Determination of Methylphosphonic Acid and Alkyl Methylphosphonic Acid Esters in Soils by Liquid Chromatography–High-Resolution Mass Spectrometry

IF 0.9 4区材料科学 Q4 MATERIALS SCIENCE, MULTIDISCIPLINARY Inorganic Materials Pub Date : 2024-03-20 DOI:10.1134/s0020168523140157

M. F. Vokuev, A. V. Braun, T. M. Baygildiev, I. V. Rybalchenko, I. A. Rodin

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Abstract

A method has been optimized for simultaneous extraction of ethyl methylphosphonic acid ester (EMPA), isopropyl methylphosphonic acid ester (IPMPA), isobutyl methylphosphonic acid ester (IBMPA), pinacolyl methylphosphonic acid ester (PMPA), and methylphosphonic acid (MPA), which are highly polar products of nerve agent hydrolysis, from soil with their further determination by high-performance liquid chromatography–high-resolution tandem mass spectrometry (HPLC–HRMS/MS). The ions observed in the fragmentation mass spectra of deprotonated EMPA, IPMPA, IBMPA, PMPA, and MPA molecules and their deuterated analogs (d3-EMPA, d3-IPMPA, d3-IBMPA, d3-PMPA, and d3-MPA), as well as possible structural formulas of the fragment ions, are presented. Liquid extraction with deionized water followed by concentration by evaporation was used to prepare soil samples for analysis. The components were separated using reverse-phase chromatography. The time required for the sample preparation and analysis of the soil samples was no more than 1 h. The detection limits in soil were 0.05 ng/g for EMPA and IPMPA, 0.02 ng/g for IBMPA and PMPA, and 1 ng/g for MPA.

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利用液相色谱-高分辨质谱法测定土壤中的甲基膦酸和甲基膦酸烷基酯

摘要优化了一种同时萃取乙基甲基膦酸酯（EMPA）、异丙基甲基膦酸酯（IPMPA）、异丁基甲基膦酸酯（IBMPA）、频哪醇甲基膦酸酯（PMPA）和甲基膦酸（MPA）的方法、通过高效液相色谱-高分辨串联质谱法（HPLC-HRMS/MS）进一步测定土壤中神经毒剂水解的高极性产物--异丁基甲基膦酸酯（IMPA）、频哪醇甲基膦酸酯（PMPA）和甲基膦酸（MPA）。介绍了在去质子化的 EMPA、IPMPA、IBMPA、PMPA 和 MPA 分子及其氚代类似物（d3-EMPA、d3-IPMPA、d3-IBMPA、d3-PMPA 和 d3-MPA）的碎片质谱中观察到的离子，以及碎片离子的可能结构式。使用去离子水进行液体萃取，然后通过蒸发浓缩来制备用于分析的土壤样本。采用反相色谱法分离各成分。土壤样品的制备和分析时间不超过 1 小时。EMPA 和 IPMPA 的检测限为 0.05 纳克/克，IBMPA 和 PMPA 为 0.02 纳克/克，MPA 为 1 纳克/克。

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来源期刊

Inorganic Materials 工程技术-材料科学：综合

CiteScore

1.40

自引率

25.00%

发文量

审稿时长

3-6 weeks

期刊介绍： Inorganic Materials is a journal that publishes reviews and original articles devoted to chemistry, physics, and applications of various inorganic materials including high-purity substances and materials. The journal discusses phase equilibria, including P–T–X diagrams, and the fundamentals of inorganic materials science, which determines preparatory conditions for compounds of various compositions with specified deviations from stoichiometry. Inorganic Materials is a multidisciplinary journal covering all classes of inorganic materials. The journal welcomes manuscripts from all countries in the English or Russian language.