固相萃取-硅烷化-气质联用分析尿中莠去津及其去烃基代谢物  

Solid Phase Extraction-Silyl Derivation-Gas Chromatography-Mass Spectrometry for the Analysis of Atrazine and Its N-Desalkalated Metabolites in Urine

作　　者：王国强[1] 朱昱[1] 齐宝坤[1] 谭家镒[1] 

机构地区：[1]中国刑事警察学院法医系,沈阳110035

出　　处：《分析化学》2009年第3期441-444,共4页Chinese Journal of Analytical Chemistry

基　　金：公安部科技创新项目(No.20049323101)资助

摘　　要：建立了固相萃取-硅烷化-气质联用分析尿中除草剂莠去津(ATRZ)及其代谢物去异丙基莠去津(DIA)、去乙基莠去津(DEA)和去乙基去异丙基莠去津(DDA)的方法。尿样加入内标,碱化后用GDX501大孔树脂进行固相萃取,萃取物进行TMS衍生化,选择离子监测气质联用法分析。尿中ATRZ、DIA、DEA和DDA的提取率分别为85.3%、78.6%、80.2%和71.7%;检出限分别为0.9、0.9、1.5和1.2μg/L;在5～500μg/L浓度范围内工作曲线的线性关系良好。方法可用于莠去津中毒者和职业接触者尿样的分析。A solid phase extraction-trimethylsilyl （TMS） derivation-gas chromatography/mass spectrometric method to detect and quantitate atrazine and its metabolites [ deisopropylatrazine （DIA）, deethylatrazine （DEA） and didealkyl atrazine （DDA） ] in urine was developed. The urine samples were basified, and extracted by solid phase extraction technique using GDX501 porous resin . The resulting extracts were TMS derivatized, and then analysed by gas chromatography-mass spectrometry in the selected ion monitoring mode. The extraction recoveries of atrazine, DIA, DEA and DDA in urine were 85.3% , 78.6% , 80.2% and 71.7% , respectively. The limit of detection of atrazine, DIA, DEA and DDA in urine were 0. 9, 0. 9, l. 5 and 1.2 μg/L, respectively. The linearity relationship were good in the concentration range of 5 500 μg/L for all 4 analytes in urine. This analytical method can be applied to the analysis of specimens of humen poisoned with atrazine or oceupationaly exposed to atrazine.

关 键 词：除草剂 莠去津 尿 气质联用法 硅烷基衍生化 固相萃取法 

分 类 号：R446.1[医药卫生—诊断学]