p-Methoxyphenacyl Bromide as a Versatile Reagent for the Determination of Alkylphosphonic and Alkylmethylphosphonic Acids by High-Performance Liquid and Gas Chromatography with Mass Spectrometric Detection

被引：6

作者：

Baygildiev, T. M. ^{[1
]}

Vokuev, M. F. ^{[1
]}

Oreshkin, D. V. ^{[2
]}

Braun, A. V. ^{[2
]}

Godovikov, I. A. ^{[3
]}

Rybalchenko, I. V. ^{[2
]}

Rodin, I. A. ^{[1
]}

机构：

[1] Moscow MV Lomonosov State Univ, Dept Chem, Moscow 119991, Russia

[2] Minist Def Russian Federat, Sci Ctr 27, Moscow 105005, Russia

[3] Russian Acad Sci, Nesmeyanov Inst Organoelement Cpds, Moscow 119334, Russia

来源：

JOURNAL OF ANALYTICAL CHEMISTRY | 2020年 / 75卷 / 13期

基金：

俄罗斯科学基金会;

关键词：

markers of toxic substances; derivatization; high-performance liquid chromatography; gas chromatography; tandem mass spectrometry; high-resolution mass spectrometry; ALKYL METHYLPHOSPHONIC ACIDS; AGENT DEGRADATION-PRODUCTS; CHEMICAL WARFARE AGENTS; ENVIRONMENTAL-SAMPLES; HYDROLYSIS PRODUCTS; DERIVATIZATION;

D O I：

10.1134/S106193482013002X

中图分类号：

O65 [分析化学];

学科分类号：

070302 ; 081704 ;

摘要：

A multipurpose reagent, p-methoxyphenacyl bromide, is proposed for the derivatization of polar products of the degradation (markers) of nerve agents, which allows their determination by high-performance liquid chromatography with tandem mass spectrometric detection or by gas chromatography in combination with high-resolution mass spectrometry. The reaction conditions for the derivatization of alkylphosphonic and alkylmethylphosphonic acids with this reagent were optimized, the features and general patterns of the formation of MS1 and MS2 spectra of derivates were found, and the conditions for their chromatographic separation by two independent methods were selected. The limits of detection reached are in the range from 0.02 to 0.2 ng/mL for high-performance liquid chromatography with tandem mass spectrometric detection and from 10 to 50 ng/mL for gas chromatography with tandem mass spectrometric detection.

引用

页码：1708 / 1718

页数：11

共 17 条

[1]

[Anonymous], 2019, QDOCLABWIBIOPT04

[2] Hydrophilic interaction liquid chromatography-tandem mass spectrometry methylphosponic and alkyl methylphosphonic acids determination in environmental samples after pre-column derivatization with p-bromophenacyl bromide [J].

Baygildiev, T. M. ;

Rodin, I. A. ;

Stavrianidi, A. N. ;

Braun, A. V. ;

Lebedev, A. T. ;

Rybalchenko, I. V. ;

Shpigun, O. A. .

JOURNAL OF CHROMATOGRAPHY A, 2016, 1442 :19-25

[3] Rapid IC-MS/MS determination of methylphosphonic acid in urine of rats exposed to organophosphorus nerve agents [J].

Baygildiev, Timur ;

Zatirakha, Alexandra ;

Rodin, Igor ;

Braun, Arkady ;

Stavrianidi, Andrey ;

Koryagina, Nadezhda ;

Rybalchenko, Igor ;

Shpigun, Oleg .

JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES, 2017, 1058 :32-39

[4] Derivatisation reactions in the chromatographic analysis of chemical warfare agents and their degradation products [J].

Black, RM ;

Muir, B .

JOURNAL OF CHROMATOGRAPHY A, 2003, 1000 (1-2) :253-281

[5]

Carey R.J., 2007, Advanced Organic Chemistry Part A: Structure and Mechanisms

[6] Postcolumn derivatization liquid chromatography mass spectrometry for detection of chemical-weapons-related compounds [J].

Creasy, WR .

JOURNAL OF THE AMERICAN SOCIETY FOR MASS SPECTROMETRY, 1999, 10 (05) :440-447

[7]

Hayes T. L., 2004, J MED CHEM DEF, V2, P121

[8] LC-MS-based procedures for monitoring of toxic organophosphorus compounds and verification of pesticide and nerve agent poisoning [J].

John, Harald ;

Worek, Franz ;

Thiermann, Horst .

ANALYTICAL AND BIOANALYTICAL CHEMISTRY, 2008, 391 (01) :97-116

[9] On-line solid-phase extraction liquid chromatography-continuous flow frit fast atom bombardment mass spectrometric and tandem mass spectrometric determination of hydrolysis products of nerve agents alkyl methylphosphonic acids by p-bromophenacyl derivatization [J].

Katagi, M ;

Tatsuno, M ;

Nishikawa, M ;

Tsuchihashi, H .

JOURNAL OF CHROMATOGRAPHY A, 1999, 833 (02) :169-179

[10]

Lazio Z.R., 2004, DESIGN EXPT CHEM ENG, DOI [10.1002/3527604162, DOI 10.1002/3527604162]

← 1 2 →