摘要
本研究建立和优化了一种利用QuEChERS方法提取和净化豇豆中5种有机磷农药残留并使用气相色谱-三重四极杆质谱法进行定性定量检测的方法。取300 g以上豇豆样品进行匀浆,称取10 g制备后的样品于50 mL离心管中,加入20 mL乙腈、萃取盐包和一颗陶瓷均质子,萃取后取出8 mL萃取液,置于15 mL QuEChERS净化管进行净化,再精确取5 mL萃取液氮吹至近干后,加入内标环氧七氯,并用2 mL乙酸乙酯-丙酮(V∶V=1∶1)定容上机。结果表明,5种有机磷在0~1.00μg·mL^(-1)有良好线性,相关系数均大于0.99;定量限在0.002~0.010 mg·kg^(-1);在0.01 mg·kg^(-1)、0.03 mg·kg^(-1)、0.10 mg·kg^(-1)3个加标水平下,回收率在75.6%~102.3%,且重复性良好。
In this study,a method for the extraction and purification of five organophosphorus pesticide residues in cowpea by QuEChERS was established and optimized,and the qualitative and quantitative detection was carried out by gas chromatography triple quadrupole mass spectrometry.In this method,more than 300 grams of cowpea samples are taken for homogenization,10 grams of samples are weighed and put into a 50 mL centrifuge tube,20 mL of acetonitrile,extraction salt package and a ceramic homoproton are added,after extraction,8 mL of extraction solution is accurately taken out,placed in a 15 mL QuEChERS purification tube for purification,the purification solution is dried with nitrogen gas until nearly dry,then the internal standard epoxy heptachlor is added.After fixed volume with 2 mL ethyl acetate and acetone(V∶V=1∶1),the samples were detected by GC-MS-MS.The results showed that the five organophosphorus had good linearity in the range of 0~1.00μg·mL^(-1),and the correlation coefficients were all greater than 0.99.The limit of quantification was 0.002~0.010 mg·kg^(-1);The recoveries were 75.6%~102.3% at the three spiked levels of 0.01 mg·kg^(-1),0.03 mg·kg^(-1) and 0.10 mg·kg^(-1),and the repeatability was good.
作者
陈嘉仪
CHEN Jiayi(Guangzhou Huaxin Testing Technology Co.,Ltd.,Guangzhou 510663,China)
出处
《现代食品》
2022年第21期145-147,共3页
Modern Food
