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目的用GC-MS建立一种人体尿液中拟除虫菊酯类农药代谢物——顺式-3-(2,2-二氯乙烯基)-2,2-二甲基环丙烷-1-羧酸(cis-Cl2 CA)、反式-3-(2,2-二氯乙烯基)-2,2-二甲基环丙烷-1-羧酸(trans-Cl2 CA)和3-苯氧基苯甲酸(3-PBA)的生物监测方法。方法采用盐酸水解后用正己烷提取,硫酸-甲醇甲酯化后进行GC-MS分析。结果采用人工模拟尿样作为空白,配制基质匹配标准条件下,cis-Cl2CA、trans-Cl2CA和3-PBA检测限度(CCα)分别为:0.19、0.28和0.53μg/L,检测容量(CCβ)分别为:0.34、0.36和0.29μg/L;3个分析物日内和日间回收率范围均在在90%～110%之间,相对标准偏差(RSD)均小于5%;样品室温保存和冷冻保存时间分别至少为4天和30天;非暴露人群的监测值均小于1.5μg/L,而暴露人群普遍高于非暴露人群,有个别的cis-Cl2CA和3-PBA超过100μg/L,trans-Cl2CA超过10μg/L。结论通过方法验证确定该方法简单、便利,耐用性好,成本低,适合进行大规模常规人群的日常生物监测研究。
OBJECTIVE To establish a GC-MS method for the determination of pyrethroid pesticide metabolites in human urine, cis-3- (2,2-dichlorovinyl) -2,2-dimethylcyclopropane- (Cis-Cl2 CA), trans-3- (2,2-dichlorovinyl) -2,2-dimethylcyclopropane- 1 -carboxylic acid (trans-Cl2 CA) Biological monitoring of benzoic acid (3-PBA). The method was hydrolyzed with hydrochloric acid and extracted with n-hexane. After sulfuric acid-methanol methyl esterification, GC-MS analysis. Results The artificial urine samples were used as blank. The detection limits (CCα) of cis-Cl2CA, trans-Cl2CA and 3-PBA were 0.19,0.28 and 0.53μg / L, Were 0.34, 0.36 and 0.29 μg / L, respectively. The recoveries of the three analytes were between 90% and 110%, with relative standard deviations (RSDs) less than 5%. The samples were stored at room temperature and cryopreserved Time were at least 4 days and 30 days respectively; the monitoring value of non-exposed group was less than 1.5μg / L, while the exposed group was generally higher than that of non-exposed group, with individual cis-Cl2CA and 3-PBA more than 100μg / L, Cl2CA exceeds 10 μg / L. Conclusion The method is validated by the method to determine the method is simple, convenient, durable and low cost, suitable for routine biological monitoring of large-scale routine population.