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特丁二甲硅烷基衍生化气相色谱-质谱法检测尿中4种苯氧羧酸类除草剂
引用本文:刘娟,朱昱,齐宝坤,谭家镒. 特丁二甲硅烷基衍生化气相色谱-质谱法检测尿中4种苯氧羧酸类除草剂[J]. 分析科学学报, 2010, 26(1). DOI: 10.3969/j.issn.1006-6144.2010.01.011
作者姓名:刘娟  朱昱  齐宝坤  谭家镒
作者单位:广州市公安局,广东广州,510030;中国刑警学院法医系,辽宁沈阳,110035
基金项目:公安部科技创新项目(No.20049323101)
摘    要:建立了尿中2,4-滴(2,4-D)、2,4-滴丙酸(2,4-DP)2、甲4氯(MCPA)和2甲4氯丙酸(MCPP)4种苯氧羧酸类除草剂的气相色谱-质谱(GC-MS)分析方法。尿样加氯化钠饱和,酸化后用乙醚萃取,萃取物进行特丁二甲硅烷基(TBDMS)衍生化后分析。尿中4种除草剂的浓度在3~3 000 ng/mL范围内工作曲线的线性关系良好,检出限在1 ng/mL以下,3、100和1 000 ng/mL水平加标回收率在97.0%~102.2%之间,精密度在6.2%~14.2%之间。该法灵敏,可用于中毒者和职业接触者尿中苯氧羧酸类除草剂的分析。

关 键 词:尿  苯氧羧酸类除草剂  硅烷基衍生化  气相色谱-质谱法

Determination of Four Phenoxy Acid Herbicides in Urine by Gas Chromatography-Mas Spectrometry
LIU Juan,ZHU Yu,QI Bao-kun,TAN Jia-yi. Determination of Four Phenoxy Acid Herbicides in Urine by Gas Chromatography-Mas Spectrometry[J]. Journal of Analytical Science, 2010, 26(1). DOI: 10.3969/j.issn.1006-6144.2010.01.011
Authors:LIU Juan  ZHU Yu  QI Bao-kun  TAN Jia-yi
Affiliation:1.Public Security Bureau of Guangzhou City;Guangzhou 510030;2.Forensic Medicine Department of China Criminal Police College;Shenyang 110035
Abstract:A method for determination of four phenoxy acid hebicides(2,4-D,2,4-DP,MCPA and MCPP) in urine by TBDMS derivatization and GC/MS determination was developed.The urine samples were saturated with sodium chloride,and extracted with diethyl ether.The extracts were derivatized with MTBSTFA in ethyl acetate and analysed by GC/MS.The detection limits of the four herbicides in urine were below 1 ng/mL.The linear relationships were good for 4 herbicides in the concentration range of 3~3 000 ng/mL.The recoveries wer...
Keywords:Urine  Phenoxy acid herbicides  Silyl derivatization  Gas chromatography-mass spectrometry  
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