阴离子交换固相萃取-气相色谱/质谱法分析人血浆中6种神经性毒剂降解产物  

Determination of Six Degradation Products of Nerve Agents in Human Plasma Using Gas Chromatography/Mass Spectrometry with Strong Anion Exchange-Solid Phase Extraction

作　　者：王清清[1] 顾明松[1] 冯建林[1] 阮金秀[1] 

机构地区：[1]军事医学科学院毒物药物研究所,北京100850

出　　处：《分析化学》2006年第1期5-9,共5页Chinese Journal of Analytical Chemistry

摘　　要：采用醋酸汞去除蛋白，实现了阴离子交换固相萃取-气相色谱／质谱法同时测定人血浆中6种神经性毒剂降解产物的三甲基硅烷衍生物。考察了不同溶剂的去蛋白效率和不同固相萃取柱对毒剂降解产物的保留行为，优化了阴离子交换树脂的洗脱条件。采用选择离子监测方式，6种降解产物在0.05～5.0mg／L范围内呈良好的线性关系，最低检出限在22μg/L以内；RSD均小于9．7％。该方法检测灵敏度高，血浆样品干扰小，是一种理想的血浆中神经性毒剂降解产物的检测方法。For the unequivocal proof of the use of chemical warfare agents （ CWA）, a simple and accurate method was explored, which could simultaneously determine six degradation products of nerve agents in human plasma, using gas chromatography/mass spectrometry （GC/MS） after trimethylsilyl derivatization. GC/MS analysis was performed after solid-phase extraction with a strong anion-exchange cartridge from the plasma samples, which was previously deproteinized by mercuric acetate. The efficiency of various deproteinization reagents and the effect of different solid-phase extraction cartridges were investigated. The concentration of eluent was also optimized. Linear calibration curves were obtained for the five alkyl methylphosphonic acids and methyl phosponic acid over concentrations ranging from 50μg/L to 5 mg/L in selected ion monitoring mode, and the detection limits were within 22μg/L. The RSD were less than 9.7%. This method offers relatively high sensitivity and reliable reproducibility. Thus, it should become a powerful method for the rapid and sensitive detection of nerve agents in biological samples.

关 键 词：气相色谱/质谱 阴离子交换固相萃取 神经性毒剂降解产物 

分 类 号：O657.63[理学—分析化学]