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食品研究与开发:2017,38(13):173-178
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SPE-GC-MS/MS法测定茶叶中49种农药残留
王吉祥,牛之瑞,冯雷,白祥,杜四淮,谭建林, 张晓红
(云南省产品质量监督检验研究院,云南 昆明 650223)
Determination of 49 Kinds of Pesticide Residues in Tea by SPE and Gas Chromatography-Tandem Mass Spectrometry
WANG Ji-xiang, NIU Zhi-rui, FENG Lei, BAI Xiang, DU Si-huai, TAN Jian-lin, ZHANG Xiao-hong
(Yunnan Product Quality Supervision and Testing Academy,Kunming 650223, Yunnan, China)
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投稿时间:2016-10-09    
中文摘要: 建立固相萃取-气相色谱-三重四极杆串联质谱法测定茶叶中 49 种农药残留的分析方法。 样品经乙腈均质 提取,经 ENVI-Carb+Florisil 固相萃取小柱进行净化后,采用气相色谱-三重四极杆串联质谱法在多反应监测(MRM) 模式下测定, 外标法定量。49 种农药成分在 10 μg/ L~100 μg/ L 范围内有良好的线性关系, 相关系数在 0.995 2~0.999 9 范围内;49 种农药成分在 3 个添加水平下(10、50、100 μg/L), 加标回收率范围为 71.43 %~115.21 % ,RSD(n=6)为 1.13 %~11.05 %;各农药成分的检出限均小于 1.06 μg/kg。该方法样品处理简单快速,灵敏度和选择性高,适用于日常 检测工作。
Abstract:To develop an analysis method based on solid -phase extraction and gas chromatography -triple quadrupole tandem mass spectrometry(SPE-GC-MS/MS) or the determination of 49 kinds of pesticide residues in Tea. Samples were extracted with acetonitrile, and then purified through ENVI-Carb+Florisil solid phase ex- traction(SPE)cartridge, the prepared samples were then analyzed by GC-MS/MS in MRM mode,and the exter- nal standard method was applied to quantify the pesticides. All the 49 pesticides showed good linearity in the range of 10 μg/ L to 100 μg/ L (R2 = 0.995 2-0.999 9),the average recoveries of all the pesticides were in the range of 71.43 % to 115.21 % at three spiked levels of 10,50,100 μg/ L,the RSD (n=6) were in the range of 1.13 % to11.05 %; and the limits of detection (LOD) were all below 1.06 μg/kg. The method is suitable for the multiresidues analysis of pesticides in Tea.
文章编号:201713037     中图分类号:    文献标志码:A
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