Coumarin-Based Photolabile Solid Support Facilitates Nonchromatographic Purification of RNA Oligonucleotides

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

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

Our Library never stops expanding. What are the most recent contributions to LabRulezGCMS Library in the week of 24th August 2026? Check out new documents from the field of the gas phase, especially GC and GC/MS techniques!<blockquote>👉 <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library">SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT GCMS AND RELATED TECHNIQUES</a></blockquote><blockquote>👉 Need info about different analytical techniques? Peek into <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library">LabRulezLCMS</a> or <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library">LabRulezICPMS</a> libraries.</blockquote>This week we bring you application notes by Shimadzu, Thermo Fisher Scientific and Waters Corporation and poster by MDCW / GC Image!<h3>1. MDCW / GC Image: Alignment and Filtering Tools for Enhanced Differencing of Two-Dimensional Chromatograms</h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://labrulez.com/pdf/P_21_Wu_3838638ea4.pdf">Full PDF for download</a></li></ul><section><div><div><div><div><div><div><h5>Challenges&nbsp;</h5>Chromatogram-like visual differencing is intuitive, yet simple pixel-to-pixel subtraction often produces noisy artifacts, fails to correct retention-time shifts, and can obscure low-intensity but meaningful differences.&nbsp;Previously, we developed comparative visualization methods [1] based on classic image-comparison techniques, including:&nbsp;<ul><li>Alignment with specialized color maps to visually highlight discrepancies between chromatograms&nbsp;</li><li>Interactive matching across two chromatograms [2], enabling both qualitative and quantitative side-by-side assessment at the individual-peak level&nbsp;</li></ul>We extend this work by presenting a more robust chromatogram differencing visualization method designed to overcome these limitations<h4>Example 1: Alignment for Data Fusion (FID vs MS)&nbsp;</h4><ul><li>Data Set: GCxGC data of a diesel fuel sample&nbsp;</li><li>Instruments: <a target="_blank" rel="noopener noreferrer" href="https://labrulez.com/en-us/gcms/library?mainauthorItems=10&amp;search=7890A">Agilent 7890A GC</a>/InfoMass L10 thermal modulator/Hexin TOFMS<ul><li>Detectors: FID (350 C, 200 Hz), MS (45-450 m/z, 50 Hz)&nbsp;</li><li>Modulation: 6 seconds with programmable cold jet gas flow (15L/min to 6 L/min)</li></ul></li></ul><h4>Example 2: Differencing (GC×GC-MS)&nbsp;</h4><ul><li>Data Set: GCxGC-TOFMS data set of different dark chocolates [3].</li><li>Instruments: <a target="_blank" rel="noopener noreferrer" href="https://labrulez.com/en-us/gcms/library?mainauthorItems=23&amp;search=AccuTof">JEOL AccuTof GC mass spectrometer</a> with an <a target="_blank" rel="noopener noreferrer" href="https://labrulez.com/en-us/gcms/library?mainauthorItems=10&amp;search=7890">Agilent 7890 GC</a></li></ul><h4>Example 3: Differencing with BPC (LC×LC-MS)&nbsp;</h4><ul><li>Data Set: LCxLC-MS data of different types of beer [4].&nbsp;</li><li>Instruments: <a target="_blank" rel="noopener noreferrer" href="https://labrulez.com/en-us/lcms/library?mainauthorItems=10&amp;search=1290+infinity+2D-LC">Agilent 1290 Infinity 2D-LC</a> solution coupled with an <a target="_blank" rel="noopener noreferrer" href="https://labrulez.com/en-us/lcms/library?mainauthorItems=10&amp;search=6530">Agilent 6530 Accurate-Mass Q-TOF LC/MS system</a></li></ul><h3>2. Shimadzu: Comprehensive and High-Sensitivity Analysis of Food Aroma by Simultaneous Scan/MRM Measurement Using Triple Quadrupole GC-MS/MS</h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://labrulez.com/pdf/an_01_01269_en_657ee319e0.pdf">Full PDF for download</a></li></ul><h4>User benefits</h4><ul><li>Simultaneous scan/MRM measurement enables comprehensive search by scan measurement and high-sensitivity analysis of trace aroma compounds by MRM in a single measurement.&nbsp;</li><li>With LabSolutions Insight Explore GCMS, deconvolution analysis of scan data and target analysis of MRM data are possible in a single software program.&nbsp;</li><li>The Multi-Mode Injection Unit (MMI), which allows rapid heating, supports aroma analysis in the thermal desorption (TD) mode</li></ul>The “aroma” of food products and beverages is a key factor that largely determines product quality and consumer preferences, and thus is an extremely important element in product development and quality control. Since the gas chromatograph mass spectrometer (GC-MS) provides excellent performance in qualitative analysis of volatile compounds, it is used to measure various aroma components that make up an odor. However, due to the diversity of aroma compounds and their wide concentration range, which extends from the ppm to the ppt order, an analytical method that allows efficient measurement of these substances is demanded.