Part 2" srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_ACS_Omega_2025_10_39_44885_44894_Table_3_Method_Validation_Summary_of_the_Estimation_of_Elexacaftor_and_Its_Impurities_Part_2_75f03ca18f.jpg 178w," sizes="100vw" width="1058" height="924"><h4>4. Conclusions</h4>For the measurement of Elexacaftor and its related substances (imp-A to imp-F and any other impurities), the suggested technique was optimized to give a sharp peak with a minimal tailing factor. This approach was found to be specific, accurate, linear, and economical. The approach offers a number of benefits, including cost-effectiveness, robustness, and increased sensitivity. It was the first time we developed a method to estimate the content of Elexacaftor drug alone in process development. The current technique has been demonstrated to be efficient in terms of cost and may be utilized to measure Elexacaftor and its related compounds in the bulk. ICH rules were followed in the method’s validation.

Quality-by-Design-Driven RP-HPLC Method Development and Validation for Impurity Analysis of Elexacaftor, a Cystic Fibrosis Drug, with LC-MS/MS-Based Degradant Identification

This study evaluated the effects of prolonged proton pump inhibitor (PPI) administration on mineral nutrient bioavailability using a rat model. Animals treated with omeprazole for up to 60 days were assessed for physiological, biochemical, and hematological changes, alongside elemental analysis using ICP-MS.Results showed significant alterations in blood markers and imbalances in essential elements such as iron, copper, and calcium in both blood and organs. These findings indicate that long-term PPI use may impair nutrient absorption and physiological stability, underscoring potential risks of mineral deficiency associated with extended PPI therapy.<blockquote><h4>The original article</h4><h4><a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/10.1021/acsomega.5c07700">Evaluation of the Long-Term Administration of Proton Pump Inhibitors (PPIs) in the Mineral Nutrient’s Bioavailability</a></h4>Andréa Santana de Brito, Angerson Nogueira do Nascimento*, Fernando Luiz Affonso Fonseca, Alexandre Minami Fioroto, Giuliana Petri, and Rafaela Garcia Vidigal do NascimentoACS Omega 2025, 10, 46, 56085–56095<a target="_blank" rel="noopener noreferrer" href="https://doi.org/10.1021/acsomega.5c07700">https://doi.org/10.1021/acsomega.5c07700</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.The human body requires a diverse array of nutrients, each fulfilling distinct physiological roles that underpin both health and disease prevention. These compounds, broadly divided into macronutrients such as proteins, carbohydrates, fats, and micronutrients, are obtained primarily through the diet. While macronutrients are consumed in larger quantities to supply energy and support tissue growth and repair, micronutrients, including a variety of vitamins and minerals, are needed in much smaller amounts. <a href="javascript:void(0);">(1−4)</a>Minerals can be further subdivided into macroelements and microelements, depending on the amounts required by the body. <a href="javascript:void(0);">(5)</a> Macroelements such as calcium, magnesium, and potassium are needed in higher concentrations and participate in structural, neuromuscular, and hydroelectrolytic balance functions. Microelements, including iron, zinc, and copper are required in trace amounts, however, they play crucial roles as enzyme cofactors, antioxidants, and regulators of immune function. <a href="javascript:void(0);">(6)</a>Among these minerals, calcium is critical for blood clotting, neuromuscular excitability, and nerve impulse transmission. Iron is essential for hemoglobin production and is a component of enzymes such as cytochrome oxidase, catalases, and dehydrogenases found in skeletal muscle. <a href="javascript:void(0);">(7−9)</a> Copper contributes to iron mobilization for hemoglobin synthesis and functions as a catalytic cofactor of cuproenzymes, which are necessary for cellular respiration, neurotransmitter biosynthesis, antioxidant defense, and connective tissue formation. <a href="javascript:void(0);">(10,11)</a> Zinc is involved in cell replication, phagocytic activity, sexual maturation, fertility, and reproduction. <a href="javascript:void(0);">(12)</a> Magnesium and potassium are essential for cardiac function, skeletal muscle contraction, and cellular respiration. <a href="javascript:void(0);">(13−15)</a> Deficiency in these nutrients can lead to disorders such as anemia, osteoporosis, arrhythmia, and chronic kidney disease. <a href="javascript:void(0);">(16−18)</a>Considering the importance of these elements in the human diet and their contributions to physiological functions, numerous bioaccessibility studies have been conducted to identify and quantify nutrients in foods. <a href="javascript:void(0);">(19)</a> However, while total nutrient concentrations provide insights into the chemical composition of foods, they do not necessarily reflect the amounts absorbed by the body. <a href="javascript:void(0);">(1,2)</a> Several factors influence nutrient bioavailability, one of which is the use of medications. For instance, proton pump inhibitors (PPIs) are particularly relevant in this context, as they are widely prescribed and concerns have been raised regarding their potential overuse. <a href="javascript:void(0);">(20−23)</a> Omeprazole, one of the most prescribed PPIs, is recommended for short-term use, typically not exceeding 8 weeks. Nevertheless, chronic and unregulated consumption is frequently observed, raising concerns about possible health risks. <a href="javascript:void(0);">(24)</a>PPIs act by increasing intragastric pH and significantly reducing hydrogen ion concentration, thereby hindering nutrient bioavailability during gastric transit. <a href="javascript:void(0);">(25,26)</a> Their use has been associated with adverse health impacts, including increased risk of infections due to suppressed gastric acidity, alterations in gastric microbiota, and bacterial overgrowth in the small intestine. <a href="javascript:void(0);">(27,28)</a> Moreover, long-term omeprazole administration may negatively affect kidney function, although the immunological mechanisms underlying PPI-induced toxicity remain unclear. <a href="javascript:void(0);">(29,30)</a>Current evidence suggests a potential impact of PPIs on nutritional status, which is potentially associated with undernutrition. However, existing studies in this field remain inconsistent. For instance, a study conducted on older hospitalized patients demonstrated no significant association between long-term PPI use and undernutrition. Conversely, in certain studies, PPI administration has been linked to weight gain. Additionally, a cardiology study indicated an association between PPIs and increased nutritional risks among patients undergoing rehabilitation following treatment for ischemic and valvular heart disease. These differences highlight the need for further investigations to evaluate the effects of PPIs on nutritional status. <a href="javascript:void(0);">(31,32)</a>In this context, this study aims to investigate the relationship between omeprazole administration and its potential effects on the absorption and bioavailability of Fe, Ca, Mg, Zn, Cu, and K. Furthermore, physiological parameters and hematological profiles were assessed in rats to provide complementary insights.