摘要
建立了蔬菜中毒死蜱及其代谢物—3,5,6-三氯-2-羟基吡啶(3,5,6-trichloro-2-pyridinol,TCP)的气相色谱-质谱/质谱分析方法。蔬菜样品采用丙酮提取,浓缩后TCP用N-甲基-N-叔丁基二甲基硅基三氟乙酰胺(MTB-STFA)衍生,再经氟罗里硅土固相萃取柱净化。采用三重四极杆质谱电子轰击多反应监测(MRM)模式测定。采用内标法对毒死蜱定量,方法的检出限为1μg/kg,加标回收率为75.57%~106.41%,相对标准偏差(RSD)为8.33%~17.58%。采用外标法对TCP定量,方法的检出限为0.5μg/kg,加标回收率为69.11%~108.43%,RSD为5.20%~19.42%。在2~100μg/L范围内,两种被测物的线性关系良好(r>0.99)。该方法可用于蔬菜中毒死蜱及其代谢物的检测。
A method was developed for the determination of chlorpyrifos and its metabolite -- 3,5,6-trichloro-2-pyridinol （TCP） in vegetables using gas chromatography-tandem mass spectrometry （GC-MS/MS）. The sample was extracted with acetone. After the concentration, TCP was derivatized with N- （tert-butyldimethylsilyl） -N-methyltrifluoroacetamide （MTBSTFA）. The purification was performed using a florisil solid-phase extraction cartridge. The analyte was detected by triple quadrupole MS in multi-reaction monitoring mode. An internal standard method was used for the quantification of chlorpyrffos, the limit of quantification was 1μg/kg, and the recoveries were in the range of 75.57% - 106.41% with the relative standard deviations （RSDs） of 8.33% - 17.58%. An external standard method was used for the quantification of TCP, the limit of quantification was 0. 5 μg/kg, and the recoveries were in the range of 59. 11% - 108.43% with the RSDs of 5.20% - 19.42%. The good linear relationships were obtained in the range of 2 - 100 p^g/L for the both target analytes. The method can be applied for the determination of chlorpyrifos and its metabolite in vegetables.
出处
《色谱》
CAS
CSCD
北大核心
2009年第1期78-81,共4页
Chinese Journal of Chromatography
基金
科技部"十一五"科技支撑计划课题(No.2006BAK02A08)
中国检验检疫科学研究院基本科研业务费专项资金项目(No.2007JK006)
关键词
气相色谱-质谱/质谱法
毒死蜱
代谢物
蔬菜
gas chromatography-tandem mass spectrometry （GC-MS/MS）
chlorpyrifos
metabolite
vegetables
