加速溶剂萃取/固相萃取净化/气相色谱质谱联用法测定浙贝母中13种有机氯及拟除虫菊酯类农药多残留___

目的：建立加速溶剂萃取，固相萃取净化/气相色谱-质谱仪(SPE/GC-MS)联用技术测定浙贝母中13种有机氯及拟除虫菊酯类农药多残留的方法。方法：样品经加速溶剂萃取(ASE)，提取液过Florisil固相萃取柱净化，氮吹至干，残留物用正己烷溶解后经GC-MS测定，以选择离子监测方式监测目标化合物的特征离子。结果：用内标法定量，加标质量浓度为0.10mg.kg-1时，13种农药的平均回收率在78.9％~106.9％之间，方法的检出限(LOD)为0.0001~0.0020 mg.kg-1，相对标准偏差在5.0％~10.3％之间。结论：本法提取效率高，测定快速，定量准确可靠，可实现对浙贝母中13种有机氯及拟除虫菊酯类农药的检测。

Abstract: Based on accelerated solvent extraction(ASE) and coupled with solid phase extraction purification(SPE) and gas chromatography-mass spectrometry(GC-MS), An analytic method was developed for determination of 13 Organic chlorine and Pyrethroid pesticide multi-residues in Fritillaria thunbergiiMiq. Methods: The sample was extracted by accelerated solvent extraction(ASE) and purified by passing through Florisil solid-phase extraction(SPE)cartridges. The elution was evaporated by nitrogen and dissolved by n-hexane. The target analytes were determined by GC-MS. The characteristic ion of the target compounds were monitored with the mode of selcted ion. Results:The recoveries ranged from 78.9% to 106.9% with standard method .The limits of detection (LODs) were in the range of 0.0001~0.0020mg.kg-1and RSD (n=3) was between 5.0% and 10.3% for the spiked sample at level of 0.10mg.kg-1. Conclusions:The method is rapid , precise and highly efficient in extraction and could be used for determination of 13 Organic chlorine and Pyrethroid pesticide residues in Fritillaria thunbergiiMiq.

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