<h4>Materials and Methods</h4><h5>Elemental Determination in Biological Samples</h5>The solutions resulting from acid digestion were analyzed by inductively coupled plasma mass spectrometry (ICP–MS, <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library?manufacturerItems=2&amp;search=icap+Q">iCAP Q</a>, Thermo Fisher Scientific, Cambridge, England) equipped with a quadrupole mass analyzer. Calibration and internal standard solutions for ICP–MS analysis were prepared from multielemental solutions (G1516 V and MICPG1583V, Quimlab Produtos de Quı́mica Fina Ltda, São José dos Campos, Brazil). Calibration and internal standard solutions were obtained by serial dilutions within the concentration range of 0.1–100 ppb. The internal standard concentration was fixed at 50 ppb. Intermediate solutions were prepared in 0.1% HNO3, with deionized water used for dilution. Linear regression was applied, and the limits of detection (LOD) and quantification (LQ) were calculated from ten measurements of the analytical blank. The instrumental parameters used in the operation of ICP–MS are described in <a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/10.1021/acsomega.5c07700#tbl1">Table 1</a>.<h4>Results and Discussion</h4><h5>Elemental Determination in Biological Samples</h5>The distribution of Fe, Cu, Mg, Zn, Ca, and K in different tissues was investigated to evaluate the effects of omeprazole administration on elemental homeostasis in rats. Synchrony among nutrient absorption, usage, and storage is essential for maintaining the physiological balance. Hence, a comprehensive evaluation of these elements is critical for identifying potential disturbances caused by drug exposure.Liver, stomach, and spleen samples were analyzed using ICP–MS. Despite the limited literature available on the effects of drugs on minerals and trace element concentrations in humans and animals, the application of ICP–MS for elemental determination in these tissues holds significant clinical and scientific relevance. <a href="javascript:void(0);">(48−50)</a> These organs were selected due to their essential roles in physiological processes. Elemental analysis provides valuable insights into their chemical composition, particularly given their participation in blood formation. Substantial alterations in their elemental composition may result in physiological complications. <a href="javascript:void(0);">(9,10,51)</a> The results are presented in <a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/10.1021/acsomega.5c07700#fig3">Figures 3</a>–<a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/10.1021/acsomega.5c07700#fig5">5</a>, with detailed discussions for each organ provided in the following sections.<img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/ACS_Omega_2025_10_46_56085_56095_Figure_3_Mean_concentrations_of_Cu_Mg_K_Zn_Fe_and_Ca_in_liver_determined_by_ICP_MS_6f22d04927.jpg" alt="ACS Omega 2025, 10, 46, 56085–56095: Figure 3. Mean concentrations of Cu, Mg, K, Zn, Fe, and Ca in liver determined by ICP–MS. Values are presented as mean ± standard deviation (μg/g). (a) Copper; (b) iron; (c) magnesium; (d) calcium; (e) potassium; and (f) zinc. The control group is represented in black, and the treatment group in blue. Statistical significance was determined by one-way ANOVA (p &lt;0.05)." srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_ACS_Omega_2025_10_46_56085_56095_Figure_3_Mean_concentrations_of_Cu_Mg_K_Zn_Fe_and_Ca_in_liver_determined_by_ICP_MS_6f22d04927.jpg 245w," sizes="100vw" width="2084" height="861"><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/ACS_Omega_2025_10_46_56085_56095_Figure_4_Mean_concentrations_of_Cu_Mg_K_Zn_Fe_and_Ca_in_stomach_determined_by_ICP_MS_bee33d2e31.jpg" alt="ACS Omega 2025, 10, 46, 56085–56095: Figure 4. Mean concentrations of Cu, Mg, K, Zn, Fe, and Ca in stomach determined by ICP–MS. Values are presented as mean ± standard deviation (μg/g). (a) Copper; (b) magnesium; (c) potassium; (d) zinc; (e) iron; and (f) calcium. The control group is represented in black, and the treatment group in blue. Statistical significance was determined by one-way ANOVA (p &lt;0.05)." srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_ACS_Omega_2025_10_46_56085_56095_Figure_4_Mean_concentrations_of_Cu_Mg_K_Zn_Fe_and_Ca_in_stomach_determined_by_ICP_MS_bee33d2e31.jpg 245w," sizes="100vw" width="2084" height="861"><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/ACS_Omega_2025_10_46_56085_56095_Figure_5_Mean_concentrations_of_Cu_Mg_K_Zn_Fe_and_Ca_in_spleen_determined_by_ICP_MS_5654555ada.jpg" alt="ACS Omega 2025, 10, 46, 56085–56095: Figure 5. Mean concentrations of Cu, Mg, K, Zn, Fe, and Ca in spleen determined by ICP–MS. Values are presented as mean ± standard deviation (μg/g). (a) Copper; (b) magnesium; (c) potassium; (d) zinc; (e) iron; and (f) calcium. The control group is represented in black, and the treatment group in blue. Statistical significance was determined by one-way ANOVA (p &lt;0.05)." srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_ACS_Omega_2025_10_46_56085_56095_Figure_5_Mean_concentrations_of_Cu_Mg_K_Zn_Fe_and_Ca_in_spleen_determined_by_ICP_MS_5654555ada.jpg 245w," sizes="100vw" width="2084" height="861"><h4>Conclusion</h4>This study evaluated the effects of omeprazole administration on the absorption and bioavailability of essential nutrients, focusing on Fe, Ca, Mg, Zn, Cu, and K. Integrated analysis of hematological and biochemical profiles, along with the elemental composition of rat organs, revealed that omeprazole treatment significantly altered mineral homeostasis and relevant physiological parameters. Evidence of iron deficiency anemia was observed, characterized by reduced circulating Fe, decreased hemoglobin levels, lower red blood cell counts, and altered hematimetric indices. In addition, reductions in Cu levels may impair intestinal Fe reabsorption. Alterations in Ca, Mg, and K concentrations also indicate potential effects on bone metabolism and cardiovascular function.Overall, these results support the hypothesis that prolonged omeprazole use may interfere with nutrient absorption and promote systemic imbalances. Further investigations with extended treatment periods are recommended, particularly considering the chronic use of proton pump inhibitors in clinical practice.