&nbsp;Non-targeted analysis by scan measurement is an effective tool for comprehensive profiling, but in many cases, it is difficult to identify the trace components that make a significant contribution to aroma due to the limits of instrument sensitivity and matrix interference. On the other hand, although widetarget analysis by the MRM (Multiple Reaction Monitoring) mode using GC-MS/MS offers high sensitivity and selectivity for several hundred target components, MRM lacks a search capability for unknown components.Therefore, this Application News article reports a technique that satisfies both comprehensive non-targeted search and highsensitivity detection of trace components in a single analysis by combining the <a target="_blank" rel="noopener noreferrer" href="https://labrulez.com/en-us/gcms/library?mainauthorItems=1&amp;search=8040+RX">GCMS-TQ 8040 RX</a>, which supports simultaneous data acquisition in simultaneous multi-component analysis measurements by scan measurement and the MRM mode, and the Smart Aroma Database for use in aroma analysis. In addition, in this experiment, the thermal desorption (TD) mode of the Multi-Mode Injection Unit (MMI) was adopted for sample introduction. This enablesintroduction of componentstapped on the adsorbent without using a dedicated TD device, thereby achieving a simplified system configuration.<h4>Conclusion&nbsp;</h4>This Application News article showed that it is possible to achieve both a comprehensive non-targeted analysis of food aroma and a high-sensitivity wide-target analysis of trace components in a single analysis, without carrying out complicated operations, by simultaneous scan/MRM measurement combining the GCMSTQ8040 RX and the Smart Aroma Database. This article also demonstrated that use of the Multi-Mode Injection Unit (MMI) enables measurements in the thermal desorption (TD) mode without using dedicated TD instrumentation, and also allows a flexible response in case of budgetary or installation space limitations. A comprehensive aroma evaluation based on this approach will facilitate the discovery of important aroma components that were easily overlooked in the past, and is expected to make important contributions to product development and quality control in the food and beverage industries.<h3>3. Thermo Fisher Scientific: Implementing EPA OTM-50 for PFAS destruction monitoring by TD-GC-MS/MS</h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://labrulez.com/pdf/an_004773_gc_td_gc_ms_epa_otm_50_pfas_an04773_na_en_99fd5fc528.pdf">Full PDF for download</a></li></ul>Per- and polyfluoroalkyl substances are used across a broad range of industrial and consumer applications. As PFAS-containing materials are treated or destroyed, incomplete decomposition can generate volatile fluorinated compounds, including short-chain and ultra-volatile species. These volatile compounds are important because they may provide evidence of incomplete mineralization once emitted from stationary sources.EPA OTM-50 was developed to provide a consistent approach for collecting and quantitatively analyzing target VFCs from emissions originating from known industrial products with incomplete thermal destruction. The EPA method uses passivated stainlesssteel canisters followed by GC-MS analysis and is applicable to gas samples collected from industrial source ducts, vents, stacks, and related emission points.&nbsp;The method is performance-based, allowing laboratories flexibility in GC column selection, GC conditions, and MS conditions, provided that GC-MS remains the basis for separation and quantitation and the required performance criteria are met. This flexibility is important because OTM-50 analytes span a challenging volatility range and may occur in complex matrices containing CO2 , water vapor, acid gases, and other volatile organic compounds.&nbsp;Gas chromatography-based approaches are well suited to volatile and neutral fluorinated compounds. Thermal desorption enables preconcentration of trace-level analytes from air samples, improving sensitivity and enabling detection at relevant levels for environmental studies.&nbsp;This application note describes implementation of EPA OTM-50 using cryogen-free thermal desorption coupled to triple quadrupole GC-MS/MS. The workflow addresses key analytical challenges: trapping ultra-volatile compounds such as CF4 , managing high levels of CO2 and humidity, achieving sub-ppbv sensitivity, and maintaining repeatable quantitative performance in support of PFAS destruction monitoring.