News from LabRulezGCMS Library - Week 19, 2025

The goal of this study was to develop and validate a sensitive and reliable analytical method for determining selected hydroxy derivatives of polycyclic aromatic hydrocarbons (OH-PAHs) in wastewater using gas chromatography-ion trap mass spectrometry (GC-ITQ-MS). Given the toxicological significance of OH-PAHs, the research aimed to optimize each stage of the analytical workflow—from extraction and derivatization to detection.The method was tailored to environmental samples and validated on real wastewater from the Płaszów treatment plant in Krakow. It enabled accurate quantification of OH-PAHs at nanogram-per-liter levels and also included a stability assessment of these compounds in the aqueous phase, revealing substantial degradation within hours.<blockquote><h4>The original article</h4><h4><a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325003176">Development of GC-ITQ-MS chromatographic system for the identification of hydroxy derivatives of polycyclic aromatic hydrocarbons in wastewater</a></h4>Justyna Pamuła, Elżbieta Sochacka-Tatara, Katarzyna Styszko&nbsp;Journal of Chromatography A, Volume 1752, 2025, 465969<a target="_blank" rel="noopener noreferrer" href="https://doi.org/10.1016/j.chroma.2025.465969">https://doi.org/10.1016/j.chroma.2025.465969</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.Humans have a significant impact on both the animate and inanimate nature, with consequences that include loss of biodiversity, climate change, urbanization, industrial development, and environmental pollution. Human activities continuously contribute to the release of increasing amounts of pollutants into the environment. The growing number of chemical compounds poses a threat to natural ecosystems and, more importantly, to human health and life [<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325003176#bib0001">1</a>]. Among these pollutants are polycyclic aromatic hydrocarbons (PAHs). Incomplete combustion processes are the primary source of PAHs emissions into the environment [<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325003176#bib0002">2</a>]. Research by global scientists indicates that the total estimated global emission of PAHs into the atmosphere comes from biofuels (56.7 %), with forest fires contributing 17.0 %. Other significant sources include the use of consumer products (6.9 %), car exhaust fumes (4.8 %), and combustion of household coal (3.7 %). Industrial activities contribute &lt;10 % of global PAH emissions, with coke production being the largest industrial source at 3.6 %. In particular, the volume of PAH emissions is positively correlated with gross domestic product (GDP) and negatively with average income [<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325003176#bib0003">3</a>]. Globally, biofuel combustion is the main source of PAHs, especially in countries with low GDP per capita such as India and China, where straw and wood are burnt for heat energy in rural areas [<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325003176#bib0004">4</a>]. In urbanized areas, PAHs are primarily emitted from automobile exhaust fumes and industrial activities [<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325003176#bib0005">5</a>].PAHs are present in all elements of the environment: water, soil, air, and food, allowing them to easily enter the human body [<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325003176#bib0002">2</a>,<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325003176#bib0006">6</a>]. PAHs have been an important focus in environmental pollution research for many years due to some being highly carcinogenic or mutagenic [<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325003176#bib0007">7</a>]. According to the International Agency for Research on Cancer (IARC), the most hazardous of the unsubstituted PAHs is benzo(a)pyrene, the only PAH classified as a group 1 human carcinogen [<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325003176#bib0008">8</a>]. Consequently, benzo(a)pyrene is commonly analyzed in the environment as a marker of carcinogenic risk associated with PAHs.PAHs are ubiquitous in the environment, leading to human exposure through skin contact, food ingestion, and inhalation [<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325003176#bib0002">2</a>,<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325003176#bib0009">9</a>] Once in the body, PAHs are transported through the bloodstream to tissues and organs. Due to their lipophilicity, they accumulate in adipose tissue, with their metabolism occurring mainly in the liver and bile ducts. PAH metabolites in the form of hydroxy derivatives (OH-PAHs) are excreted from the body within a few days [<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325003176#bib0010">10</a>]. OH-PAHs with lower molecular weight (fewer than four benzene rings) are excreted primarily in urine, while those with higher molecular weight (four or more rings) are mainly excreted primarily through bile and feces [<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325003176#bib0011">11</a>]. PAH metabolites are used as biomarkers of PAH exposure [<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325003176#bib0012">12</a>]. There is a need for improved sample preparation techniques that enable more efficient extraction of OH-PAH from the sample matrix. Innovative methods are proposed, including thin-film SPME membranes using polydimethylsiloxane (PDMS) in combination with Ordered Mesoporous Carbon [<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325003176#bib0013">13</a>], electromembrane extraction [<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325003176#bib0014">14</a>], or magnetic sorption on Fe3O4@HCP-BA, a magnetic composite consisting of magnetite (Fe3O4) and hyper-cross-linked boronic acid polymer (HCP-BA) [<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325003176#bib0015">15</a>].OH-PAHs have the potential to be more dangerous to living organisms than their parent compounds [<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325003176#bib0012">12</a>]. Despite the potential risk of OH-PAHs, there is limited research on their occurrence in the environment. Selected OH-PAHs have been determined in lake water [<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325003176#bib0016">16</a>], surface soil [<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325003176#bib0017">17</a>], and air particulates [<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325003176#bib0018">18</a>]. The only available study on OH-PAH concentration levels in wastewater is by Pojan and Marcomini, which used liquid chromatography coupled with a mass spectrometer [<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325003176#bib0019">19</a>].This research aimed to develop and validate a methodology for determining selected hydroxy derivatives of PAHs in wastewater using gas chromatography coupled with a mass spectrometer. Using the analytical method, the stability of these compounds in the sewage matrix was assessed, and preliminary tests were conducted on municipal sewage to determine the concentrations of OH-PAHs. Additionally, the research investigated the stability of selected OH-PAHs in wastewater.<h4>2. Experimental</h4><h5>2.3. Instrumentation</h5>The gas chromatograph coupled with a mass spectrometer (GC-ITQ-MS) used was a <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=3&amp;search=TRACE+1310">TRACE 1310</a> Thermo Scientific gas chromatograph equipped with a <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/1747">Thermo Scientific TG-SQC capillary chromatographic colum</a>n, 30 m in length, with an internal diameter of 0.25 mm, and a film thickness of 0.25 µm (filled with 5 % phenyl and 95 % methylpolysiloxane). The setup also included an <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=3&amp;search=ITQ+900">ITQ 900</a> Thermo Scientific ion trap mass spectrometer and a <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/422">Tri Plus RSH Thermo Scientific autosampler</a>. The identification of hydroxy derivatives of PAHs was enabled by the mass spectrometer. Destructive ionization of molecules was achieved using an EI energy of 70 eV. A single standard was subjected, after derivatization, to multiple analyzes in the SCAN detector mode, allowing the scanning of the entire mass spectrum range from 50 to 500 m/z. This enabled the determination of spectra for the compounds studied, which had been converted into volatile derivatives using BSTFA and MTBSTFA. Subsequently, optimal column operating conditions were selected to allow for the chromatographic separation of the OH-PAHs mixture.<h4>3. Result and discussion</h4><h5>3.2. Selection of chromatographic separation parameters</h5>The separation of compounds on a chromatographic column is determined by the operating conditions of the column. The selection of the appropriate chromatography temperature depends on the boiling points of the components of the mixture being separated [<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325003176#bib0023">23</a>]. According to <a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325003176#tbl0001">Table 1</a>, the range of boiling points of the compounds is 105 °C. In such cases, isothermal chromatography does not produce the desired results, leading to asymmetric, broad, and asymmetric peaks. Therefore, the column temperature programming is used. This involves maintaining a constant temperature for a certain period, then increasing it at a preset rate, and maintaining the new temperature for a specified duration.The development of optimal chromatographic separation began with the introduction of GC operating parameters presented in the work of Campo and colleagues [<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325003176#bib0024">24</a>]. The authors identified 12 hydroxy derivatives of PAHs in urine samples, including all those that were the subjects of the current investigation. However, the obtained chromatogram was not satisfactory, prompting the development of a new separation method for two derivatization reagents, BSTFA and MTBSTFA. The exact operating parameters of the GC are presented in Table A.1., in the appendices.<div>The analytical method was developed to enable qualitative and quantitative determination of hydroxy derivatives of PAHs in sewage. Real sewage is a mixture of many dissolved chemical compounds, which, when analyzed using GC-ITQ-MS, cause significant noise in the chromatogram. Given the high noise level when the analysis in SCAN mode, it was decided to develop a selective ion monitoring (SIM) method. This detector operating mode allows recording the current intensity only for selected ions with characteristic masses. The SIM method is particularly useful when a given compound is present in small amounts and when the matrix effect is significant, resulting in a reduced detection sensitivity. Based on the information in <a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325003176#tbl0002">Table 2</a> and the retention times of individual compounds, three time intervals were introduced during ion monitoring, increasing the sensitivity of the method. <a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325003176#fig0001">Fig. 1</a> shows chromatograms for wastewater enriched with standard solutions of selected OH-PAHs at a concentration of 3 µg/ml using the MTBSTFA derivatizer.<img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/Journal_of_Chromatography_A_Volume_1752_2025_465969_Fig_1_Chromatograms_for_wastewater_enriched_with_OH_PAH_standards_for_the_SIM_method_using_the_MTBSTFA_derivatization_reagent_67d468ce41.jpg" alt="Journal of Chromatography A, Volume 1752, 2025, 465969: Fig. 1. Chromatograms for wastewater enriched with OH-PAH standards for the SIM method using the MTBSTFA derivatization reagent." srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_Journal_of_Chromatography_A_Volume_1752_2025_465969_Fig_1_Chromatograms_for_wastewater_enriched_with_OH_PAH_standards_for_the_SIM_method_using_the_MTBSTFA_derivatization_reagent_67d468ce41.jpg 245w," sizes="100vw" width="2667" height="1601"><h4>4. Conclusion</h4>In this study, a GC-ITQ-MS-based method was developed and validated for the determination of selected hydroxy derivatives of polycyclic aromatic hydrocarbons (OH-PAHs) in wastewater. The method was optimized for solid-phase extraction (SPE) and derivatization, ensuring high recoveries and selectivity. The results confirmed that MTBSTFA is an effective derivatization reagent for all analyzed OH-PAHs, with optimized reaction conditions enhancing sensitivity. The method was successfully applied to real wastewater samples, identifying OH-PAHs in concentrations ranging from several to several hundred ng/L.<div>A comparative analysis with the HPLC-MS method of Pojana and Marcomini [<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325003176#bib0019">19</a>] revealed key differences in analytical performance (<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0021967325003176#tbl0005">Table 5</a>). GC-ITQ-MS demonstrated superior sensitivity (lower LOD and LOQ values) and selectivity due to the derivatization step and the use of Selective Ion Monitoring (SIM) mode. Additionally, the method allowed for the detection of a broader range of OH-PAHs in real wastewater samples. In contrast, HPLC-MS provided a simplified workflow by eliminating the need for derivatization, though at the cost of higher detection limits and a narrower range of detectable OH-PAHs.An important aspect of this research was the assessment of OH-PAH stability in wastewater, which highlighted significant degradation within the first few hours after sampling. These findings underscore the importance of immediate sample processing and appropriate storage conditions to prevent data distortion.The developed GC-ITQ-MS method offers a robust and sensitive tool for OH-PAH monitoring, significantly contributing to environmental analytical chemistry. Given the potential health and ecological risks posed by OH-PAHs, further research should focus on their behavior in wastewater treatment processes and their environmental fate. This work provides a solid foundation for future studies on OH-PAHs and their impact on aquatic ecosystems.</div></div>

