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GC-MS/MS法测定铁皮石斛中19种农药残留

     

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10μg/L~200μg/L范围内有良好的线性关系,相关系数在0.9931~0.9998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。%To develop an analysis method based on gas chromatography-triple quadrupole tandem mass spec-trometry (GC-MS/MS) for the determination of 19 kinds of pesticide residues in Dendrobium officinale pre-scription. 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 GC-MS/MS in MRM mode,and the external standard method was applied to quantify the pesticides. All the 19 pesti-cides showed good linearity in the range of 10μg/L to 200μg/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 10,100,200μg/L,the RSD (n=5) were in the range of 1.43%to 5.74%;and the limits of detection (LOD) were all below 0.58μg/L. The method is suitable for the multiresidues analysis of pesticides in Dendrobium officinale prescription.

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