论文部分内容阅读
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79.9%～105.7%之间,方法的检出限(LOD)为0.0001～0.0020mg·kg-1,相对标准偏差在4.9%～10.5%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。
Objective: To establish a method for determination of 13 residues of organochlorine and pyrethroid pesticides in Fritillaria cirrhosae by Accelerated Solvent Extraction / Solid Phase Extraction / Gas Chromatography - Mass Spectrometry (SPE / GC-MS). Methods: The sample was subjected to accelerated solvent extraction (ASE). The extract was purified by Florisil solid phase extraction (SPE), dried over nitrogen and dissolved in hexane. The residue was characterized by GC-MS and monitored by selective ion monitoring . Results: The average recoveries of 13 pesticides ranged from 79.9% to 105.7% with the mass concentration of 0.10 mg · kg-1 and the limit of detection (LOD) was 0.0001 ~ 0.0020 mg Kg-1, the relative standard deviation of 4.9% to 10.5%. Conclusion: The method has high extraction efficiency, rapid determination, accurate and reliable quantitative determination of 13 organochlorine and pyrethroid pesticides in Fritillaria cirrhosa.