Development of GC-ITQ-MS chromatographic system for the identification of hydroxy derivatives of polycyclic aromatic hydrocarbons in wastewater

In the week from May 5, the following webinars await you in the field of gas / solid phase and especially Raman, FTIR, GC and GC/MS.<blockquote><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/webinars">👉 DETAILS AND REGISTRATION IN THE WEBINARS SECTION</a>👉 Search and filter in the largest global database with over 4 500 GC, LC, MS and spectroscopy webinars.</blockquote><h5>1. Thermo Fisher Scientific: Food Integrity: Strategies to Ensure Authenticity and Combat Fraud</h5><ul><li>Wednesday, May 7, 2025, 15:30 CEST</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/webinar/5095">Registration</a></li></ul>Gain insights into the pressing challenges of food fraud and authenticity and discover the latest tools and technologies in food authenticity testing.<h5>2. Agilent Technologies: Multi-Residue Pesticide Analysis in Food: Regulations and Analytical Approaches</h5><ul><li>Wednesday, May 7, 2025, 19:30 CEST</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/webinar/5081">Registration</a></li></ul>In this webinar, we will discuss recent regulatory developments for pesticide residue analysis relevant to India and the South Asia-Pacific region.<h5>3. Thermo Fisher Scientific: Migration and Update of the Chromatography Data System</h5><ul><li>Thursday, May 8, 2025, 11:00 CEST</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/webinar/4829">Registration</a></li></ul>In this webinar, we will discuss the necessity of regular updates for the Thermo Scientific Chromeleon software, as well as the transition to newer operating systems or database platforms.<h5>4. Technology Networks/Agilent Technologies: The Role of Mass Spectrometry in Advancing Space Science</h5><ul><li>Thursday, May 8, 2025, 17:00 CEST</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/webinar/4950">Registration</a></li></ul>In this webinar, our expert speaker will discuss how mass spectrometry contributes to key areas of space science, including soil and environmental sample analysis.<h5>5. Agilent Technologies: Using the Analytical Target Profile (ATP) for Efficient Procedure Lifecycle Management</h5><ul><li>Thursday, May 8, 2025, 19:00 CEST</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/webinar/4876">Registration</a></li></ul>This presentation will explore ATP's key role in determining analytical procedure and performance criteria, guiding procedure design, validation, and ensuring continuous improvement.<h5>6. Agilent Technologies: Surfactant analysis by FTIR in cleaning products</h5><ul><li>Thursday, May 8, 2025, 20:00 CEST</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/webinar/5044">Registration</a></li></ul>This seminar covers how to identify and quantify actives and raw materials in cleaning products and quickly assess material quality using FTIR technology.

Webinars LabRulezGCMS Week 19/2025

In the week from May 12, the following webinars await you in the field of gas / solid phase and especially Raman, FTIR, GC and GC/MS.<blockquote><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/webinars">👉 DETAILS AND REGISTRATION IN THE WEBINARS SECTION</a>👉 Search and filter in the largest global database with over 4 500 GC, LC, MS and spectroscopy webinars.</blockquote><h5>1. Bruker: Enhancing Quality Control in Food and Feed Production</h5><ul><li>Wednesday, May 14, 2025, 09:00 CEST</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/webinar/5027">Registration</a></li></ul>Join us for an insightful online seminar where BRUKER and RETSCH will explore comprehensive QC solutions for food and feed production.<h5>2. Waters Corporation: 8th Annual Swiss BASF and Waters Workshop on Extractables and Leachables/Food Contact Materials</h5><ul><li>Thursday, May 15, 2025, 09:00 CEST</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/webinar/4772">Registration</a></li></ul>Waters AG and BASF Schweiz AG have the pleasure to invite you to the Annual Swiss Networking Workshop on Extractables and Leachables/Food Contact Materials.<h5>3. Wiley: Navigating the Challenges of Contaminants: Advanced Solutions and Insights on Microplastics and PFAS</h5><ul><li>Thursday, May 15, 2025, 10:00 CEST</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/webinar/5102">Registration</a></li></ul>Join us to explore key challenges of emerging contaminants like microplastics and PFAS. Discover advanced solutions for compliance and safety in water analysis and environmental monitoring.<h5>4. LECO: GCxGC-MS: The Gold Standard Approach for Fragrance Allergens Analysis</h5><ul><li>Thursday, May 15, 2025, 16:00 CEST</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/webinar/4952">Registration</a></li></ul>This webinar will showcase how comprehensive two-dimensional gas chromatography is a must-have technology for quantifying fragrance allergens with high confidence.<h5>5. Agilent Technologies: Ensuring Peak Performance: Comprehensive Guide to GC Column Care</h5><ul><li>Thursday, May 15, 2025, 16:00 CEST</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/webinar/4907">Registration</a></li></ul>Join us as we discuss proper column installation and handling for all Agilent GCs including the Intuvo 9000. We will also address the common modes of column degradation.

