尿中五氯酚的毛细管气相色谱测定方法研究

A Study on Determination of PCP in Urine by Capillary Gas Chromatography

本文报道了尿中五氯酚（ＰＣＰ）的毛细管气相色谱测定方法。尿样中的ＰＣＰ经醋酐衍生、正已烷同步萃取后，毛细管色谱柱分离，电子捕获检测器检测，２，４，６－三溴酚（ＴＢＰ）作内标，峰高比定量。尿样经不同处理，可分别测定尿中游离ＰＣＰ和总的ＰＣＰ。取尿样２ｍｌ，最低检出限为２．６μｇ／Ｌ，线性范围０～６０００μｇ／Ｌ，精密度（ＲＳＤ）为３．１％～９．４％，加标回收率为８６．３％～１０１．２％。方法简便、快速、灵敏、准确。

A method of determining pentachlorophenol(PCP)in urine by capillary gas chromatography was described in this paper.Acetylation and extraction or samples were performed simultaneously using the acetic anhydride as derivatization reagent,the hexane as extraction reagent.The derivatives of PCP were separated and measured on a capillary column with ECD.Quantitation of the PCP was based on the ratio of two peaks height of PCP and 2,4,6-tribromophenol(TBP)which was internal standard.The detection limit was 2.6μg/L when 2ml urine specimen was taken.The linear range of calibration curve was 0～6000μg/ml.The precision ranged from 3.1%～9.4% and the recoveries of spiked samples ranged from 86.3%～101.2%.The method was shown to be simple,fast,sensitive and accurate.