丙烯腈尿中代谢物—腈乙基巯基尿酸的测定

Determination of the metabolite of acrylonitrile, s cyanoethyl mercapturic acid by high performance liquid chromatography

建立了柱前荧光衍生—高效液相色谱法测定丙烯腈（ＡＣＮ）在人尿中的代谢物—Ｓ－２－腈乙基巯基尿酸［Ｎ－乙酰－Ｓ－２－腈乙基半胱氨酸（ＣＥＭＡ）］。尿中ＣＥＭＡ的酸性水解产物Ｓ－２－羧乙基半胱氨酸（ＣＥＣ）与邻苯二甲醛反应生成强荧光物质。该衍生物经Ｃ１８柱分离后，用荧光检测器检测。方法检测限为３μｍｏｌ／Ｌ，尿中ＣＥＭＡ浓度为５０、２００μｍｏｌ／Ｌ时批内平均相对标准偏差为２．９％，尿加标平均回收率为９４％。ＡＣＮ现场工人的尿样经高效液相色谱—质谱联机（ＨＰＬＣ—ＭＳ）分离鉴定，确证尿中巯基尿酸结构为ＣＥＭＡ。正常人尿中未检出该化合物。该方法应用于３４例ＡＣＮ现场工人尿中ＣＥＭＡ的测定。

A HPLC assay was developed to identify and measure the metabolite of acrylonitrile (ACN), s cya noethyl mercapturic acid (CEMA) in urine. O phthalaldehyde was utilized as a pre column derivatizing agent in the assay. This derivative was isolated with a good selectivity by HPLC employing reversed phase ODS columns. The quantitative analysis of mercapturic acid derivative was reproducible and the detectable limit of it was 3 μmol/L. The average relative standard deviation for the runs carried out on the same day was approximately 2.9% at the range of 50～200μmol/L of CEMA, and the mean analytical recovery from spiked urine samples was 94%. The structure of metabolites in the urine from workers exposed to acrylonitrile was identified as CEMA by high performance liquid chromatography mass (HPLC MS).