Webinars LabRulezGCMS Week 20/2025

Our Library never stops expanding. What are the most recent contributions to LabRulezGCMS Library in the week of 12th May 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 technical note by Agilent Technologies, application note by Shimadzu and poster by MDCW!<h3>1. Agilent Technologies: How Does Bleed Impact GC/MS Data and How Can It Be Controlled?</h3><ul><li>Technical note</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/te_bleed_impact_gc_ms_data_5994_7586en_agilent_1_728100a153.pdf">Full PDF for download</a></li></ul><h4>Understanding column bleed&nbsp;</h4>Column bleed remains one of the most commonly observed yet misunderstood aspects of mass spectrometry (MS) data. Bleed elevates chromatographic baselines and creates spectral interference, lowering the quality of and confidence in your data. To understand bleed, it must first be considered where the bleed originates. While columns come in a wide variety of phase types, the most commonly used columns today, such as the 1, 5, and 624, are categorized as wall-coated open tubular (WCOT) columns. These columns are composed of fused silica tubing (with varying internal diameters, measured in mm), internally coated with a thin film of stationary phase (with varying thicknesses, measured in μm), as shown in Figure 1. This coated stationary phase interacts with analytes and creates the selectivity and retention characteristics of the chromatography; but, these same characteristics are the origins of column bleed.Column phases can be made from a wide variety of polarities of liquid polymers with a polysiloxane backbone. When heat is applied, the terminal end of the stationary phase polymer starts to bend back and attack itself, which is called "backbiting." Ring structures, which are thermodynamically stable, become liberated and increase the noise and raise the baseline, as shown in Figure 2. The process is then repeated. The higher the temperature provided, the faster the reaction is driven, which is why there is an increase in baseline at temperatures above 300 °C.&nbsp;An increase in the rise of a baseline can be problematic for low signal-to-noise analytes, as peak integration can negatively impact data quality. Stable, flat baselines optimize the accuracy and repeatability of peak integration. When working with sensitive detectors, such as MS, an increase in the sensitivity of the detector also increases the background noise and bleed detection, causing excess column bleed to be detrimental to the sensitivity of trace level compounds.<h4>Experimental</h4>An Agilent<a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=1&amp;search=+8890+GC"> 8890 GC</a> coupled with a flame ionization detector (FID), and an Agilent <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=1&amp;search=5977B+GC%2FMSD+">5977 Series B GC/MSD </a>were used to collect data. Data acquisition was performed using Agilent <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=1&amp;search=OpenLab+ChemStation">OpenLab ChemStation</a> and <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=1&amp;search=MassHunter+acquisition+software">MassHunter acquisition software</a>. Additionally, an Agilent <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=1&amp;search=Intuvo+9000+GC">Intuvo 9000 GC</a> coupled with an FID was used to collect data. <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=1&amp;search=J%26W+DB-5Q">J&amp;W DB-5Q and J&amp;W&nbsp;HP‑5Q GC columns </a>were compared to various conventional, commercially available 5ms GC columns.<h4>Results and discussion&nbsp;</h4><h5>Comparisons of bleed profiles at upper temperature&nbsp;limits&nbsp;</h5>To compare the thermal stability of the HP-5Q columns to conventional 5ms columns, columns were installed on an 8890 GC equipped with dual split/splitless inlets and dual FIDs, and experiments were done in tandem. After confirming that column connections were properly installed, free of leaks, and conditioned, the oven temperature was ramped up to temperatures of 330 and 340&nbsp;°C and held for 10 minutes each. Then, the oven temperature was ramped to a final temperature of 350&nbsp;°C (the programed MAOT of the column phases) and held for 30 minutes. As shown in Figure&nbsp;4, both the DB-5Q and HP-5Q maintained ultralow FID response at the upper temperature limits, both maintaining column bleed levels below 1.0 pA at 340 °C. Also, when operating the columns at 350 °C (the programmed maximum temperature) over a period of 10 hours, both the DB-5Q and HP-5Q maintained bleed levels below 2.0 pA, while the conventional 5ms columns X and Y had bleed levels at 10 and 4 pA respectively, demonstrating the increased thermal stability of the DB-5Q and HP-5Q GC columns.<h4>Conclusion&nbsp;</h4>While column bleed is a normal phenomenon, there are ways to decrease its impact on the analysis and sensitivity of the detector being used. Improved column technology, with the introduction of the Agilent J&amp;W DB-5Q and HP-5Q GC columns, has provided an increase in thermal stability that dramatically reduces column bleed. The decrease in column bleed at high temperatures allows an increase in sensitivity of mass spectrometers, as the spectral interference from ions due to backbiting of column phase is reduced. This demonstrates that the DB-5Q and HP-5Q GC columns are optimal for use with sensitive detectors such as GC/MS, triple quadrupole GC/MS, and GC/Q-TOF.<h3>2. MDCW: Group-type quantitation of hydrocarbons in aviation fuel using GC×GC–FID&nbsp;</h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/2025_001_MDCW_ASTM_D8396_9a3aa6f3e5.pdf">Full PDF for download</a></li></ul>Accurate hydrocarbon composition of finished fuels, such as aviation fuel, is required to ensure quality control and to determine the effects of processes in fuel production. This has become even more important with the development of novel renewable fuels, such as sustainable aviation fuels (SAFs).Here, we demonstrate the use of reverse fill/flush (RFF) flow-modulated GC×GC–FID and automated group-type data processing to provide fast and accurate quantitative information on hydrocarbon composition.<h4>Experimental</h4><ul><li>Samples: A reference standard and reference blends of both diesel and aviation turbine fuel.&nbsp;</li><li>GC×GC: Modulator: INSIGHT®-Flow reverse fill/flush (RFF) flow modulator (SepSolve Analytical); Modulation period (PM): 7.8 s. Carrier gas: H2.&nbsp;</li><li>Column set: ASTM D8396 reverse phase column set (SepSolve Analytical, PN: OEM-SEP-COLKIT-10)&nbsp;</li><li>FID: Total H2 flow (column &amp; fuel): 50 mL/min; Air flow: 350 mL/min: Makeup gas flow: 5 mL/min; Temperature: 300 °C.&nbsp;</li><li>Software: <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?search=ChromSpace%C2%AE+GC%C3%97GC+software">ChromSpace® GC×GC software</a> for instrument control and data processing</li></ul><h4>Results and discussion</h4><h5>Optimising the GC×GC separation&nbsp;</h5>Separation was optimised using a custom column set and larger loop volume, enabling excellent separation of the key chemical classes (Figure 2).The INSIGHT-Flow modulator used in this study has an adjustable sample loop (in the range of 25-250 μL) for greater flexibility in method development. The reference standard was analysed in replicate (n=10) to assess method repeatability and precision. The relative standard deviation (RSD) of the raw peak areas were all &lt;2%, while the calculated mass percent values were consistently within 0.5% of the known composition.&nbsp;<h5>Group-type classifications&nbsp;</h5>Group-type analysis of these key chemical classes was then performed on various fuels using the ‘stencil’ workflow in ChromSpace software (Figure 3). Once a stencil is created, it can be saved and applied to multiple data files in an automated batch sequence to generate area percent reports. This means that the method is then scalable across multiple GC×GC–FID platforms for fast classification. This proven workflow has already gained accredited status in a number of high-throughput environmental labs for the analysis of total petroleum hydrocarbons (TPH).<h4>Conclusions</h4>This poster has shown an end-to-end workflow for ASTM Method D8396, specifically:&nbsp;<ul><li>Proven reverse fill/flush modulation using the INSIGHT-Flow, a modulator in operation in numerous high-throughput labs across the world.&nbsp;</li><li>Optimal class separation with a tried-and-tested column set.&nbsp;</li><li>Fast, straightforward group-type data processing with ChromSpace software.&nbsp;</li><li>Doubled productivity with optional dual-channel GC×GC technology.&nbsp;</li><li>A retrofittable solution for all popular GCs, allowing existing systems to be upgraded to GC×GC capability</li></ul><h3>3. Shimadzu: Analysis of Dechlorane Plus Residues in Environmental Water Using <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=1&amp;search=GCMS-TQ8050+NX">GCMS-TQ8050 NX</a> with Boosted Efficiency Ion Source(BEIS) and Long-Life Filament</h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_03_gcmsms_566_en_93e41bdffc.pdf">Full PDF for download</a></li></ul>User Benefits:<ul><li>The combination of the BEIS and long-life filament enables high sensitivity analysis while maintaining long-term stability.</li><li>The 13C-Dechlorane 602 is used as internal standard(IS) in the optimization method to avoid the interference of isotope IS with target components in MRM mode.</li></ul>Dechlorane Plus (DP) is a synthetic substance mainly used as an adhesive, sealant and flame retardant for polymers in the industrial field. Due to its strong persistence and bioaccumulation, there is a significant risk to human and environmental health. In 2018, the European Chemicals Agency (ECHA) identified it as a Substance of Very High Concern (SVHC), and in June 2021 proposed to add it to Appendix XVII of the REACH regulation to restrict it, proposing to ban the production and use of DPs and prohibit the production and launch on the market of goods with DP content equal to or greater than 0.1% (by weight). In May 2023, the Stockholm Convention on Persistent Organic Pollutants (POPs) listed DP in Appendix A. At the same time, DP is also included in China's List of new pollutants under Key Control (2023 version).&nbsp;A method for the determination of residues of DPs in environmental water was established by using the Shimadzu <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=1&amp;search=GCMS-TQ8050+NX">GCMS-TQ8050 NX</a> equipped with Boost Efficiency Ion Source and long-life filament. This application news provides an important analytical method for determine the residue levels of new pollutantsin environment with high sensitivity and good stability.<h4>Quantitative Analysis</h4>In the initial scheme, 13C-DP was used as the IS. However, due to the same retention time of 13C-DP and the target compound, the characteristic ions cause interference, resulting in a large calibration curve intercept and a high RF RSD (&gt;80%). Therefore, 13C-Dechlorane 602 is used as the IS instead. Its retention time differsfrom target DP, which helps avoid the interference.<h4>Evaluation of Durability in Analysis of Standard Solution and Samples</h4>The sample solution and 0.5 ng/mL standard solution were tested to evaluate the long-term durability of response. A total of 500 analyses of the sample and 80 analyses of standard solution were conducted. Fig.3 shows the durability test results of the standard solution. The horizontal axis shows the number of analyses, while the vertical axis shows the peak area ratio for each analysis number. The results indicate that the changes in peak area ratio and ion proportion were within ±20% of the average value (calculated from very beginning 20 injections).<h4>Conclusion</h4>A method for the determination of DP residues in environmental water was established by using the Shimadzu GCMS-TQ8050 NX combined with BEIS and long-life filament. The target compound exhibited good linearity in the concentration range of 0.2 to 50.0 ng/mL and the RF RSD of calibration curve was less than 15 %. The standard solution of 0.2 ng/mL was injected for 10 consecutive times to measure the LOD with results of 0.063 and 0.103 ng/mL. The durability of DP response was investigated by alternating test of sample solution and standard solution, and the peak area ratio in standard solution fluctuated within 20% in 500 injection of samples. The recovery rate of 1 ng/mL in blank samples was around 102 %. The method has high sensitivity and good repeatability and is suitable for the determination of DP residues in surface water, groundwater, industrial wastewater, and domestic sewage.