Evaluation of the Long-Term Administration of Proton Pump Inhibitors (PPIs) in the Mineral Nutrient’s Bioavailability

The expansion of hop cultivation in Brazil has increased interest in understanding its chemical characteristics. This study compared three Brazilian hop cultivars (Comet, Cascade, and Sorachi Ace) with imported hops using GC×GC–MS and chemometric tools, focusing on essential oils and α- and β-acids.Results showed that Brazilian hops exhibited chemical profiles similar to imported hops of the same cultivar, clustering primarily by cultivar. While imported hops contained higher levels of myrcene and β-pinene, Brazilian hops showed elevated concentrations of several sesquiterpenes, highlighting their promising potential for the brewing industry.<blockquote><h4>The original article</h4><h4><a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/10.1021/acsfoodscitech.5c00718">Comparative Assessment of the Chemical Composition of Locally Cultivated and Imported Hops (Humulus lupulus L.) in Brazil Using Chemometrics</a></h4>Letícia Fagundes Pereira, Stanislau Bogusz Júnior, Leandro Wang Hantao, Gabriela Aguiar Campolina, Amanda Francine Minetto, Andre Luis Carvalho Souza, Lucas Barboza de Mori, Maria das Graças Cardoso, Cleiton Antônio Nunes, and Marcio Pozzobon Pedroso*ACS Food Sci. Technol. 2025<a target="_blank" rel="noopener noreferrer" href="https://doi.org/10.1021/acsfoodscitech.5c00718">https://doi.org/10.1021/acsfoodscitech.5c00718</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.Hops, responsible for imparting bitterness, flavor, and characteristic aroma to beer, have gained increased prominence in recent years, driven by changes in consumer preferences and the growing appreciation for beverages with differentiated sensory attributes. <a href="javascript:void(0);">(1)</a> In this context, hops have come to be used in much larger quantities than in traditional brewing methods, aiming to produce beers with more intense flavors and aromas. This increase in usage, along with the adoption of irrigation methods, genetic improvements, and the development of more efficient pesticides and fertilizers, has contributed to the global expansion of hop cultivation. <a href="javascript:void(0);">(2−4)</a>Hops are originally cultivated in temperate regions, with the United States and Germany being the largest producers, accounting for approximately 77% of global production. As cultivation has expanded, hop-growing regions have spread to various parts of the world, including Australia, New Zealand, South Africa, and Brazil. In Brazil, the growing number of breweries has driven higher hop consumption. As one of the world’s largest beer producers, the country relies heavily on imports, which reached about 57 million USD in 2020. This high demand, coupled with the need to lower production costs, has fostered the development of domestic hop cultivation. <a href="javascript:void(0);">(5,6)</a>The first hop harvests in Brazil date back to 2017, and the crop has been expanding nationwide. In 2023, hop cultivation areas increased by 113% compared to 2022, totaling approximately 112 ha, with a focus on the southern and southeastern regions, because in some parts of the country, the shorter natural photoperiod requires the use of supplemental lighting. <a href="javascript:void(0);">(7,8)</a> This new scenario demands studies that evaluate everything from the genetic conditions of hop seedlings to the characteristics of hops used in brewing.The quality and characteristics of hops can be influenced by several factors. Among the most relevant are the degree of ripeness at harvest, processing and pelletization methods, moisture control, and storage conditions. Additionally, chemical properties such as the content and composition of essential oils, as well as levels of α-acids and β-acids, are highly relevant to the aroma and bitterness attributes. <a href="javascript:void(0);">(9)</a> These characteristics are directly related to hop quality and the attributes they confer to beer, with an intrinsic relationship between chemical composition and sensory properties. Thus, the use of techniques to determine chemical characteristics is a valuable parameter for evaluating hop quality, highlighting the importance of understanding their chemical composition. <a href="javascript:void(0);">(10−12)</a>Resins make up about 10 to 30% of hop dry matter and contain α- and β-acids that contribute to beer bitterness. <a href="javascript:void(0);">(13,14)</a> On the other hand, essential oil imparts the characteristic hop aroma and flavor to beer and is composed mainly of hydrocarbons (50 to 80%) and oxygenated compounds (up to 30%). <a href="javascript:void(0);">(15−17)</a>Considering the importance of hop chemical composition, hop quality can be comparatively assessed. The quality of Cascade hops grown in Sardinia was evaluated in comparison with hops cultivated in the United States and New Zealand. The levels of α- and β-acids and essential oil composition were assessed, and compatible proportions of these acids and oil compounds were found across the different samples. <a href="javascript:void(0);">(18)</a> Hops from different cultivars cultivated organically and conventionally in Brazil were also compared in terms of essential oil composition and α- and β-acid levels. Minor chemical composition variations were observed among the different cultivars and within the same cultivar across the two cultivation methods. <a href="javascript:void(0);">(19)</a> The essential oil composition of Cascade hops cultivated in Brazil was compared with samples of the same cultivar grown in the United States. The essential oils of the Brazilian samples showed lower levels of myrcene, humulene, and caryophyllene, and higher levels of trans-β-farnesene, β-selinene, and α-selinene than those from the U.S. samples. <a href="javascript:void(0);">(20)</a> In another study, cones of Cascade and Chinook cultivars grown in Brazil were compared with commercial pellets of the same cultivars imported from the United States, considering the content and composition of essential oils. The results showed that 40% of the Brazilian samples presented essential oil content within the expected range, and regarding composition, the hops were mainly differentiated by cultivar type, with no distinction between Brazilian-grown hops and commercial pellets. <a href="javascript:void(0);">(21)</a>Additionally, the adaptation of some hop cultivars to the northeastern region of Brazil has been evaluated. When comparing bitter acids, xanthohumol, and essential oils from hop flowers to commercial hop pellets, a similar profile was observed among samples from different growing locations, despite being in different hop forms. <a href="javascript:void(0);">(22)</a> Comparisons between hops grown in Brazil and imported cultivars have also been conducted using extracts obtained with dichloromethane <a href="javascript:void(0);">(23)</a> and through the volatile profile of the samples. <a href="javascript:void(0);">(24)</a> In both cases, differences were observed between Brazilian and imported samples, with compounds identified as being distinct among hops grown in different regions.These findings demonstrate that hops of the same cultivar may exhibit different chemical characteristics depending on the cultivation region, resulting in site-specific properties and generating a regional identity. <a href="javascript:void(0);">(25)</a> However, considering the expansion of hop cultivation in Brazil, there are still few studies involving Brazilian hops and the evaluation of their chemical characteristics. Furthermore, there is a lack of studies assessing bitter acids and essential oils obtained through official methods, and comparing different hop cultivars cultivated and marketed in Brazil with the same imported cultivars, which are currently the most commonly used in beer production. Therefore, this study investigates the chemical characteristics of three hop cultivars (Cascade, Comet, and Sorachi Ace) produced and marketed in Brazil, comparing them with imported hops of the same cultivars.