摘要
建立了尿中除草剂莠去津（ATRZ）代谢物去乙基莠去津（DEA）、去异丙基莠去津（DIA）及去乙基去异丙基莠去津（DDA）的分析方法。尿样加入内标2-氨基-4-甲氧基石-甲基-1，3，5-三氮嗪（AMMT），碱化后用高极性GDXS01大孔树脂吸附、乙酸乙酯洗脱进行固相萃取，萃取物在乙腈溶剂中用N-甲基-N-特丁二甲硅烷基三氟乙酰胺（MTBSTFA）进行衍生化，衍生物进行选择离子监测气相色谱-质谱联用法分析。ATRZ不发生特丁二甲硅烷基（TBDMS）衍生化，则以非衍生化形式同时进行分析。尿中DEA、DIA、DDA、ATRZ的萃取率分别为80％、78％、71％和85％，检出限分别为0．2、0．2、0．1、1μg/L。尿样中ATRZ的3种代谢物质量浓度在0．5～100μg／L范围内，ATRZ在5～1000μg/L范围内线性关系良好。在1、50μg／L加标水平下3种代谢物的回收率分别为97％～103％和98％～101％，相对标准偏差分别为9．2％～11．7％和5．2％～8．9％；空白尿中添加10μg/L和500μg/L ATRZ的回收率分别为101％和99％，相对标准偏差分别为12．7％和6．7％。该方法灵敏度高，可以分析莠去津中毒者和职业接触莠去津者尿中的莠去津及其代谢物。
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-butyldimethyhrifluoroaeetamide （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 effieieneies 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 0. 2, 0.2, 0. 1, 1μg/L, respectively. The calibration curves were linear in the range of 0. 5 - 100 Ixg/L for 3 metabolites and 5 - 1 000μg/ 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 9.2% -11.7 % and 5.2% -8.9% , respectively. The recoveries of ATRZ at two concentration levels of 10 μg/L and 500 μg/L were 101% and 99% with RSDs of 12.7% and 6.7% , 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.
出处
《分析测试学报》
CAS
CSCD
北大核心
2011年第2期176-180,共5页
Journal of Instrumental Analysis
基金
公安部科技创新项目(20049323101)
关键词
除草剂
莠去津
尿
气相色谱质谱联用法
固相萃取法
硅烷基衍生化法
herbicide
atrazine
urine
gas chromatography - mass spectrometery
solid phase extraction
silyl derivatization
