尿中苯基脲类除草剂代谢物气相色谱分析

目的建立尿中苯基脲类除草剂代谢物的气相色谱分析方法。方法在检材中加入环己烷、固体氯化钠等试剂，分取有机相，在60℃水浴中加入衍生化试剂反应0．5h，冷却后洗去衍生化试剂，分取有机相进样进行气相色谱分析。结果尿中苯基脲类代谢物4一氯苯胺和3，4-二氯苯胺的检出限在5ng／mL以下，回收率良好，相对标准偏差均低于5％。在0．1μg～5μg／mL间线性关系良好。结论该法高效、灵敏、简便，适合对尿等生物检材中脲类除草剂的代谢物的定性和定量测定。

Determination of Phenylurea herbicide's metabolite in Urine by Gas Chromatography with Electron Capture Detector

A method for determination of 4-chloroaniline, 3,4-dichloroaniline, major metabolites of monolinuron and linu- ron in urine by Gas Chromatography and Electron Capture detector combined with dihloracetyl and 1-chlor-2-fluoroacetyl derivat- ization was developed. The samples was extracted by cyclohexane at pH 10. 8 from urine and derived with derivative reagent at 60℃ in a water bath for 0. 5 h. The detection limit of 4-chloroamine and 3,4-dichloroamine in urine was below 5ng/mL. The re- coveries of 4-chloroamine and 3,4-diehloroamine in urine were between 101.2%- 103. 1 %. The relative standard deviation was less than 5% and the linear relationship was quite good between 0.1μg~5μg/mL. The results showed that the method is efficient, sensitive for qualitative and quantitative determination of 4-chloroaniline and 3,4-dichloroaniline in urine or other biological samples.