<h4>Experimental&nbsp;</h4><h5>Instrument configuration&nbsp;</h5>The analytical system consisted of a <a target="_blank" rel="noopener noreferrer" href="https://labrulez.com/en-us/gcms/library?mainauthorItems=6&amp;search=UNITY-Kori-CIA">Markes UNITY</a>-Kori-CIA Advantage HL-xr thermal desorption system coupled to a <a target="_blank" rel="noopener noreferrer" href="https://labrulez.com/en-us/all/products/485">TSQ 9610 Triple Quadrupole GC-MS/MS</a> equipped with a <a target="_blank" rel="noopener noreferrer" href="https://labrulez.com/en-us/gcms/library?mainauthorItems=3&amp;search=nevervent">Thermo Scientific™ NeverVent™ AEI Ion Source</a> (Figure 1). The Markes thermal desorber configuration included cryogen-free focusing, controlled canister introduction, and water and CO2 management strategies.<h4>Conclusions&nbsp;</h4>This work demonstrates implementation of EPA OTM-50 using thermal desorption coupled to triple quadrupole GC-MS/MS for the analysis of volatile fluorinated compounds in air, with solutions helping to solve key analytical challenges for this type of analysis.&nbsp;<ul><li>Alignment with EPA OTM-50 scope: supports canisterbased analysis of VFCs emitted from stationary sources, including compounds associated with incomplete PFAS destruction.&nbsp;</li><li>Cryogen-free preconcentration: enables practical trapping and transfer of volatile analytes without reliance on liquid cryogens, reducing operational complexity.&nbsp;</li><li>Improved selectivity through MS/MS: SRM acquisition on the TSQ 9610 Triple Quadrupole GC-MS/MS improves confidence in target identification and quantitation in complex emission matrices.&nbsp;</li><li>Dual-method strategy for broad volatility coverage: separate sample volumes for CF4 and the remaining VFCs enable analysis across the challenging OTM-50 volatility range.&nbsp;</li><li>CO2 and humidity management: controlled dilution, selective trap purging, and Kori-xr water management address two of the most significant matrix challenges in stationary source emissions.&nbsp;</li><li>Robust quantitative performance: calibration across 0.1–100 ppbv (0.125–50 ppbv for CF4 ) showed R2 ≥ 0.998 for reported compounds or &lt; 20% RSD for Average Response Factor, with pptv MDLs and repeatability generally consistent with OTM-50 precision expectations.&nbsp;</li><li>Industrial relevance: the workflow supports chemical manufacturing, PFAS treatment, and waste management facilities seeking defensible data to evaluate destruction efficiency and identify products of incomplete destruction.&nbsp;</li></ul>Overall, the combination of Markes thermal desorption technology with the Thermo Scientific TSQ 9610 Triple Quadrupole GC-MS/MS provides a practical, selective, and robust analytical approach for laboratories implementing EPA OTM-50 for volatile PFAS and VFC monitoring in air.<h3>4. Waters Corporation: Analysis of Polybrominated Diphenyl Ether Flame Retardants in Environmental Matrices Using Atmospheric Pressure Chemical Ionization GC-MS/MS</h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://labrulez.com/pdf/720009524_en_58a948f96a.pdf">Full PDF for download</a></li></ul><h4>Benefits&nbsp;</h4><ul><li>The performance of atmospheric pressure gas chromatography (APGC ™) on Xevo™ TQ Absolute Mass Spectrometer for the analysis of PBDEs is equal-to or better-than traditional analysis using electron impact magnetic sector making it well suited for use in the most challenging regulatory and standard methods.</li><li>The ability of APGC to tolerate high carrier gas flow helps improve method performance for the most challenging members of this class inlcuding BDE 209 which reduces the need for maintenance and reanalysis of samples.</li><li>Operator training is reduced to weeks from months through conversion of the method from a magnetic sector to tandem quadrupole mass spectrometer.</li><li>Use of a single, inexpensive, readily available gas for chromatographic separation, ionization and MS/MS fragmentation provides a simpler, more sustainable system.