Analysis of N Desalkalated Metabolites of Atrazine in Urine by Gas Chromatography-Mass Spectrometry with t Butyldimethylsilyl Derivatization[J]. 2011,30(2):176-180.
Analysis of N Desalkalated Metabolites of Atrazine in Urine by Gas Chromatography-Mass Spectrometry with t Butyldimethylsilyl Derivatization[J]. 2011,30(2):176-180.DOI:
An analytical method was developed for the dertermination of atrazine(ATRZ) metabolites,including deethylatrazine(DEA),deisopropylatrazine(DIA)and didealkylatrazine(DDA),in urine sample. The samples were added 2 amino 4 methoxyl 6 methyl s triazine(AMMT) as internal standard followed by alkalification,then extracted by solid phase extraction technique using high polar GDX501 porous resin as sorbent and ethyl acetate as elution solvent. The extracts were derivatized with N methy N t butyldimethyltrifluoroacetamide(MTBSTFA) in acetonitrile and analyzed by gas chromatography-mass spectrometry under the selected ion monitoring mode.Without being derivatized in this method condition,ATRZ can also be analyzed by original form. The extraction efficiencies of DEA,DIA,DDA and ATRZ in urine were 80%,78%,71% and 85%,respectively.The detection limits of DEA,DIA,DDA and ATRZ in urine were 02,02,01,1 μg/L,respectively. The calibration curves were linear in the range of 05-100 μg/L for 3 metabolites and 5-1 000 μg/L for ATRZ. The recoveries of 3 metabolites at two concentration levels of 1 μg/L and 50 μg/L were 97%-103% and 98%-101% with RSDs of 92%-117 %and 52%-89%,respectively. The recoveries of ATRZ at two concentration levels of 10 μg/L and 500 μg/L were 101% and 99%with RSDs of 127% and 67%,respectively. The method is sensitive,and could be applied in the analysis of ATRZ and its metabolites in urine samples of human poisoned by ATRZ or occupationaly exposed to ATRZ.