<h4>2. Material and Methods</h4><h5>2.4. GC × GC–MS and GC × GC–FID Analyses</h5>To perform chromatographic analyses, essential oil samples were diluted to obtain 5% (v/v) solutions in hexane and were analyzed in triplicate. A GC × GC system was a <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=3&amp;search=TRACE+1300">TRACE 1300 chromatograph</a> equipped with an FID and a transmission quadrupole mass spectrometer (QMS) (Thermo Fisher Scientific-Waltham, MA, USA). Samples were introduced using the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/63">TriPlus RSH autosampler</a>, into which 1 μL of sample was injected. The injector was operated at 250 °C with a split ratio of 1:10. The oven temperature program started at 60 °C, which was maintained for 3 min, and then the temperature was increased at 3 °C min–1 to 210 °C. Helium was used as the carrier gas at a constant flow rate of 0.5 mL min–1. The auxiliary gas was maintained at 20 mL min–1. Flow modulation was performed using an INSIGHT modulator (SepSolve Analytical–Waterloo, Canada). The modulation period was 5 s. The columns used in the first and second dimensions were Rxi-5 ms of 30 m × 0.25 mm (0.25 μm) and Rxi-17 ms of 5 m × 0.25 mm (0.25 μm) columns, respectively. Further analytical details are provided in our previous papers. <a href="javascript:void(0);">(27,28)</a> The FID temperature was 250 °C. For the mass spectrometer, the transfer line and ion source temperatures were 260 and 250 °C, respectively. Electron ionization (EI) was used to acquire the mass spectra in the m/z range of 50–350.For data acquisition, <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/1758">Xcalibur software</a> (Thermo Fisher Scientific–Waltham, MA, USA) was used, and the data were processed with GC Image software (GCI, TX, USA), allowing for the integration of the chromatographic peaks to obtain the peak areas. To identify the essential oil compounds, the mass spectra of each compound were compared with those contained in the NIST database, with a minimum similarity of 80% between the spectra required for compound identification. Furthermore, by injecting a homologous series of n-alkanes from C8 to C20, the linear retention indices (LTPRI) of the compounds were calculated using the van den Dool and Kratz equation. <a href="javascript:void(0);">(29)</a> The calculated LTPRI were then compared with those reported in the literature (NIST and Adams), with tolerated deviations of up to ±10 between the theoretical and experimental values. <a href="javascript:void(0);">(30)</a><h4>3. Results and Discussion</h4><h5>3.2. Essential Oils and GC × GC Analysis</h5>In addition to α- and β-acids, essential oils are another parameter of great importance for hop quality, and their composition should be evaluated. Thus, the results of the essential oils of hops are displayed in <a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/10.1021/acsfoodscitech.5c00718#fig3">Figure 3</a>, as well as the reference values for each cultivar reported by imported brands. The data were also subjected to ANOVA and Tukey’s test and the results are presented in <a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/suppl/10.1021/acsfoodscitech.5c00718/suppl_file/fs5c00718_si_001.docx">Table S2</a>.<img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/ACS_Food_Sci_Technol_2025_Figure_3_Essential_oil_content_of_hop_samples_3895b58b6f.jpg" alt="ACS Food Sci. Technol. 2025: Figure 3. Essential oil content of hop samples." srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_ACS_Food_Sci_Technol_2025_Figure_3_Essential_oil_content_of_hop_samples_3895b58b6f.jpg 245w," sizes="100vw" width="1365" height="626">When comparing the obtained levels of essential oils with those expected according to the range reported by reference brands, <a href="javascript:void(0);">(33)</a> Brazilian hops Comet cmB1, Sorachi Ace sB2 and sB3 presented values below expectations, while imported hops presented levels compatible. The I1 brand packaging specified that the yields considered the average of the last harvests, and variations may occur. Lower essential oil contents in Brazilian hops could be due harvest variation, but this information was not available to the consumer. These variations may occur, for example, as a consequence of changes in climatic conditions, which have been reported to influence the composition of bitter acids and essential oils in hops cultivated within the same region across different years. <a href="javascript:void(0);">(35)</a> In addition, lower values can be also associated with factors related to the processing steps of Brazilian hops. After harvesting, several factors contribute to the reduction of the amount of essential oil in hops, such as the drying and pelletizing processes and storage conditions, especially when there is no control of temperature, since high temperatures contribute to the volatilization and loss of essential oil. <a href="javascript:void(0);">(11,17)</a> The lower oil content of Brazilian hops may also be associated with plant age, as plants with less than three years of cultivation may not have reached sufficient maturity to produce the expected levels of essential oil. <a href="javascript:void(0);">(21)</a> However, this information was not available for the samples analyzed as they were currently available in the market, and the fact that hop cultivation in the country is recent suggests that some of them may have been obtained from plants younger than three years, resulting in pellets with essential oil content below the expected values.Finally, when comparing the essential oil content for each cultivar, it can be observed that the Brazilian Cascade hops presented levels equivalent to their imported counterparts and to values reported in the literature. <a href="javascript:void(0);">(18,20,36)</a> When applying ANOVA and the Tukey test (<a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/suppl/10.1021/acsfoodscitech.5c00718/suppl_file/fs5c00718_si_001.docx">Table S2</a>), it is noted that the two Brazilian samples are equivalent to the imported sample cI2, while the imported sample cI1, which presented a lower essential oil content, differs significantly from the samples cI2 and cB1. For the Comet cultivar, only the B2 brand was comparable to the imported samples, resenting essential oil content equivalent to that of the imported sample cmI2. For Sorachi Ace, none of the Brazilian samples matched the essential oil content of the imported ones and all samples presented essential oil contents that differed significantly from each other. Given that Brazilian hops had α-acid levels compatible with the imported cultivars but some exhibited lower essential oil content, it was essential to evaluate the composition of these oils to determine if the chemical profile of Brazilian hops was comparable to that of imported hops. Additionally, it was important to investigate whether there was a trend toward the production of specific compounds that might differentiate Brazilian hops from imported ones.