</li></ul>With the 2001 signing of the Stockholm Convention, the stage was set for global harmonization of efforts to monitor for POPs in the environment.1 By 2004, when countries began implementing the convention, measures aimed at reducing or eliminating intentional and unintentional release of POPs into the environment were supported by annexes that defined the different chemical classes of highest interest which included PBDEs. To date, 185 states plus the European Union have joined in this effort which includes requirements for monitoring for POPs in multiple environmental matrices. Because the implications of unintentional or intentional noncompliance may be subject to enforcement action, high confidence data is needed to support surveillance and reporting efforts. Furthermore, high sensitivity analysis is required due to the possibility of steadily increasing trace levels of PBDEs across years of time through transport in the environment that tends to increase concentrations of persistent organic pollutants such as these in cooler Arctic regions of the globe through the grasshopper effect.2 These requirements initially led to the development of gas chromatography electron ionization high resolution magnetic sector based analytical methods. The performance of EI GC-HRMS in the hands of a well-trained operator and a lab with rigorous quality control procedures has proven to provide the sensitivity and specificity required of the forensic data used in legal actions, for compliance reporting and for providing the greatest protection to populations and the environment.&nbsp;However, GC-HRMS has several limitations, including extensive education and training requirements, slow acquisition speeds, and significant laboratory space demands. In contrast, more modern techniques such as tandem quadrupole (TQ) mass spectrometry (MS/MS) offer broad improvements in these areas. Additionally, limitations imposed by EI such as frequent source maintenance and shortcomings caused by carrier gases other than helium hamper this time-honored technique. The more recent combination of APCI with TQ has demonstrated promise in overcoming these limitations while providing data of equivalent confidence to EI GCHRMS.&nbsp;After having been deployed in many labs, GC-APCI has continued to contribute to the study of PBDEs in multiple matrices and applications. An evaluation of the first generation of GC-APCI MS/MS, analyzing PBDEs in marine and food samples, reported higher response for higher brominated (Br8-10) congeners than GC-EI-HRMS.3 Later work reported GC-APCI MS/MS LODs comparable or better than EI MS/MS for plasma extracts.4 Recent work reported on the use of GC-APCI HRMS (QTof) as part of the continuation of a 20 year study analyzing aquatic organisms to evaluate environmental PBDE trends.5 In this work, 24 PBDEs plus hexabromobiphenyl were analyzed on a XevoTM TQ Absolute Tandem Quadrupole Mass Spectrometer using the APGC ionization source.<h4>Experimental</h4><ul><li>GC system: <a target="_blank" rel="noopener noreferrer" href="https://labrulez.com/en-us/gcms/library?mainauthorItems=10&amp;search=8890">8890 (Agilent Technologies, Inc.)&nbsp;</a></li><li>Column: Rtx®-1614, 15 m x 0.25 mm ID x 0.10 µm film (Restek Corporation)</li><li>MS system: <a target="_blank" rel="noopener noreferrer" href="https://labrulez.com/en-us/all/products/554">Xevo TQ Absolute Mass Spectrometer</a></li><li>Software: <a target="_blank" rel="noopener noreferrer" href="https://labrulez.com/en-us/all/products/1544">waters_connect™</a> for Quantitation Software</li></ul><h4>Conclusions&nbsp;</h4>An all-nitrogen configuration for APGC on Xevo TQ Absolute Mass Spectrometer was successfully applied to the analysis of PBDEs in environmental matrices by adapting a reference method previously used on magnetic sector EI GC-HRMS. All performance criteria were equal-to or better-than those typically achieved by magnetic sector which demonstrates feasibility of GC-APCI MS/MS as an alternative for the most challenging regulatory and standard analytical methods. Furthermore, the change from a vacuum source to the atmospheric ionization source makes the use of high nitrogen carrier gas flow practical which has advantages for operating cost versus helium while achieving similar chromatographic separation and sensitivity. The move to tandem quadrupole mass spectrometry from high resolution mass spectrometry updates the method for improved performance measures such as higher acquisition speeds and high specificity MS/MS while also requiring reduced training time and expertise as compared with magnetic sectors.</div></div></div></div></div></div></section>

News from LabRulezGCMS Library - Week 35, 2026

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LabRulez

2026 AOAC INTERNATIONAL Annual Meeting & Exposition

Bruker at the 7th European Symposium on Single Cell Proteomics

Shimadzu at 2026 AOAC Annual Meeting & Exposition

ICP-MS for Hybrid Photoelectrode Characterization

Modern Methods for Faster Microbial Analysis

Addressing LC Method Optimization - Scaling For Efficiency, Throughput And Reproducibility