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首页> 外文期刊>Forensic science international >Efficient derivatization of methylphosphonic and aminoethylsulfonic acids related to nerve agents simultaneously in soils using trimethyloxonium tetrafluoroborate for their enhanced, qualitative detection and identification by EI-GC-MS and GC-FPD
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Efficient derivatization of methylphosphonic and aminoethylsulfonic acids related to nerve agents simultaneously in soils using trimethyloxonium tetrafluoroborate for their enhanced, qualitative detection and identification by EI-GC-MS and GC-FPD

机译：使用三甲基四氟硼酸盐同时在土壤中同时衍生与神经剂相关的甲基膦酰基和氨基乙基磺酸，其增强，定性检测和EI-GC-MS和GC-FPD鉴定

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Trimethyloxonium tetrafluoroborate (TMO center dot BF4) has been used in the simultaneous derivatization of phosphonic and 2-aminoethylsulfonic acids related to nerve agents in different soils for their enhanced detection and identification by electron ionization gas chromatography-mass spectrometry (EI-GC-MS). The panel of acids consisted of five Schedule 2 phosphonic acids (methyl methylphosphonic acid, ethyl methylphosphonic acid, isopropyl methylphosphonic acid, pinacolyl methylphosphonic acid and cyclohexyl methylphosphonic acid) along with two sulfonic acids, N,N-diethyl-2-aminoethylsulfonic acid and N, N-diisopropyl-2-aminoethylsulfonic acid. The acids were converted to their corresponding methyl esters at ambient temperature when present at a 10 mu g g(-1) concentration in three separate soils: Virginia type A soil, Ottawa sand and Nebraska EPA soil. The concentration of the acids reflects values typically encountered during proficiency tests (PTs) administered annually by the Organisation for the Prohibition of Chemical Weapons (OPCW). Derivatization times to yield detectable signals for the methyl ester products for all the acids was found to vary among all three soil samples, however, it was found that generally the most optimal time across all the matrices involved was 3 h after the addition of TMO center dot BF4. Concomitantly, the analysis of the samples was complemented using GC coupled to flame photometric detection (GC-FPD). The inclusion of GC-FPD in the analysis yielded stronger signals for all seven methylated analytes making their detection after merely 3 h possible relative to the ones initially obtained with EI-GC-MS. Regarding the three soils employed in our study, a greater methylating efficiency was found in the Virginia type A soil and Ottawa sand yielding results that were significantly larger in magnitude to those found during the same time points for the Nebraska EPA soil sample. Prolonged reaction times (up to 72 h) were explored to find the time for the highest yield of methyl ester production were found instead to be deleterious to the process showcasing the importance of the fast yielding nature of the process specifically in situations where time-sensitive analysis is crucial (e.g. OPCW-PT). Published by Elsevier B.V.
机译：三氟硼酸盐（TMO中心点BF4）已被用于同时衍生的膦和2-氨基乙基磺酸与不同土壤中的神经剂相关的磷酸盐和2-氨基乙基磺酸，用于通过电子电离气相色谱 - 质谱（EI-GC-MS）的增强检测和鉴定。酸面板由五附表2膦酸（甲基甲基膦酸，乙基甲基膦酸，异丙基甲基膦酸，吡啶基甲基膦酸和环己基甲基膦酸）组成，以及两个磺酸，N，N-二乙基-2-氨基乙基磺酸和n ，N-二异丙基-2-氨基乙基磺酸。当在三个单独的土壤中以10μgg（-1）浓度存在时，在环境温度下将酸转化为它们的相应甲酯：弗吉尼亚型土壤，渥太华沙子和内布拉斯加州的欧洲央行土壤。酸的浓度反映了通常在每年禁止化学武器（OPCW）的熟练睾丸（PTS）期间遇到的值。衍生时间以产生用于所有酸的甲酯产物的可检测信号在所有三种土壤样品中都会变化，但发现，在加入TMO中心后，涉及的所有基质的最佳时间通常是3小时点BF4。同时，使用GC耦合到火焰光度检测（GC-FPD）来补充样品的分析。在分析中包含GC-FPD，对于所有七种甲基化分析物产生更强的信号，使其在仅3小时之后，相对于最初用EI-GC-MS获得的甲基化分析物。关于我们研究中使用的三种土壤，在弗吉尼亚型土壤中发现了更大的甲基化效率，其土壤和渥太华砂产生结果，其幅度明显大于内布拉斯加州EPA土壤样品的相同时间点。探讨了延长的反应时间（高达72小时），以发现发现甲酯产生的最高产量的时间，而是有害的，而是对该过程的重要性特别是在时间敏感的情况下具体的过程的重要性分析至关重要（例如OPCW-PT）。 elsevier b.v出版。

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