<h5>3.3. Chemometrics</h5>To gain a deeper understanding of these differences, an exploratory data analysis was conducted using unsupervised HCA and heat map construction. This analysis aimed to identify clusters among the samples. The HCA shown in <a target="_blank" rel="noopener noreferrer" href="https://pubs.acs.org/doi/10.1021/acsfoodscitech.5c00718#fig4">Figure 4</a> reveals clustering based on hop cultivar, without distinctions related to sample origin. Additionally, it was possible to identify the most prominent variables for each cultivar, with a consistent pattern observed in samples of the same cultivar, regardless of their origin. Another notable finding is the clustering of both imported and Brazilian samples, observed in the I2 and B2 brand samples of the Comet cultivar, as well as in the I1 and B1 brand samples of the Cascade cultivar. For the Sorachi Ace cultivar, it is observed that the sB2 sample is grouped with the imported samples sI1 and sI2, indicating a greater similarity between their characteristics than the sB3 sample. Similarly, for the Comet cultivar, the B2 brand sample also grouped with the imported ones, which may be evidence of the greater proximity of the samples of this brand with the imported hops. It is also possible to observe the clustering between the Sorachi Ace and Cascade samples, suggesting similarities between these two cultivars. Both have an aroma profile in which the sweet fruity and citrus characteristics stand out, which should contribute to this clustering. <a href="javascript:void(0);">(32)</a><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/ACS_Food_Sci_Technol_2025_Figure_4_Heat_map_of_the_triplicate_of_hop_essential_oil_of_cascade_c_comet_cm_and_sorachi_ace_s_samples_and_HCA_of_samples_and_compounds_9f655428c7.jpg" alt="ACS Food Sci. Technol. 2025: Figure 4. Heat map of the triplicate of hop essential oil of cascade (c), comet (cm) and sorachi ace (s) samples, and HCA of samples and compounds." srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_ACS_Food_Sci_Technol_2025_Figure_4_Heat_map_of_the_triplicate_of_hop_essential_oil_of_cascade_c_comet_cm_and_sorachi_ace_s_samples_and_HCA_of_samples_and_compounds_9f655428c7.jpg 245w," sizes="100vw" width="1741" height="862">In view of the results presented, there are similarities between hops grown in Brazil and their imported counterparts, which demonstrate great potential for Brazilian production. Nevertheless, there is a need for greater attention to the postharvest processing steps to ensure the integrity of essential oils and mitigate losses. Regarding the aromatic characteristics of hops, PLS-DA analysis revealed some differences for those grown in Brazil, with a higher concentration of some essential oil compounds, such as selinene isomers, than in imported hops, which may indicate specific characteristics of hops grown in Brazil. However, this conclusion cannot be definitively drawn due to the limited number of hop samples, batches and cultivars evaluated. Therefore, future analyses require a larger number of samples, including those from different batches and harvests, to confirm the evidence observed in this study. Furthermore, future work would also benefit from a more comprehensive evaluation of the chemical and sensory characteristics of hops, along with a sensory analysis of beers produced with these hops, to determine whether these compounds contribute unique attributes to Brazilian hops. Nevertheless, this study represents an important initial assessment of the quality of Brazilian hops and provides a basis for more comprehensive future investigations.

Comparative Assessment of the Chemical Composition of Locally Cultivated and Imported Hops (Humulus lupulus L.) in Brazil Using Chemometrics

Our Library never stops expanding. What are the most recent contributions to LabRulezGCMS Library in the week of 22nd December 2025? 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: Analysis of Ethylene or Propylene Stream Cracking Gas Products</h3>Using the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=990+micro">Agilent 990 Micro GC</a><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_ethylene_propylene_stream_cracking_gas_products_5994_8803en_agilent_0cfe53e8f7.pdf">Full PDF for download</a></li></ul>Ethylene or propylene cracking gas products are produced from various feedstocks, including naphtha, light naphtha, atmospheric diesel, depressurized diesel, hydrotreating tail oils, ethane, and liquefied petroleum gas, among others.&nbsp;During gas cracking, yields of ethylene or propylene products should be monitored to measure the effectiveness of the process. The results of these analyses provide important process control data for optimizing cracking production and improving cracking yield—a key process parameter for cracking plants. Common cracking gas products are composed of hydrogen (H2 ), nitrogen (N2), and light hydrocarbons such as ethylene (C2H4), ethane (C2H6), propylene (C3H6), propane (C3H8), and 1-butene (C4H8), among&nbsp;others.&nbsp;The <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=990+micro">Agilent 990 Micro GC</a> enables fast and accurate detection of ethylene or propylene stream cracking gas products, a fundamental measure for determining the effectiveness of the cracking process. The system's demonstrated utility in refinery gas analysis further supports its suitability.<h4>Conclusion&nbsp;</h4>This study demonstrates the applicability of the Agilent 990 Micro GC for analyzing ethylene or propylene stream cracking gas products, providing essential process control data for optimizing cracking production and yield. Quantitation precision was evaluated through 10&nbsp;consecutive analyses of calibration standard gases, showing retention time (RT) repeatability (%RSD) less than 0.1% and area repeatability (%RSD) less than 1.0% for all compounds. These results confirm the instrument's excellent performance in reliably qualifying and quantifying these stream cracking gas&nbsp;products.<h3>2. EST Analytical: Purge and Trap Extraction of Tea Flavor Components</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_Tea_Flavor_Analysis_by_Purge_and_Trap_9bb392c2c1.pdf">Full PDF for download</a></li></ul>Purge and Trap (P&amp;T) sampling is a universally accepted technique for the analysis of volatile compounds in water. The United States Environmental Protection Agency (USEPA), the World Health Organization (WHO) and the American Society for Testing and Materials (ASTM) have all published methods using P&amp;T for water matrices. However, food and flavor manufacturers have yet to use this technique for the analysis of the volatile flavor components of their products. SPME has become the more accepted technique for flavor analysis.&nbsp;Both SPME and P&amp;T have their limitations. P&amp;T is recommended for volatile analytes and does not work when compounds have higher boiling points. Still, P&amp;T is a reliable technique that has the ability to purge out all of the volatile analytes of a system and detect very low concentrations of those analytes. On the other hand, SPME can be used for sampling a larger amount of semi-volatile compounds and fiber coating selection aids in better discrimination of analyte sampling. Yet, SPME is not an exhaustive sampling technique thus there are detection limitations to the technique. This application note will examine the analysis of white tea samples using P&amp;T sampling.