摘要
建立了气相色谱-串联质谱定量检测花茶、绿茶、红茶和黑茶4类茶叶中氟氯氰菊酯、氯氰菊酯和氰戊菊酯3种拟除虫菊酯农药残留量的方法。样品采用乙腈进行提取,优化洗脱液配比,选择Carb/NH2和SLH双柱串联净化富集。采用外标法定量,30 min内完成农药残留检测。3种拟除虫菊酯的检出限分别为0.4、1.0和0.3μg/kg,在0.05~2.00 mg/kg内线性关系良好,相关系数均大于0.999。在0.10、0.50和2.00 mg/L 3个添加水平下,空白加标样品的回收率为80.6%~116.3%。茶叶实际样品检测结果的日内相对标准偏差(RSD)为1.3%~12.6%,日间RSD为2.7%~12.1%。该法操作简单,重现性好,适用于茶叶中拟除虫菊酯类农药残留的检测。
A rapid determination method of three pyrethroid pesticides (cyfluthrin, cypermethrin and fenvalerate) in tea was developed by series two. solid phase extraction. column cleanup and external standard method coupled with gas chromatography. tandem mass spec. trometry (GC-MS/MS) in 30 min. The pesticide residues in tea were extracted with acetonitrile, and cleaned up by Carb/NH2 and SLH solid. phase extraction columns. After filtration, the target compounds were analyzed by GC-MS and quantified by the external standard method. Under the optimized conditions, good linear ranges of 0.05-2.00 mg/kg were obtained. The limits of detection varied from 0.3 to 1.0 mu g/kg. The linear correlation coefficients were greater than 0.999. At three spiked levels (0.10, 0.50 and 2.00 mg/L), the average recoveries were determined between 80.6% and 116.3% in the four matrices. The inter. day relative standard deviations were between 1.3% - 12.6%, and the intra. day relative standard deviations were between 2.7% and 12.1%. This method is simple, fast, and has a good reproducibility, which can meet the requirements of the rapid detection of pyrethroid pesticides in tea.
出处
《色谱》
CAS
CSCD
北大核心
2017年第8期860-866,共7页
Chinese Journal of Chromatography
基金
国家自然科学基金(21375083)
山西省高等学校大学生创新创业训练项目(2015348)
山西大同大学博士科研启动项目(2008K3)
2016年度山西省留学人员科技活动择优资助项目(No.14)~~
关键词
气相色谱-串联质谱
拟除虫菊酯农药
茶叶
gas chromatography-tandem mass spectrometry (GC-MS/MS)
pyrethroid pesticides
tea
