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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
【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。
【Abstract】 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 0.9,0.9,1.5 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 occupationaly exposed to atrazine.
【Key words】 Atrazine; herbicide; urine; solid phase extraction; trimethylsilyl derivatization; gas chromato-graphy-mass spectrometry;
- 【文献出处】 分析化学 ,Chinese Journal of Analytical Chemistry , 编辑部邮箱 ,2009年03期
- 【分类号】R446.1
- 【被引频次】11
- 【下载频次】330