News from LabRulezGCMS Library - Week 20, 2025

The study aimed to develop a reliable GC–MS/MS method for multiresidue pesticide analysis in mealworm (Tenebrio molitor) larvae, which are known for their complex composition and high lipid content. The standard QuEChERS-based method was unsuitable for this matrix, so the authors optimized the extraction protocol by using 0.1% formic acid in acetonitrile and PSA-based cleanup to minimize matrix effects and improve analyte recovery.The final method enabled the detection and quantitation of 247 pesticides with high accuracy and low detection limits. Its application to field samples revealed triadimenol uptake from feed, indicating the method's practical utility. This approach provides a valuable tool for pesticide monitoring in edible insects for regulatory and industry purposes.<blockquote><h4>The original article</h4><h4><a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S2590157525002330">GC–MS/MS–based multiresidue pesticide analysis in mealworm (Tenebrio molitor) larvae: Optimization of standard QuEChERS-based method to minimize matrix effects</a></h4>Hyun Ho Noh, Chang Jo Kim, So-Hee Kim, Hye-Ran Eun, Yongho Shin, Won Tae Jeong&nbsp;Food Chemistry: X, Volume 27, April 2025, 102386<a target="_blank" rel="noopener noreferrer" href="https://doi.org/10.1016/j.fochx.2025.102386">https://doi.org/10.1016/j.fochx.2025.102386</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 consumption of animal products has increased with the increasing global population, and the demand for consumable crop–derived calories and proteins is expected to increase 2.1-fold by 2050 (<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S2590157525002330#bb0050">Hunter et al., 2017</a>). Given the need to promote sustainable food production, considerable attention has been drawn to decreasing the reliance of pest management on chemicals (<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S2590157525002330#bb0110">Rockstrom et al., 2017</a>). However, the fact that wheat, corn, and cotton losses due to pests reached 38.3&nbsp;% in 1964–2003 (<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S2590157525002330#bb0085">Poppe et al., 2003</a>) indicates the importance of pesticides for preventing crop damage by fungi, insects, mites, weeds, and other pests and thus securing stable food production (<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S2590157525002330#bb0015">Burger et al., 2008</a>). Additionally, climate and weather changes directly and indirectly affect crop production and pest reproduction, distribution, and migration. Thus, food production should be increased while reducing the use of chemicals (<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S2590157525002330#bb0090">Porter et al., 1991</a>).Insects are rich in proteins (40&nbsp;%–70&nbsp;%), minerals, and vitamins, thus holding promise as alternative protein sources for the food industry (<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S2590157525002330#bb0040">Gravel &amp; Doyen, 2020</a>). Over 2000 insect species are consumed in various countries, including those in Asia and Europe (<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S2590157525002330#bb0135">van Huis, 2020</a>). The production of edible insects is more environmentally friendly and sustainable than livestock farming (<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S2590157525002330#bb0030">FAO, 2013</a>), and the growth of the domestic and international insect market is expected to continue. Edible insects include members of the orders Lepidoptera, Coleoptera, Orthoptera, and Hymenoptera (<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S2590157525002330#bb0145">Yoo et al., 2013</a>). In particular, the larvae of the mealworm beetle (Tenebrio molitor) have a protein content of 46.44&nbsp;% and are nutritionally rich alternative food sources (<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S2590157525002330#bb0105">Ravzanaadii et al., 2012</a>). However, edible insects may contain harmful substances, such as microorganisms, chemicals, and parasites, with numerous studies reporting the detection of pesticides, including organophosphates and benzoquinones (<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S2590157525002330#bb0010">Belluco et al., 2013</a>).Pesticides are toxic to humans and the environment and can harm the immune, reproductive, and nervous systems. In response to the concerns related to pesticide residues in agricultural products and human exposure (<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S2590157525002330#bb0020">Damalas &amp; Eleftherohorinos, 2011</a>; <a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S2590157525002330#bb0065">Lushchak et al., 2018</a>), the European Union (EU) has established 464 maximum residue limits to regulate pesticides in terrestrial invertebrates, including insects (<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S2590157525002330#bb0025">EU, 2024</a>). In South Korea, the Rural Development Administration and Ministry of Food and Drug Safety set safety guidelines and residue limits for various crops, while the National Agricultural Products Quality Management Service and Ministry of Food and Drug Safety conduct safety investigations on harmful substances, including pesticide residues, in domestically produced and distributed agricultural products to ensure safe food production. However, no residue limits have been established for pesticides in edible insects in South Korea, which indicates the need to establish and monitor pesticide residue analysis methods, particularly for applying uniform PLS (positive list system) standards and future maximum residue limits.Owing to the high protein and fat contents of mealworm larvae, the analysis of pesticide residues therein requires pretreatment to prevent contamination (<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S2590157525002330#bb0105">Ravzanaadii et al., 2012</a>), as exemplified by protein and fat removal based on the QuEChERS method and n-hexane treatment (<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S2590157525002330#bb0045">Houbraken et al., 2016</a>; <a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S2590157525002330#bb0100">Ramluckan et al., 2014</a>; <a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S2590157525002330#bb0115">Shin et al., 2020</a>). Acetonitrile/hexane partitioning is necessary to improve the recovery rates of high-distribution-coefficient pesticides during gas chromatography-tandem mass spectrometry (GC–MS/MS) analysis (<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S2590157525002330#bb0120">Shin et al., 2018</a>). Additionally, adsorbents commonly employed in the QuEChERS method, such as primary secondary amine (PSA), C18, Z-Sep, Z-Sep+, and HLB (hydrophilic lipophilic balance), should be used to remove potential interferents from the extract. Herein, we aimed to (i) develop a method for the simultaneous analysis of multiple pesticides and related metabolites in mealworm larvae using a GC–MS/MS–based modified QuEChERS approach and (ii) validate the effectiveness of this method by applying it to real mealworm larvae. The method improves routine residual pesticide analysis procedures to provide a breakthrough the analysis of high-protein and high-fat samples.<h4>2. Materials and methods</h4><h5>2.4. Instrumentation</h5>Pesticide analysis was performed using an Agilent <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=1&amp;search=7000C+triple-quadrupole">7000C triple-quadrupole mass spectrometer </a>coupled with an Agilent <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=1&amp;search=7890B+gas+chromatograph+">7890B gas chromatograph </a>(Santa Clara, CA, USA). The carrier gas (helium) was supplied at a flow rate of 1 mL/min. Samples were injected in the solvent vent mode, and the vent flow rate was held at 50 mL/min for the first 1.5 min, decreased to 25 mL/min, and maintained (5 psi) for 0.3 min. The target analytes were separated on an HP-5 ms column (30 m × 250 μm × 0.25 μm). The oven temperature was held at 50 °C for 3 min, increased to 185 °C at 30 °C/min, 250 °C at 5 °C/min, and 300 °C at 10 °C/min, and held for 7 min. The source and transfer line temperatures were set to 250 and 290 °C, respectively. Electron ionization was performed at 70 eV, and all pesticides were analyzed in the dynamic multiple reaction monitoring mode.<h4>3. Result and discussion</h4><h5>3.1.2. Partitioning efficiency</h5>Mealworm larvae have a fat content of 21.9&nbsp;wt% (<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S2590157525002330#bb0055">Imathiu, 2020</a>) and should therefore be defatted prior to analysis to remove interferents and prevent the contamination of the GC–MS/MS instrument. Therefore, n-hexane, a nonpolar solvent effective for fat removal, was employed (<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S2590157525002330#bb0100">Ramluckan et al., 2014</a>). Additionally, n-hexane (partition coefficient&nbsp;=&nbsp;3.90) has a higher affinity than acetonitrile (partition coefficient&nbsp;=&nbsp;−0.34) and can therefore extract nonpolar pesticides that may remain in the extraction solvent. Using n-hexane-saturated acetonitrile, we examined the effect of partitioning frequency on recovery rates (<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S2590157525002330#t0010">Table 2</a>). Each additional partitioning led to a higher pesticide recovery, with four partitions yielding a 22 percentage point increase in recovery (84.6&nbsp;%) compared with a single partition. At this level, 209 pesticides demonstrated acceptable recovery rates (70&nbsp;%–120&nbsp;%) and precisions (RSD&nbsp;≤&nbsp;20&nbsp;%). Thiocarbamate and organochlorine pesticides exhibited low recovery rates, probably because of their high partition coefficients (log P&nbsp;=&nbsp;4.1–6.9) due to their low polarities, and were therefore retained in the n-hexane phase (<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S2590157525002330#bb0070">Mathieu et al., 2015</a>; <a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S2590157525002330#bb0075">Mdeni et al., 2022</a>). However, the recovery rates of these pesticides increased with the increasing partitioning frequency (<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S2590157525002330#f0005">Fig. 1</a>). Therefore, partitioning with n-hexane-saturated acetonitrile was concluded to be essential for improving the recovery of pesticides with high partition coefficients, and the optimal number of partitions was identified as four.<img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/Food_Chemistry_X_Volume_27_April_2025_102386_Fig_1_Recovery_rates_bars_and_partition_coefficients_log_P_triangles_of_10_representative_pesticides_2_79886fbb41.jpg" alt="Food Chemistry: X, Volume 27, April 2025, 102386: Fig. 1. Recovery rates (bars) and partition coefficients (log P, triangles) of 10 representative pesticides showing a strong dependence of recovery (>25 %) on the number of partitionings (N = 1, 2, 3, and 4). Error bars are the standard deviations of the recovery rates (n = 4)." srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_Food_Chemistry_X_Volume_27_April_2025_102386_Fig_1_Recovery_rates_bars_and_partition_coefficients_log_P_triangles_of_10_representative_pesticides_2_79886fbb41.jpg 245w," sizes="100vw" width="1600" height="957"><h5>3.3. Real sample analysis</h5>Among the 24 samples collected from domestic mealworm larva farms, 11 contained the triazole fungicide triadimenol at concentrations of 14–996&nbsp;μg/kg (<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S2590157525002330#f0020">Fig. 4</a>) and were therefore noncompliant with the EU residue limit for terrestrial invertebrates (10&nbsp;μg/kg). Considering that the triadimenol residue limit for wheat, the primary ingredient of bran fed to mealworms, is 100&nbsp;μg/kg, pesticide absorption probably occurred through bran consumption. Thus, the established method for the multiresidue analysis of 247 pesticides in mealworm larvae was concluded to be applicable in field settings and enable both quantitative and qualitative analyses.<img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/Food_Chemistry_X_Volume_27_April_2025_102386_Fig_4_Chromatograms_of_triadimenol_obtained_for_acetonitrile_control_pure_standard_2_c9e6bb0fed.jpg" alt="Food Chemistry: X, Volume 27, April 2025, 102386: Fig. 4. Chromatograms of triadimenol obtained for acetonitrile, control, pure standard (10 µg/kg), matrix-matched standard (10 µg/kg), and mealworm samples (6, 8, 15, 18, 20, 21, 22, 26, 28, 30, and 31)." srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_Food_Chemistry_X_Volume_27_April_2025_102386_Fig_4_Chromatograms_of_triadimenol_obtained_for_acetonitrile_control_pure_standard_2_c9e6bb0fed.jpg 187w," sizes="100vw" width="1436" height="1200"><h4>4. Conclusions</h4>A GC–MS/MS–based multiresidue method for the detection and quantitation of 247 pesticides in mealworm larvae was developed, optimizing the standard QuEChERS procedure to account for matrix complexity and high fat content, and validated. Pesticide recovery rates were maximized by combining 0.1&nbsp;% formic acid in acetonitrile (extraction solvent) with the original QuEChERS packet. Further cleanup (PSA d-SPE) effectively removed matrix interferences without significant analyte loss, enhancing detection accuracy. According to the results of validation tests, the developed method exhibited high linearities, acceptable recovery rates, and low detection limits for most analytes and was therefore concluded to be robust and suitable for both quantitative and qualitative analyses. The analysis of 24 field samples revealed detectable levels of triadimenol, suggesting its potential uptake from bran feed. Thus, this validated approach was concluded to be suitable for application in regulatory and industrial settings, offering a reliable tool for monitoring pesticide residues in mealworm larvae and similar edible insect matrices.