&nbsp;<h4>Experimental</h4>The <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/2160">EST Analytical Evolution Purge and Trap</a> was set up with a Vocarb™ 3000 trap while the <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/2159">Centurion WS autosampler </a>was set to run in soil mode. The sampling system was configured to an <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=7890">Agilent 7890A Gas Chromatograph (GC) </a>and <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=5975C">5975C inert XL Mass Spectrometer (MS) </a>for separation and analysis. As the compounds of interest for this analysis were volatile, a Restek Rxi® 624 Sil MS 30m X 0.25mm X 1.8um column was affixed in the GC. Sampling and analysis parameters were optimized and are listed in Tables 1 and 2.<h4>Conclusions</h4>Using purge and trap to evaluate the flavor compounds of the tea samples was a reliable sampling technique. The findings were repeatable and the chromatography was excellent. The resulting flavor compounds were easily purged out of the tea matrix and as the technique is exhaustive, there was excellent detection of the flavor compounds in the system. This sampling technique established purge and trap to be an exceptional method for the determination of volatile analytes in tea.<h3>3. Shimadzu: Real-Time Measurement of CH4 and CO2 Concentrations for Estimating Methane Emissions from Rice Fields</h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_01_00887_en_adf24e951d.pdf">Full PDF for download</a></li></ul><h5>User Benefits</h5><ul><li>The portability of this gas analyzer means the user can decide where to place it, such as near a rice field, to continuously measure CH4 and CO2 emissions.&nbsp;</li><li>The CGT-7100 analyzer unit has a built-in pump, filter, dehumidifier, and other sample pretreatment equipment, so it does not require other equipment to perform measurements.</li><li>Data can be stored on a USB flash drive for easy editing on a computer or sharing with other departments.</li></ul>CH4 is a gas that has a greenhouse effect about 28 times greater*1 than CO2. One source of CH4 gas emissions is flooded rice fields. They release the CH4 gases generated by microorganisms living in the soil into the atmosphere. Since CH4 emissions from rice fields account for a significant proportion of greenhouse gases emitted from the agriculture, forestry, and fishery industry, various measures are being implemented to reduce emissions, such as managing the water and soil used in rice fields and improvingthe fertilizers used.&nbsp;The closed chamber method measures variations in gas concentrations due to gases exchanged with plants, such as rice. 1) In this article, a <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=1&amp;search=CGT-7100">CGT-7100</a> portable gas analyzer measures the concentration of CH4 and CO2 generated inside a specialized chamber placed on the surface of rice paddy soil.<h4>CH4 Emitted from Rice Fields&nbsp;</h4>The amount of CO2 emitted from a rice field depends on the amount breathed (emitted) from the rice plant and photosynthesized (absorbed), whereas the amount of CH4 emitted depends on the microorganisms in the soil. Fig. 2 illustrates the process of CH4 emission from rice fields. The microorganisms generate CH4 by decomposing organic matter in the soil. When a rice field is flooded with water, the supply of oxygen to the soil stops and anaerobic microorganisms actively generate CH4. It is thought that the generated CH4 is emitted into the atmosphere via two pathways. One pathway is via the roots and stalks of the rice plants (pathway 1).2),3) Due to the functions of the microorganisms, CH4 concentrations in the soil become higher than inside the plant, resulting in a concentration gradient that dissolves into the root cells. The dissolved CH4 becomes a gas within the narrow gaps between cells and moves along the gaps to the leaf sheath above ground. Pores on the leaf surface then discharge the CH4 into the atmosphere. In the other pathway (pathway 2), CH4 in the soil forms bubbles that are released directly into the atmosphere without passing through the rice plant. Pathway 1 increases the CH4 concentration inside the chamber by a certain proportion, but the quantity and frequency of CH4 emissions via pathway 2 are not clearly known, so there is an element of uncertainty about the estimated quantity of CH4 emitted from rice fields4). Therefore, the frequency that bubbles formed was estimated by analyzing the CH4 concentration measurement results to determine how quickly the CH4 concentration increasedper unit area (methane flux).<h4><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=1&amp;search=CGT-7100">CGT-7100 Portable Gas Analyzer&nbsp;</a></h4>The CGT-7100 is an all-in-one portable continuous gas concentration measuring system (Fig. 3). Because the compact main unit includes a pretreatment unit with a built-in electronic cooler for removing water moisture, a filter for removing dust, and a pump for suctioning sample gas into the analyzer system, the analyzer can be operated independently*2. Up to three components can be selected for measurement. In addition to two of the CO2, CO, and CH4 components being measured by the non-dispersive infrared absorption (NDIR) method, one component can also be selected for measurement by an O2 analyzer (optional), based on the limiting current type zirconia method. Changes in concentrations over time can be monitored with a wide range of measurements, from ppm to vol%. With the minimum sample gas flowrate of 100 mL/min (optional), gas concentrations can be measured in small sample quantities, and the sample gas flowrate can be varied within the range of 100 to 400 mL/min. As shown in the measurement process flow diagram below, samples can also be measured without losses by including a recirculation system that returns the sample gas discharged from the analyzer to the measurementlocation (inside the chamberin this case).<h4>Non-Dispersive Infrared Absorption (NDIR) Method&nbsp;</h4>The CGT-7100 uses the non-dispersive infrared absorption (NDIR) method for measurements. CO2 and other heteronuclear gases have unique infrared light absorption spectra. Gas concentrations can be measured selectively by passing infrared light through the sample gas and using the detector to measure the quantity of infrared light in the absorption band that is unique to a given type of gas. Robust and reliable measurements are achieved with the optical system in the NDIR unit, which has an excellent track record among online gas analyzers.<h4>Conclusion&nbsp;</h4>This article describes an example of using a CGT-7100 portable gas analyzer to estimate the amount of CH4 and CO2 emitted from a rice field by continuously measuring CH4 and CO2 concentrationsinside the chamberplaced in a rice paddy.&nbsp;Since the CGT-7100 is a continuous gas analyzer, it is ideal for measuringchangesin gas concentrationsin realtime. The CGT-7100 can be used to observe changes in the levels of CH4 and CO2 or the effects of bubble formation when implementing rice field water and soil management or fertilizer improvement measures.&nbsp;With its built-in sample gas pretreatment and sampling functionality, gas concentrations can be conveniently measured without the need for additional equipment, and the portability of the analyzer means it can measure gas concentrations in a wide variety of locations. If used with a communication unit, measurement data can be viewed and saved remotely via a computer or tablet to accommodate a wide range of testing and research applications.

