Hooijschuur E W, Kientz C E, Brinkman U A
Department of Analytical Chemistry and Applied Spectroscopy, Free University, Amsterdam, The Netherlands.
J Chromatogr A. 2001 Sep 14;928(2):187-99. doi: 10.1016/s0021-9673(01)01133-5.
Microcolumn liquid chromatography (microLC) and capillary electrophoresis (CE) coupled on-line with flame photometric detection (FPD) have been used for the screening of polar breakdown products of chemical warfare agents in water and soil samples, provided during Official Proficiency Tests organized by the Technical Secretariat of the Organization for the Prohibition of Chemical Weapons. CE-FPD is shown to be a powerful and rapid method for the determination of alkylphosphonic acids, which are the breakdown products of organophosphorus nerve agents. Gradient elution microLC-FPD is more sensitive and robust but less rapid in the determination of these compounds. In addition, microLC-FPD can be applied to screen for hydrolysis products of sulfur mustard and its analogues. Both methods can be applied without prior derivatization and are extremely selective. In order to unambiguously identify the relevant compounds, electrospray ionization (tandem) mass spectrometry, gas chromatography-mass spectrometry and nuclear magnetic resonance spectrometry were applied.
微柱液相色谱（microLC）和毛细管电泳（CE）与火焰光度检测（FPD）在线联用，已用于筛查在禁止化学武器组织技术秘书处组织的官方能力验证测试中提供的水和土壤样品中化学战剂的极性分解产物。结果表明，CE-FPD是测定烷基膦酸的一种强大而快速的方法，烷基膦酸是有机磷神经毒剂的分解产物。梯度洗脱微柱液相色谱-火焰光度检测法在测定这些化合物时更灵敏、更稳定，但速度较慢。此外，微柱液相色谱-火焰光度检测法可用于筛查芥子气及其类似物的水解产物。这两种方法无需预先衍生化即可应用，且具有极高的选择性。为了明确鉴定相关化合物，采用了电喷雾电离（串联）质谱、气相色谱-质谱和核磁共振光谱法。