GC–MS/MS–based multiresidue pesticide analysis in mealworm (Tenebrio molitor) larvae: Optimization of standard QuEChERS-based method to minimize matrix effects

Our Library never stops expanding. What are the most recent contributions to LabRulezGCMS Library in the week of 19th May 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, poster by MDCW and technical note by Thermo Fisher Scientific!<h3>1. Agilent Technologies: Py-GC/MS/MS Microplastic Analysis of Samples Containing Interfering Substances</h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_microplastic_analysis_pygcmsms_5994_7637en_agilent_1_6caa53726f.pdf">Full PDF for download</a></li></ul>Microplastics, defined as plastic fragments with a particle size of 5 mm or less, originate from various products, such as cosmetics, clothing, food packaging, and plastic waste. Microplastics have been detected in water, soil, and air environments,5 as well as in food and within living organisms.7 Consequently, numerous analytical techniques are being developed to investigate the extent of microplastic contamination and its impacts.&nbsp;Microplastics can be seen with the naked eye or a microscope when the particle size is large, but observation is difficult when the size is small, and quantitative analysis by type of plastic is difficult. Techniques using spectroscopic instruments, such as IR or Raman, or thermal analysis instruments such as Py-GC/MS or thermal extraction desorption (TED)-GC/MS have been widely used.1, 2, 3, 4 IR and Raman spectroscopy can be used to identify the type, shape, size, and count of microplastics on filters after sample preparation and filtration. These techniques rely on spectroscopic analysis of the microplastics retained on the filter. For Py-GC/MS or TED-GC/MS, the microplastics collected on the filter are thermally decomposed, and the resulting compounds are analyzed with GC/MS, allowing for the quantification of each type of microplastic8 (by weight). In particular, Py-GC/MS has recently been recognized as an ASTM International method11 and is widely applied as an analytical method for analyzing microplastics in drinking water.12 In the case of environmental samples or food samples with complex matrices, additional matrix effects can negatively impact analytical performance or result in thermal decomposition products that cannot be separated from microplastic thermal decomposition product peaks, causing interference and overlapping with target ions.6&nbsp;In this application, we applied Py-GC/MS/MS (MRM mode) to microplastic analysis to determine whether accurate quantitative analysis of microplastics is possible even in samples containing complex matrices.<h5>Instrument and analysis conditions&nbsp;</h5>The instruments used were a Frontier Lab pyrolyzer (<a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=42&amp;search=Py-3030D">Py-3030D</a>) and an Agilent <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=8890+GC">8890 GC</a> coupled to a <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=10&amp;search=7000E+triple+quadrupole+gc%2Fms">7000E triple quadrupole GC/MS system</a>. The temperature of the pyrolyzer was set to 600 °C, as shown in Table 1, and the components produced by thermal decomposition were passed through the GC inlet (320 °C, split 50:1), cryo-focused by liquid nitrogen applied to the front end of deactivated metal capillary column (UA-5, 30 m x 0.25 mm x 0.25 µm) in the Microjet Cryo Trap, separated by the GC oven temperature program after about 3 minutes, and transferred to the mass spectrometer. The analysis conditions are shown in Tables 1, 2, 3, and 4.<h4>Results and discussion</h4><h5>Chromatogram</h5>Chromatograms resulting from the analysis of the microplastics calibration standard (MPCS) that includes 11 types of microplastics are shown in Figure 1 for both Scan and MRM modes. The Scan mode total ion chromatogram (TIC) can be processed into extracted ion chromatograms (EIC) to confirm the target ion (m/z) for each indicator peak, as seen on the left side of Figure 1. The MRM TIC and EIC are shown on the right side of Figure 1. As can be seen, MRM mode can reduce matrix interference and enhance selectivity. Calibration curves can be created using either Scan or MRM mode using concentration of the MPCS.<h4>Conclusion</h4>We have established a quantitative analysis method using Py-GC/MS/MS (MRM mode) for complex matrix samples and trace levels of microplastics.&nbsp;Under the established Py-GC/MS/MS (MRM mode) conditions, the linearity of the calibration curves generated for the 11 types of microplastics, ranging from several hundred ng to several µg, was excellent (R² &gt; 0.99). Compared to Scan (Target EIC) mode, noise is reduced by two to several times when analyzed in MRM mode, and accordingly, the S/N ratio is increased when analyzed in MRM mode, enabling the detection of microplastics with better selectivity. In addition, when there is matrix interference during sample analysis, more accurate quantitative results can be obtained by applying the MRM mode, and Py-GC/MS/MS (MRM mode) can be very useful for quantifying complex matrix samples and trace levels of microplastics.<h3>2. MDCW: Analysis of (micro-)plastic-associated chemicals released into marine environments by comprehensive multidimensional gas chromatography-mass spectrometry</h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/MDC_2025_Poster_d31ebb1c76.pdf">Full PDF for download</a></li></ul>Plastic materials contain many different chemicals, which include functional additives as well as trace levels of non-intentionally added substances. Plastic released into the environment acts as a vector for these chemicals, which may cause harm to exposed organisms. The complex mixture of chemical classes and concentrations within plastics is a challenge for analysis, which can be addressed through the use of multidimensional analytical approaches.&nbsp;Here, the chemical composition of different polymer samples was analysed using comprehensive multidimensional gas chromatography coupled to time-of-flight mass spectrometry. Ultrasonication assisted extractions with solvent represents a ‘worse-case-scenario’ in relation to environmental leaching, and provides a starting point for non-target analysis of microplastic leaching in marine environments.<h4>Results</h4>All the virgin polymer samples released chemicals under organic extraction. As shown in Figure 1, the Hexane DCM:MeOH MeOH EtOAc number of compounds released by each polymer was influenced by the solvent used for the extraction. Additionally, the conventional polymers released a higher number of chemicals than the biopolymers, particularly LDPE and PP.&nbsp;The high number of compounds released by LDPE and PP is due to the release of polymer-derived alkanes. The use of GC ×GC enabled separation and identification of other plastic-associated compounds from the alkane series (see respective chromatograms). In contrast, the other polymers released a range of compound classes. Some of the compounds identified in the extracts, for example phthalates, are detrimental to both human and environmental health.&nbsp;<h4>Conclusion</h4>Chemical extracts from several polymer samples demonstrated that virgin polymer samples contain chemicals which are not chemically bonded to the bulk polymer material – and therefore have potential to be released into the environment. Future leaching studies can be informed by the chemical identifications made, and increase the confidence that those compounds identified in leachates did originate from the respective polymer.<h3>3. Shimadzu: Quantitative Analysis of Furan and Alkylfuran in Processed Food Using a Triple Quadrupole GC-MS System and an SPME Arrow</h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_01_00876_en_96a8b1c14c.pdf">Full PDF for download</a></li></ul>User Benefits:<ul><li>Using an <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=1&amp;search=SPME+Arrow+">SPME Arrow </a>allows for highly sensitive analysis of furan and alkylfuran in processed food.</li><li>The MRM mode enables highly reliable analysis even in complex matrices.</li><li>An <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=1&amp;search=AOC-6000+Plus+autosampler">AOC-6000 Plus autosampler</a> helps increase productivity and repeatability through automated pretreatment.