News from LabRulezGCMS Library - Week 52, 2025

News from LabRulezLCMS Library - Week 52, 2025

Our Library never stops expanding. What are the most recent contributions to LabRulezICPMS Library in the week of 22nd December 2025? 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 Shimadzu!<h3>1. Agilent Technologies: Trace Elemental Analysis of Precursor Materials Using ICP-MS/MS</h3>Robust detection of Pt, Ag, Cd, and Ti in high-metal matrices using the <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library?manufacturerItems=1&amp;search=8900+ICP-QQQ">Agilent 8900 ICP-QQQ</a> and reactive cell gases&nbsp;<ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_precursor_materials_8900_icp_ms_5994_8841en_agilent_81f1d8ffb5.pdf">Full PDF for download</a></li></ul>Precursor materials are fundamental to the fabrication of integrated circuits (ICs). In atomic layer deposition (ALD), they enable the controlled growth of ultrathin films on semiconductor substrates—an essential capability for scaling advanced device architectures. Because even trace metal impurities in precursors can degrade film performance and device yield, both suppliers and manufacturers routinely analyze these materials. Due to its sensitivity and multi-elemental capabilities, inductively coupled plasma mass spectrometry (ICP-MS) is the industry standard for assessing elemental impurities in semiconductor materials.1 However, the high concentration of the metallic (high-matrix) content of precursors and the prevalence of polyatomic and doubly charged ion (M++) spectral overlaps arising from the matrix on key analytes present challenges for accurate analysis by single-quadrupole ICP-MS. At one time, high-resolution (HR)-ICP-MS (m/Δm up to 10000) was the best choice for solving these kinds of analytical problems. But some interferences require a resolution that exceeds the capability of current HR-ICP-MS instruments. In these cases, the samples are sometimes diluted to reduce the concentration of matrix elements, but dilution cannot totally solve the interference and may negatively affect detection limits.&nbsp;Triple quadrupole ICP-MS (ICP-QQQ or ICP-MS/MS) combined with collision/reaction (CRC) gases overcomes these limitations by selectively removing or avoiding interferences without compromising sensitivity. Agilent ICP-QQQ systems use two quadrupoles (Q1 and Q2) as unit mass filters, enabling MS/MS operation and the controlled use of reactive cell gases. Q1 controls which ions enter the CRC and Q2 controls which ions reach the detector.2–4&nbsp;In this study, we evaluated the performance of the Agilent 8900 ICP-QQQ to determine key analytes in three simulated precursor materials. Each sample contained a highconcentration matrix of hafnium (Hf), zirconium (Zr), or molybdenum (Mo), which cause interferences on platinum (Pt), silver (Ag), and cadmium (Cd) and titanium (Ti), respectively. To demonstrate the 8900 ICP-QQQ system’s ability to remove spectral interferences without sacrificing sensitivity, we quantified the four analytes in the three matrices using optimized instrument operating conditions.<h4>Experimental</h4><h4>Instrumentation&nbsp;</h4>An <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library?manufacturerItems=1&amp;search=8900+ICP-QQQ">Agilent 8900 Semiconductor configuration ICP-QQQ</a> (#200) fitted with the optional m-lens was used for all measurements. The 8900 #200 includes an inert (HF-resistant) sample introduction system comprising a 200 μL/min MicroFlow PFA nebulizer, a PFA spray chamber, endcap, and connector tube, and a demountable torch with a 2.5 mm internal diameter (id) sapphire injector. The cones comprised a Pt-tipped sampling cone and Pt-tipped, Ni-based skimmer cone for m-lens. The samples were self-aspirated using an Agilent SPS 4 autosampler. Hot plasma conditions (1% CeO+ /Ce+ ) were used during the analysis of the high-matrix samples.&nbsp;The 8900 ICP-QQQ was operated in MS/MS mode for all measurements. Ammonia (NH3 ) —plus a flow of helium (He) as a buffer gas—and oxygen (O2 ) were used as reactive cell gases to resolve the matrix-based interferences. Various CRC tuning modes and Q1–Q2 mass setting combinations were tested to obtain the best conditions for each analyte. The optimized operating conditions for the analysis are detailed in Table 1.<h4>Conclusion&nbsp;</h4>The Agilent 8900 Semiconductor configuration ICP-QQQ was evaluated for its ability to eliminate spectral interferences on four analytes—Pt, Ag, Cd, and Ti—in simulated semiconductor precursor materials using MS/MS and reactive cell gases. To accommodate challenging samples comprising Hf (500 ppm), Zr (500 ppm), and Mo (360 ppm) under hot plasma conditions (1% CeO+ /Ce+ ), the 8900 was equipped with the optional m-lens.&nbsp;Ammonia was applied in both on-mass and mass-shift modes to quantify Pt, Ag, and Cd at single-digit or sub-ppt levels. Oxygen on-mass mode effectively removed Mo-based doubly charged ion interferences on Ti, enabling accurate detection at single-digit ppt concentrations. Repeated analysis of the MoCl5 samples spiked at 50 ppt with %RSDs below 10% demonstrated the instrument’s robustness and consistent performance for ultratrace quantification in complex matrices.&nbsp;The 8900 ICP-QQQ delivered low background, high sensitivity, and reliable interference control, making it suitable for method development and trace-level screening of semiconductor materials.<h3>2. Metrohm: Fat content analysis in olive pomace with NIR spectroscopy</h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_nir_137_download_bb86ed4a7f.pdf">Full PDF for download</a></li></ul>Olive pomace is the main residue of the olive oil extraction process. It is a thick sludge – the remaining pulpy material after most of the oil is removed from the olive paste. To extract the remaining oil it contains, the olive pomace is treated with solvents. After refining and mixing this with edible virgin olive oil for flavor, aroma, and color, olive pomace oil is obtained. Olive pomace oil is used in cooking for its milder flavor and stability at high temperatures [1], as well as being nutritionally relevant due to its high oleic acid content (C18:1) [2]. Olive pomace fat analysis is necessary to check the efficiency of the oil removal process. The official method to determine this requires a time-consuming drying step followed by solvent extraction. Near-infrared spectroscopy (NIRS) is a fast, chemical-free method for olive pomace testing without any sample preparation.