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食品研究与开发:2016,37(14):-
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GC-MS/MS法测定铁皮石斛中19种农药残留
(云南省产品质量监督检验研究院,云南昆明650223)
Determination of 19 Kinds of Pesticide Residues in Dendrobium officinale Prescription by Gas Chromatography-Triple Quadrupole Tandem Mass Spectrometry
(Yunnan Product Quality Supervision and Testing Academy,Kunming 650223,Yunnan,China)
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投稿时间:2015-08-03    
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铁皮石斛中19种农药残留的分析方法。石斛样品经乙腈提取,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。19种农药成分在10 μg/L~200 μg/L范围内有良好的线性关系,相关系数在0.993 1~0.999 8范围内;19种农药成分在3个添加水平下(10、100、200μg/L),加标回收率范围为 82.83%~109.29%,RSD%(n=5)为1.43%~5.74%;各农药成分的检出限均小于0.58μg/L。该方法可应用于石斛中多种农药残留的同时检测。
Abstract:To develop an analysis method based on gas chromatography-triple quadrupole tandem mass spectrometry(GC-MS/MS)for the determination of 19 kinds of pesticide residues in Dendrobium officinale prescription.Dendrobium officinale prescription samples were extracted with acetonitrile,and then purified through ENVI-Carb/Florisil solid phase extraction(SPE)cartridge.The prepared samples were then analyzed by GCMS/MS in MRM mode,and the external standard method was applied to quantify the pesticides.All the 19 pesticides showed good linearity in the range of 10 μg/L to 200 μg/L(r=0.993 1-0.999 8),the average recoveries of all the pesticides were in the range of 82.83%to 109.29%at three spiked levels of 10,100,200 μg/L,the RSD(n=5)were in the range of 1.43%to 5.74%;and the limits of detection(LOD)were all below 0.58 μg/L.The method is suitable for the multiresidues analysis of pesticides in Dendrobium officinale prescription.
文章编号:201614033     中图分类号:    文献标志码:
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