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

被引:36
作者
Katagi, M [1 ]
Tatsuno, M [1 ]
Nishikawa, M [1 ]
Tsuchihashi, H [1 ]
机构
[1] Osaka Prefectural Police HQ, Forens Sci Lab, Chuo Ku, Osaka 5410053, Japan
关键词
mass spectrometry; derivatization; LC; chemical warfare agents; sarin; soman; VX; alkyl methylphosphonic acids;
D O I
10.1016/S0021-9673(98)01049-8
中图分类号
Q5 [生物化学];
学科分类号
071010 ; 081704 ;
摘要
For proof of the presence of chemical warfare agents sarin, soman and VX, a rapid, accurate and sensitive method which allows us to determine their hydrolysis products ethyl methylphosphonic acid, isopropyl methylphosphonic acid and pinacolyl methyl phosphonic acid was explored by using continuous flow frit fast atom bombardment (FAB) LC-MS and LC-MS-MS. After derivatization of analytes with p-bromophenacyl bromide, LC-MS-MS analyses for screening were performed by a flow injection method. The three alkyl methylphosphonic acids (AMPAs) were eluted within 5 min, and the detection limits for the three AMPAs ranged from 1 to 5 ng/ml. For confirmation of the screening results, LC-MS-MS analysis with chromatographic separation was conducted by using a narrow bore column. The three AMPAs were all eluted with excellent separation within 25 min, and the detection limits ranged from 1 to 20 ng/ml. Quantitative measurement was performed by LC-MS in selected ion monitoring (SIM) mode with chromatogaphic separation. Linear calibration curves were obtained for the three AMPAs and the detection limits ranged from 0.5 to 3 ng/ml. The relative standard deviation for peak area ranged from 3.4 to 6.0% at 50 ng/ml for the three AMPAs. (C) 1999 Elsevier Science B.V. All rights reserved.
引用
收藏
页码:169 / 179
页数:11
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