<h4>EXPERIMENTAL EQUIPMENT</h4>140 samples of olive pomace were measured on a <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library?manufacturerItems=56&amp;search=NIR+Analyzer">Metrohm NIR Analyzer</a>. All measurements were performed in reflection mode (1000–2250 nm) using the large cup accessory. The samples were measured in rotation to collect spectral data from several areas. Spectral averaging of signals from several spots helped to reduce sample inhomogeneity. Metrohm software was used for all data acquisition and prediction model development.<h4>RESULTS</h4>The obtained NIR spectra of olive pomace samples (Figure 1) were used to create a prediction model for quantification of fat content. The quality of the prediction model was evaluated using a correlation diagram (Figure 2) which displays a high correlation between the NIR prediction and the reference values measured with Soxhlet extraction. The respective figures of merit (FOM) display the expected precision of a prediction during routine analysis.<h4>CONCLUSION&nbsp;</h4>This Application Note shows the feasibility of using NIR spectroscopy for olive pomace fat analysis. By using NIRS, chemical-free analysis can be conducted within seconds—a quick, easy, cost-effective alternative to determine the efficiency of the olive pomace oil removal process.<h3>3. Shimadzu: Analysis of Pharmaceutical Raw Materials Compliant with ICH Q3D Guideline Using ICP-MS with Collision Mode</h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_01_00925_en_c760bf6c08.pdf">Full PDF for download</a></li></ul><h4>User Benefits</h4><ul><li>The 24 elements identified in the ICH Q3D guideline can be measured with high sensitivity.</li><li>Pharmaceutical raw materials that are dissolved in ethanol can be easily analyzed using the Shimadzu ICP-MS organic solvent system.</li></ul>The presence of impurities in pharmaceutical ingredients is a concern within the medical pharmaceutical industry. Therefore, the International Council on Harmonisation of Technical Requirementsfor Registration for Pharmaceuticalsfor Human Use requires the management of metallic impurities in pharmaceuticals through guidelines using ICP-MS (ICH Q3D) 1), 2) . This standard specifies the Permitted Daily Exposure (PDE) for 24 elements of toxicological concern in oral preparations, injectables, and inhalants.&nbsp;In the case of oral preparations, only the seven elements of Classes 1 and 2A are considered, except in instances where elements are intentionally added, such as when used as catalysts during synthesis. However, the sources of elemental impurities are diverse and include not only components such as active pharmaceutical ingredients and excipients but also manufacturing equipment and utensils.&nbsp;ICP-MS has the advantage of being able to analyze various trace elements simultaneously. It is often used for the analysis of elemental impuritiesin pharmaceuticals. The analyte for ICP-MS is usually a liquid sample, so solid samples require pretreatment.&nbsp;In this Application News, we measured three types of pharmaceutical raw materials and analyzed the impurities using the Shimadzu ICP-MS organic solvent system. Furthermore, the accuracy, precision, detection limits and specificity of 24 target elements are presented according to USP3), 4) and EP, assuming measurements below the Control Threshold of 30 % of the PDE.<h4>Instrument Configurations and Analysis Conditions&nbsp;</h4>Table 2 shows the instrument configuration for ICP-MS (<a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library?manufacturerItems=3&amp;search=ICPMS-2040">ICPMS-2040</a>). The organic solvent system was used to introduce the ethanol. By using the platinum sampling cone, damage from long-term exposure to organic solvents during analysis can be reduced. To reduce the labor required for sample preparation, the internal standards were added using the Online Internal Standard Kit. The analysis conditions are shown in Table 3.<h4>Accuracy and Precision Validation Results&nbsp;</h4>Measurements were carried out for n = 3 spiked samples with the target concentration of 50 % and 150 %, and n = 6 spiked samples with the target concentration and the blank (unspiked) sample. Spike recovery was calculated by averaging the quantitative values of all samples. Tables 6 to 8 show the measurement results.&nbsp;Accuracy: Spike recovery of the samples at each of the target concentrations of 50 %, 100 %, and 150 % was in the range of 94 % to 111 %, thereby satisfying the acceptance criterion. Precision (Repeatability): RSD of the spiked samples with the target concentration ranged from 0.27 % to 3.79 %, satisfying the acceptance criterion.&nbsp;Limit of quantitation: As accuracy for 50 % of the target concentration satisfied the acceptance criterion, the limit of quantitation could be confirmed.&nbsp;<h4>Specificity&nbsp;</h4>ICP-MS analysis often requires evaluation for potential interference by isotypes, polyatomic ions originating from Ar, oxides of coexistent elements and chloride ions. Here, the Cd was assessed. MoO, originating from the Class 3 element Mo, causes interference with Cd. A 1350 μg/L Mo solution (concentration equivalent to 1.5J) was analyzed, and the amount of interference with Cd was measured. Here, in addition to using collision gas, interelement correction was also performed. Table 5 shows the results.&nbsp;When the collision gas was used without interelement correction, interference by MoO was reduced but not eliminated. However, the quantitative value was below the lower limit of detection when the collision gas was used in combination with interelement correction. This result confirmed that the use of interelement correction, together with a collision gas, enables the appropriate correction of interference that could not be eliminated by the collision gas alone.<h4>Conclusion&nbsp;</h4>In this Application News, we measured three types of pharmaceutical raw materials and analyzed 24 elements indicated in the ICH Q3D guideline using the Shimadzu ICP-MS organic solvent system. In accordance with the pharmacopeias (USP, EP), the accuracy, precision, quantification limit, and specificity were confirmed. The results of the validation demonstrated that the performance meets the acceptance criteria with a sufficient margin. Based on the above, it was determined that the Shimadzu ICPMS-2040 is an effective analytical method for the 24-element analysis of pharmaceutical raw materials that can be dissolved in ethanol.

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