</li></ul>Furan and alkylfuran compounds are commonly found in many foods, including coffee. They are known as volatile organic compounds that contribute to aroma. However, recent studies in various countries have reported health concerns regarding these compounds and monitoring of furan and alkylfuran has been recommended in the EU1) .&nbsp;These compounds are frequently measured using the HSGC/MS method, which is convenient and effective when present at relatively high concentrations. However, for samples containing low concentrations, pretreatment for concentration is necessary. This Application News article describes a method using an SPME Arrow and GC-MS/MS system that enables more consistent analysis even at trace concentrations in complex matrix samples.<h4>Instrument Configuration and Analytical Conditions</h4>The analysis was performed using an AOC-6000 Plus multifunctional autosampler and a <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=1&amp;search=GCMS-TQ8040+NX">GCMS-TQ8040 NX </a>triple quadrupole gas chromatograph mass spectrometer system (Fig. 1). The AOC-6000 Plus is a multifunctional autosampler that can automatically switch between various sample injection methods, such as liquid injection, headspace injection, and solid-phase microextraction (SPME), depending on the sample and purpose (Fig. 2). In this analysis, an SPME Arrow, which offers improved durability compared to a traditional SPME fiber, was used forsample analysis. When using sampling methods involving concentration, such as the SPME method, matrix-derived impurities may also be concentrated, making it difficult to improve sensitivity due to interference from impurities. In this analysis, high sensitivity for analyzing furan in processed foods was achieved by using the SPME method in combination with the MRM mode of the triple quadrupole GC-MS system.<h4>Comparison of SIM and MRM</h4>To confirm the improvement in selectivity with MRM, analysis using the SIM mode was also conducted. Generally, the MRM mode of a triple quadrupole GC-MS system offers better selectivity compared to the SIM mode, leading to higher sensitivity and more consistent detection. Fig. 5 shows the SIM and MRM chromatograms of four components detected in baby food. While each component was detectable with both modes, the MRM mode provided higher selectivity, whereas the SIM mode was more susceptible to interference from impurities. Therefore, manual peak integration or changes to the quantitative ions may be required in the SIM mode depending on the sample.<h4>Conclusion</h4>Quantitative analysis of furan and alkylfuran in processed food was conducted using an SPME Arrow and a triple quadrupole GC-MS system. The AOC-6000 Plus multifunctional autosampler allows for highly sensitive and reproducible quantification of furan compounds using the SPME Arrow method. Additionally, by enhancing selectivity with the MRM mode of the triple quadrupole GC-MS system, more reliable analytical results were obtained.<h3>4. Thermo Fisher Scientific: Data-driven GC and GC-MS instrument monitoring with SmartStatus intelligent software&nbsp;</h3><ul><li>Technical note</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/tn_001883_gc_ms_gc_ms_ms_smartstatus_tn001883_na_en_99ce72eef2/tn-001883-gc-ms-gc-ms-ms-smartstatus-tn001883-na-en.pdf">Full PDF for download</a></li></ul>Rising costs can significantly impact an analytical laboratory’s profit margin, and it is crucial to maintain productivity and ensure maximum asset utilization to stay competitive. To balance increased overhead costs, including analytical gases and staff pay, laboratories must ensure that analytical instrumentation consistently produces results, without interruption. Re-analyzing entire runs due to drops in sensitivity, unnecessary downtime, and underutilization of consumables is expensive and time consuming.&nbsp;Thermo Scientific™ <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=3&amp;search=SmartStatus">SmartStatus</a>™ instrument tracking can help laboratories realize additional cost savings. This is done by using data-driven insights to accurately determine when to perform maintenance and replace consumables and parts, so that the system consistently runs smoothly for all samples and meets specifications in the initial analysis. This ensures that consumables and parts are replaced on the correct schedule and avoids excess instrument downtime.&nbsp;SmartStatus instrument tracking is an intelligent instrument health software that allows users to track key aspects of their GC-MS system. It is available as standard on the Thermo Scientific™ <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/483">TRACE™ 1600 GC series</a>, Thermo Scientific™ <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=3&amp;search=AI%2FAS+1610+liquid+autosampler">AI/AS 1610 liquid autosampler</a>, Thermo Scientific™ <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/484">ISQ™ 7610 GC-MS series</a>, and the Thermo Scientific™ <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/485">TSQ™ 9610 GC-MS/MS series</a>. In this technical note, the new SmartStatus instrument tracking capabilities are highlighted with examples of how it can enable analytical laboratories to keep instruments producing consistent results.<h4>SmartStatus software overview&nbsp;</h4>SmartStatus intelligent software, available within Thermo Scientific™ <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/products/76">Chromeleon™ Chromatography Data System (CDS)</a>, allows monitoring of the entire analytical system including Thermo Scientific™ autosamplers, GC, GC detectors (FID and TCD), and mass spectrometers (MS). Hundreds of key instrument parameters are monitored by SmartStatus software, which provides real-time data and insights informing the user to potential problems before they arise to ensure maximum instrument uptime. This allows users to make informed decisions on which parts of the analytical system require attention and when. By performing preventative maintenance using data-driven guidance, optimal instrument performance is sustained day in and day out. Figure 1 shows the SmartStatus software overview page for a TSQ 9610 triple quadrupole MS coupled to a TRACE 1610 GC and AI/AS 1610 liquid autosampler. This overview page allows a user to quickly determine if the system is ready to run or requires attention.&nbsp;For more information on instrument status, there is a detailed view for each part of the system. This next level view shows how many injections have been performed for the various GC consumables, the lifetime of the MS detector and filament, and when the last tune was performed. Figure 2 shows an example of the GC and MS parameters and how they are monitored. Each parameter is represented as a counter gauge. As the usage increases, the gauge changes color to quickly notify the user of any maintenance that is required or will be needed soon. This allows users to plan maintenance in advance to fit it around their schedule and workload. SmartStatus instrument tracking can be monitored directly in Chromeleon CDS, and consumables usage can also be monitored directly on the TRACE 1610 GC touch screen through the dedicated instrument health icon, as shown in Figure 3.<h4>Conclusion&nbsp;</h4>SmartStatus software is intelligent and data-driven, allowing users to make informed decisions on when to perform maintenance on their GC and GC-MS systems. Its features and advantages include:<ul><li>At-a-glance system ready status allowing the analyst to act only when needed, removing wastes&nbsp;</li><li>User customizability of monitored parameters, threshold, and time units, which gives users control to monitor the system in a way that fits their needs&nbsp;</li><li>Intelligent preventative maintenance alerts ensuring maintenance to be performed before issues arise, keeping the instrument up and running longer</li><li>Consumable tracking that enables sustainable operation and maximization of the use of each consumable&nbsp;</li><li>Smart Support for rapid remote diagnosis to ensure any instrument issues can be resolved without delay&nbsp;</li></ul>Utilizing SmartStatus software on the TRACE 1600 series GC, TSQ 9610 GC-MS/MS, and ISQ 7610 GC-MS gives the analyst data-driven insights to make informed decisions that allow laboratories to operate more sustainably by maintain productivity, maximizing consumable usage, and reducing laboratory costs.

