代谢
为了验证化学战剂(CWA)沙林、梭曼和VX的使用,我们探索了一种简单、快速且准确的方法,通过间接光度检测离子色谱(IPD-IC)同时确定它们在人类血清中的降解产物,包括异丙基甲基膦酸(IPMPA)、戊醇甲基膦酸(PMPA)、乙基甲基膦酸(EMPA)和甲基膦酸(MPA)。本方法使用阴离子交换柱进行IC分析,样品预处理采用Ag+型阳离子交换树脂柱。四种甲基膦酸可以得到很好的分离。提出的条件如下:洗脱液为0.5 mM邻苯二甲酸-0.1 mM三羟甲基氨基甲烷-5%乙腈;流速为1.0 ml/min;温度为50度;紫外检测器波长为266 nm。所有四种甲基膦酸在30分钟内洗脱,几乎没有受到血清中杂质的干扰。甲基膦酸、乙基甲基膦酸和异丙基甲基膦酸的线性校准曲线浓度范围为50 ng/ml至1 ug/ml,戊醇甲基膦酸的浓度范围为100 ng/ml至1 ug/ml。甲基膦酸的相对标准偏差在500 ng/ml时为3.8至6.9%,甲基膦酸、乙基甲基膦酸和异丙基甲基膦酸的检测限为40 ng/ml,戊醇甲基膦酸的检测限为80 ng/ml。该方法适用于人类血清样本的分析。
For the verification of the use of chemical warfare agents (CWA), sarin, soman and VX, a simple rapid and accurate method which allows us to simultaneously determine their degradation products, isopropyl methylphosphonic acid (IPMPA), pinacolyl methylphosphonic acid (PMPA), ethyl methylphosphonic acid (EMPA) and methylphosphonic acid (MPA), in human serum, was explored by indirect photometric detection ion chromatography (IPD-IC) which employs an anion-exchange column. IC analysis was performed after sample preparation with an Ag+-form cation-exchange resin cartridge, and the four methylphosphonic acids could be separated well. The proposed conditions are as follows: eluent, 0.5 mM phthalic acid-0.1 mM Tris (hydroxymethyl) aminomethane-5% acetonitrile; flow-rate, 1.0 ml/min; temperature, 50 degrees C; UV detector, 266 nm. All four methylphosphonic acids were eluted within 30 min with hardly any disturbance by impurities in the serum. Linear calibration curves were obtained for methylphosphonic acid, ethyl methylphosphonic acid and isopropyl methylphosphonic acid in the concentration range from 50 ng/ml to 1 ug/ml and for pinacolyl methylphosphonic acid from 100 ng/ml to 1 ug/ml. The relative standard deviation for the methylphosphonic acids ranged from 3.8 to 6.9% at 500 ng/ml and the detection limits were 40 ng/ml for methylphosphonic acid, ethyl methylphosphonic acid and isopropyl methylphosphonic acid and 80 ng/ml for pinacolyl methylphosphonic acid. The method would be suitable for analysis of human serum samples.
来源:Hazardous Substances Data Bank (HSDB)