有毒化学品分析中用作标准化合物的氘化甲基膦酸衍生物的合成

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引用次数: 0

摘要

采用气相色谱-质谱联用方法对环境和生物医学样品中有毒化学物质(TC)进行定量测定时,保证检测、鉴定和准确性的方法之一是使用内标物(is)作为被分析样品的添加剂,与目标TC相比,内标物含有稳定同位素,如D、13c、15n、18o。在这种情况下,优先考虑最容易获得的稳定氘化化合物。用稳定同位素标记的IS被广泛应用于许多研究中,以开发各种有毒化学物质,特别是烷基膦酸的分析方法。为了及时和高质量地完成分配给指定实验室的任务,似乎有必要拥有一个标记有稳定IS同位素的样品物理库,对应于那些在分析样品中最有可能出现的TC。首先是沙林、索曼、环沙林、VX、VR、CVX等稳定的分解产物,即甲基膦酸及其乙基、异丙基、丁基、异丁基、蒎醇酯和环己基酯,以及相应的对称二酯。根据本文的目的,我们合成了去甲基膦酸及其衍生物的IS组合物:去甲基膦酸的O-烷基酯的酸性氯化物、去甲基膦酸的O-烷基酯、去甲基膦酸的O-二烷基酯,以及酪氨酸和三肽tyr - thr - lyys与去甲基膦酸的O-异丙基和O-环己基酯的氯化物的加合物。研究了合成物质的NMR 2 Н、31 Р、GC-MS和HPLC-MS的光谱特征
本文章由计算机程序翻译,如有差异,请以英文原文为准。
Synthesis of Deuterated Methylphosphonic Acid Derivatives for Use as Standard Compounds in the Analysis of Toxic Chemicals
One of the ways to ensure high reliability of detection, identification and accuracy of quantitative determination of toxic chemicals (TC) in environmental and biomedical samples by gas and liquid chromatography-mass spectrometry methods is to use internal standards (IS) as additives to the analyzed sample, which, in contrast from target TC, contain stable isotopes such as D, 13 C, 15 N, 18 O. In this case, preference is given to the most accessible stable deuterated compounds. IS labeled with stable isotopes are widely used in numerous studies to develop methods for the analysis of various toxic chemicals, in particular, alkylphosphonic acids. For the prompt and high-quality performance of the tasks assigned to the assigned laboratory, it seems necessary to have a physical bank of samples labeled with stable IS isotopes, corresponding to those TC, the appearance of which in the analyzed samples is most likely. These include, first of all, stable decomposition products of such as sarin, soman, cyclosarin, VX, VR, CVX, namely, methylphosphonic acid, its ethyl, isopropyl, butyl, isobutyl, pinacolyl and cyclohexyl esters, as well as the corresponding symmetric diesters . In accordance with the objectives of the article, we have synthesized the IS composition of deuteromethylphosphonic acid and its derivatives: acid chlorides of O-alkyl esters of deuteromethylphosphonic acids, acid O-alkyl esters of deuteromethylphosphonic acids, O, O-dialkyl esters of deuteromethylphosphonic acids, and also adducts of tyrosine and tripeptide Tyr-Thr-Lys with chlorides of O-isopropyl and O-cyclohexyl esters of deuteromethylphosphonic acid. NMR 2 Н, 31 Р, GC-MS and HPLC-MS spectral characteristics of the synthesized substances were studied
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