News from LabRulezGCMS Library - Week 21, 2025

This study aims to develop an environmentally friendly analytical method for detecting organochlorine and organophosphorus pesticides in drinking water. It combines dispersive liquid-liquid microextraction (DLLME) using a natural deep eutectic solvent (NADES) with GC-MS/MS analysis. The NADES, composed of DL-menthol and decanoic acid, is safe, biodegradable, and cost-effective.Key experimental parameters were optimized using multivariate analysis to enhance extraction efficiency. The method demonstrated high sensitivity with LOQs as low as 0.2 ng/L and good recovery rates across various spiking levels in real water samples, proving its suitability for routine pesticide monitoring.<blockquote><h4>The original article</h4><h4><a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0039914024013468">Natural deep eutectic solvent-based dispersive liquid-liquid microextraction of pesticides in drinking waters combined with GC-MS/MS detection</a></h4>Аsya Hristozova, Lorena Vidal, Miguel Ángel Aguirre, Kiril Simitchiev, Antonio Canals &nbsp;Talanta, Volume 282, 2025, 126967<a target="_blank" rel="noopener noreferrer" href="https://doi.org/10.1016/j.talanta.2024.126967">https://doi.org/10.1016/j.talanta.2024.126967</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.Organochlorine pesticides (OCPs) are resistant to environmental degradation and accumulate in soils and sediments, exposing humans to pesticide effects through the food chains, drinking water, and breathing [<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0039914024013468#bib27">27</a>]. The Stockholm Convention (2001) classifies certain OCPs as persistent organic pollutants (POPs), prohibiting their production and use [<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0039914024013468#bib28">28</a>]. Organophosphorus pesticides (OPPs) are less harmful than OCPs but have decreased usage due to their persistence and neurotoxicity [<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0039914024013468#bib29">29</a>]. The negative effects of pesticides on human health can be prevented by monitoring of the food, water, and air. Hence the monitoring of low-level pesticide residues in bottled drinking water is a global concern [<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0039914024013468#bib30">[30]</a>, <a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0039914024013468#bib31">[31]</a>, <a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0039914024013468#bib32">[32]</a>]. However, the monitoring itself requires and generates a huge amount of hazardous organic wastes with obvious harmful effects on the environment and humans. So, efforts have been made to lower the limits of detection of the target analytes by employing environmentally benign sample preparation processes such as stir bar extraction [<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0039914024013468#bib33">33</a>] or dispersive liquid-liquid microextraction [<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0039914024013468#bib23">23</a>]. In this view the development of new green solvents which are aimed to reduce or fully eliminate the hazardous wastes can be regarded as very worthful.Therefore, the current research aims to develop a new and sensitive analytical method using a combination of dispersive liquid-liquid microextraction (DLLME) assisted by vortex and using an environmentally friendly extractant (i.e., NADES: DL-menthol and decanoic acid in molar ratio 2:1) for the preconcentration of organochlorine and organophosphorus pesticides followed by gas chromatography-tandem mass spectrometry (GC-MS/MS).<h4>2. Materials and methods</h4><h5>2.2. Instrumentation, apparatus and software</h5>Experiments were performed using a <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=2&amp;search=GC-MS%2FMS+TSQ+9000">GC-MS/MS TSQ 9000</a> (Thermo Fisher Scientific, USA) with electron ionisation (EI) at 70&nbsp;eV, equipped with a triple quadrupole mass filter and Programmable Temperature Vaporising (PTV) injector. The system was operated by Excalibur software 4.1. Extract with volume of 1&nbsp;μL was injected manually with a 10&nbsp;μL glass syringe. The study was conducted utilizing a PTV glass liner with Three Baffles, 1&nbsp;mm ID, 2.75&nbsp;mm OD, 120&nbsp;mm Length (Thermo Fisher Scientific, USA). The PTV injector was used in split mode (split ratio 50:1), starting with 65&nbsp;°C initial inlet temperature followed by gradient heating at 14.5&nbsp;°C sec−1 to 290&nbsp;°C. GC column TG-SQC 15&nbsp;m&nbsp;×&nbsp;0.25&nbsp;mm, 0.25&nbsp;μm film thickness (Thermo Fisher Scientific, USA) was used for chromatographic separation. The oven temperature program was as follows: 120&nbsp;°C – held for 1&nbsp;min; increased at the rate of 40&nbsp;°C min−1 to 155&nbsp;°C, rating 4&nbsp;°C min−1 to 187&nbsp;°C, rating 1&nbsp;°C min−1 to 194&nbsp;°C and rating 25&nbsp;°C min−1 to a final temperature of 290&nbsp;°C and held for 10&nbsp;min. The solvent delay time and total analysis time were 2.5&nbsp;min and 31&nbsp;min, respectively. Helium (purity 99.9999 %) at a flow rate of 1.2&nbsp;mL&nbsp;min−1 was used as a carrier gas. The transfer line and the ion source temperatures were set at 250&nbsp;°C and 230&nbsp;°C, respectively.A Vortex Lab Dancer (IKA®, Germany), a centrifuge KA-1000 (Jiangsu Zhengji Instruments Co., Ltd., China), FT-IR VERTEX 70 Spectrometer (Bruker, Germany) and a pH meter with a combined glass electrode SensoDirect pH 110 (Lovibond® Water Testing, Germany) were used in the study.The software Statistica® version 14.1 (TIBCO, Santa Clara, USA) was used in the optimisation procedure and graphical visualization of the results. AGREEprep software was applied for the evaluation of the greenness metric of the developed method.<h4>3. Results and discussion</h4><h5>3.1. Assessment of the matrix effects in GC-MS/MS</h5>To the best of our knowledge, the matrix effects provoked by NADES (MNT:DA) as a matrix medium analysed by GC-MS/MS have not been previously studied. The influence of MNT:DA on the instrumental sensitivity was evaluated by measurements of two sets of 3 standard solutions (with concentrations up to 2000&nbsp;μg&nbsp;L−1 in the final solution) prepared in acetonitrile as well as in NADES (matrix-matched medium). The slopes of the calibration curves were compared according to Equation <a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0039914024013468#fd1">(1)</a>. The standard deviations of the slopes were also assessed, and the propagated standard deviation of the corresponding slope ratios was further calculated.<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0039914024013468#tbl1">Table 1</a> shows the derived slope ratio values, as well as the combined uncertainty. The chromatogram of the target analytes is presented on <a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0039914024013468#fig2">Fig. 2</a>.<img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/Talanta_Volume_282_2025_126967_Fig_2_Reconstituted_ion_current_chromatogram_RTIC_of_each_target_analyte_c57d9f9bb4.jpg" alt="Talanta, Volume 282, 2025, 126967: Fig. 2. Reconstituted ion current chromatogram (RTIC) of each target analyte." srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_Talanta_Volume_282_2025_126967_Fig_2_Reconstituted_ion_current_chromatogram_RTIC_of_each_target_analyte_c57d9f9bb4.jpg 114w," sizes="100vw" width="1099" height="1500">The sensitivity for all target analytes increased in the tested medium of MNT:DA compared to acetonitrile. The enhancement was in the range of 27–74 % (<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0039914024013468#tbl1">Table 1</a>), indicating a favourable effect of the MNT:DA medium during the GC-MS/MS analysis. As a general trend, it can be seen that the longer the retention time of the target analyte, the higher sensitivity is achieved using NADES as a matrix solution. A possible explanation for this “matrix-induced response enchantment effect” could be a reduction of the thermal stress when the target analytes are passing through the GC liner [<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0039914024013468#bib35">35</a>,<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0039914024013468#bib36">36</a>]. Such favourable matrix impact was also seen when employing several types of liners for pesticide detection using a combination of cloud point extraction with Triton X-100 and GC-MS or GC-MS/MS [<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0039914024013468#bib37">37</a>].<h5>3.2. Optimisation of dispersive liquid-liquid microextraction</h5>Considering the simultaneous determination of 19 target analytes (organochlorine and organophosphorus pesticides) and the number of variables influencing the extraction step a multivariate study [<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0039914024013468#bib38">38</a>] was used for extraction variables optimisation. This optimisation approach follows the principles of Green Analytical Chemistry [<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0039914024013468#bib39">39</a>] to reduce significantly the number of experiments, consumption of samples, reagents, energy and time. An approach at two steps has been used for the multivariate optimisation of the experimental factors: a Plackett-Burman design, to identify between significant and non-significant factors as a screening method followed by a central composite design (CCD) to obtain the optimal values for the significant factors. Seven factors with potential effect on DLLME were evaluated by the Plackett-Burman design: (i) sample volume (6 and 10&nbsp;mL); (ii) NADES volume (50 and 100&nbsp;μL), (iii) sample pH (5 and 7); (iv) extraction time (1 and 3&nbsp;min); (v) centrifugation speed (900 and 1300×g); (vi) centrifugation time (5 and 10&nbsp;min); and (vii) ionic strength, NaCl concentration (0 and 3 %, w v−1). <a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0039914024013468#appsec1">Table S4</a> shows the constructed matrix of factors and their values used at each experimental run.The results derived from the Plackett-Burman design for all studied analytes are presented as registered responses (i.e., peak areas) in Table S5 and as Pareto charts of the standardised effects of the factors on Figure S1. The factors showing a significant effect on the registered peak areas of all the analytes were the NADES and the sample volumes. The other five factors have no influence on the DLLME of the studied pesticides. Taking into account the effects from the Pareto charts the following values were set for further experiments: addition of NaCl is not necessary (negative effect), centrifugation speed at 900×g (negative effect) and extraction time 3 min (positive effect). Due to practical reasons, the values of the non-significant factors centrifugation time and pH are set to 5 min (due to the temperature increase with prolonged centrifugation time) and 7 for model solutions or native pH of the analysed drinking water, respectively.Further optimisation of the NADES and sample volumes was performed by applying a central composite design (CCD). The factor values incorporated in the CCD were: (i) sample volume (5.2, 6.0, 8.0, 10.0, and 10.8&nbsp;mL), and (ii) NADES volume (40, 50, 75, 100, and 110&nbsp;μL). The constructed CCD matrix is given in <a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0039914024013468#appsec1">Table S6</a> and the responses (i.e., peak areas) are shown in <a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0039914024013468#appsec1">Table S7</a>. The response surface diagrams obtained from CCD for alpha-HCH, Hexachlorobenzene, Chlorpyrifos, Aldrin, Heptachlor and p,p-DDE are shown in <a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0039914024013468#appsec1">Fig. S2</a>. It was found that the modelled functions for all studied pesticides have similar shapes – the registered peak area increases when the NADES volume is reduced and/or the sample volume is enlarged.Aiming group extraction of the pesticides further a desirability function was calculated according to Equation <a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0039914024013468#fd2">(2)</a> and response surface optimisation was applied (<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0039914024013468#fig3">Fig. 3</a>).<img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/Talanta_Volume_282_2025_126967_Fig_3_Desirability_function_response_surface_diagrams_23ad6064be.jpg" alt="Talanta, Volume 282, 2025, 126967: Fig. 3. Desirability function response surface diagrams." srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_Talanta_Volume_282_2025_126967_Fig_3_Desirability_function_response_surface_diagrams_23ad6064be.jpg 104w," sizes="100vw" width="1003" height="1500"><h4>4. Conclusions</h4>The NADES-based-DLLME methodology was successfully combined with GC-MS/MS and was applied for the analysis of organochlorine and organophosphorus pesticides in bottled drinking water by direct liquid injections of the NADES extractant phase into the gas chromatographic system. The last does not deteriorate the instrumental measurements in SRM mode allowing selective determination of the target analytes. The proposed analytical method is fast and simple and meets several conceptual green principles such as the miniaturisation of sample preparation, the use of a natural solvent, and the simultaneous quantification of 19 analytes, among others. Besides, the optimisation of the method was carried out by multivariate analysis, minimizing the consumption of sample, reagents and time. The figures of merit of the developed method were evaluated. It is important to highlight that the obtained absolute recoveries for most of the studied pesticides are close to 100 %; the gain in the value of the registered signals for the target analytes in the NADES phase is larger than the volume ratio of the initial and final solution due to positive matrix effect of the DES on the GC-MS/MS system. Finally, the developed method has been successfully applied to analyse drinking water samples, showing just a partial recovery for one out of nineteen studied pesticides (i.e., p,p-DDT).

