M. F. Vokuev, A. V. Braun, T. M. Baygildiev, I. V. Rybalchenko, I. A. Rodin
{"title":"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","authors":"M. F. Vokuev, A. V. Braun, T. M. Baygildiev, I. V. Rybalchenko, I. A. Rodin","doi":"10.1134/S0020168523140157","DOIUrl":null,"url":null,"abstract":"<p>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.</p>","PeriodicalId":585,"journal":{"name":"Inorganic Materials","volume":"59 14","pages":"1396 - 1405"},"PeriodicalIF":0.9000,"publicationDate":"2024-03-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"0","resultStr":"{\"title\":\"Determination of Methylphosphonic Acid and Alkyl Methylphosphonic Acid Esters in Soils by Liquid Chromatography–High-Resolution Mass Spectrometry\",\"authors\":\"M. F. Vokuev, A. V. Braun, T. M. Baygildiev, I. V. Rybalchenko, I. A. Rodin\",\"doi\":\"10.1134/S0020168523140157\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"<p>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.</p>\",\"PeriodicalId\":585,\"journal\":{\"name\":\"Inorganic Materials\",\"volume\":\"59 14\",\"pages\":\"1396 - 1405\"},\"PeriodicalIF\":0.9000,\"publicationDate\":\"2024-03-20\",\"publicationTypes\":\"Journal Article\",\"fieldsOfStudy\":null,\"isOpenAccess\":false,\"openAccessPdf\":\"\",\"citationCount\":\"0\",\"resultStr\":null,\"platform\":\"Semanticscholar\",\"paperid\":null,\"PeriodicalName\":\"Inorganic Materials\",\"FirstCategoryId\":\"88\",\"ListUrlMain\":\"https://link.springer.com/article/10.1134/S0020168523140157\",\"RegionNum\":4,\"RegionCategory\":\"材料科学\",\"ArticlePicture\":[],\"TitleCN\":null,\"AbstractTextCN\":null,\"PMCID\":null,\"EPubDate\":\"\",\"PubModel\":\"\",\"JCR\":\"Q4\",\"JCRName\":\"MATERIALS SCIENCE, MULTIDISCIPLINARY\",\"Score\":null,\"Total\":0}","platform":"Semanticscholar","paperid":null,"PeriodicalName":"Inorganic Materials","FirstCategoryId":"88","ListUrlMain":"https://link.springer.com/article/10.1134/S0020168523140157","RegionNum":4,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"Q4","JCRName":"MATERIALS SCIENCE, MULTIDISCIPLINARY","Score":null,"Total":0}
Determination of Methylphosphonic Acid and Alkyl Methylphosphonic Acid Esters in Soils by Liquid Chromatography–High-Resolution Mass Spectrometry
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.
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.