Natural deep eutectic solvent-based dispersive liquid-liquid microextraction of pesticides in drinking waters combined with GC-MS/MS detection

In the week from May 19, the following webinars await you in the field of gas / solid phase and especially Raman, FTIR, GC and GC/MS.<blockquote><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/webinars">👉 DETAILS AND REGISTRATION IN THE WEBINARS SECTION</a>👉 Search and filter in the largest global database with over 4 500 GC, LC, MS and spectroscopy webinars.</blockquote><h5>1. Thermo Fisher Scientific: Let’s Talk Chromeleon: Interactive Q&amp;A with Product Experts</h5><ul><li>Wednesday, May 21, 2025</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/webinar/5178">Registration</a></li></ul>Join us for an exclusive opportunity to connect directly with Thermo Scientific Chromeleon Chromatography Data System (CDS) product experts in this interactive webinar session.<h5>2. AZoM: Mechanical Recycling Meets Innovation: Real-Time Analysis in the Extrusion Process</h5><ul><li>Tuesday, May 20, 2025</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/webinar/5170">Registration</a></li></ul>Felix Mehrens and Niklas Rode present inline extrusion monitoring using Raman spectroscopy—a real-time method for continuous control and improved recyclate quality.<h5>3. Thermo Fisher Scientific: Analytical Possibilities Before, During and After the Recycling of Lithium Ion Batteries</h5><ul><li>Tuesday, May 20, 2025</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/webinar/4992">Registration</a></li></ul>In this webinar you will learn about lithium-ion battery recycling process and the role of analytical instrumentation in lithium-ion battery recycling.<h5>4. Shimadzu Corporation: Enhancing Food Testing: New And Improved Method For MOSH/MOAH Contamination</h5><ul><li>Tuesday, May 20, 2025</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/webinar/5104">Registration</a></li></ul>Join our Digital Classrooms session to explore improved MOSH/MOAH detection, compliance strategies, and practical solutions to reduce contamination risks.<h5>5. Agilent Technologies: Part 1: Characterizing catalysts using an UV-VIS/NIR system with the Praying Mantis diffuse reflectance accessory</h5><ul><li>Thursday, May 22, 2025</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/webinar/4925">Registration</a></li></ul>In Part 1 of this workshop, we discuss the capabilities of the Praying Mantis accessory from Specac/Harrick in combination with the Cary 5000 UV-VIS/NIR System.<h5>6. Altium International/Agilent Technologies: Microplastics Analysis Technologies from Agilent: Overview, comparison, and benefits from the different techniques IR &amp; GCMS/Pyr/TD/TED</h5><ul><li>Thursday, May 22, 2025</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/webinar/5165">Registration</a></li></ul>We invite you to a webinar about Agilent solutions for microplastics analysis: two complementary techniques will be approached—LDIR and GC-MS.<h5>7. The Analytical Scientist/LECO: Breaking Down Barriers with Non-Target Screening</h5><ul><li>Wednesday, May 21, 2025</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/webinar/5077">Registration</a></li></ul>This session will explore the latest advancements in NTS and its applications in environmental analysis – with a view to developing broadly applicable workflows.<h5>8. Thermo Fisher Scientific: Comprehensive characterization of electrolytes in lithium-ion batteries</h5><ul><li>Wednesday, May 21, 2025</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/webinar/4993">Registration</a></li></ul>This webinar focuses on the comprehensive characterization of major components and impurities in lithium-ion battery electrolytes using GC-MS, IC-MS, and ICP-MS.

Webinars LabRulezGCMS Week 21/2025

In the 2 weeks from May 26, the following webinars await you in the field of gas / solid phase and especially Raman, FTIR, GC and GC/MS.<blockquote><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/webinars">👉 DETAILS AND REGISTRATION IN THE WEBINARS SECTION</a>👉 Search and filter in the largest global database with over 4 500 GC, LC, MS and spectroscopy webinars.</blockquote><h5>1. Phenomenex: GC Troubleshooting Quick Guide: Quick Fixes for Common Problems</h5><ul><li>Wednesday, June 4, 2025, 10:00 CEST</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/webinar/5179">Registration</a></li></ul>Join expert Zachary Woodward for a hands-on guide to troubleshooting gas chromatography. Learn to spot symptoms, locate issues, and apply maintenance for fast, effective fixes.<h5>2. Separation Science/Markes International: Expanding the Sample Extraction Toolkit for Food Analysis by GC-MS</h5><ul><li>Wednesday, June 4, 2025, 11:00 CEST</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/webinar/5119">Registration</a></li></ul>Discover a versatile platform for overcoming challenges in food analysis beyond conventional limits.<h5>3. Agilent Technologies: Let's Talk About IR Microscopy</h5><ul><li>Thursday, June 5, 2025, 20:00 CEST</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/webinar/2272">Registration</a></li></ul>The basics of IR microscopy will be discussed with an emphasis on the newest technologies.

Webinars LabRulezGCMS Week 22-23/2025

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Natural deep eutectic solvent-based dispersive liquid-liquid microextraction of pesticides in drinking waters combined with GC-MS/MS detection

Webinars LabRulezGCMS Week 22-23/2025

News from LabRulezGCMS Library - Week 21, 2025

GC–MS/MS–based multiresidue pesticide analysis in mealworm (Tenebrio molitor) larvae: Optimization of standard QuEChERS-based method to minimize matrix effects

Webinars LabRulezGCMS Week 21/2025

News from LabRulezGCMS Library - Week 20, 2025

Webinars LabRulezGCMS Week 20/2025

Development of GC-ITQ-MS chromatographic system for the identification of hydroxy derivatives of polycyclic aromatic hydrocarbons in wastewater

News from LabRulezGCMS Library - Week 19, 2025

Webinars LabRulezGCMS Week 19/2025

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