通过式固相萃取结合气相色谱•串联质谱法测定陈皮中农药残留  

Determination of Pesticide Residues in Citri Reticulatae Pericarpium by SPE-GC-MS/MS

作　　者：熊颖[1] 李纯[1] 任晋 顾利红[1] 栗建明[1] 侯惠婵[1] Xiong Ying;Li Chun;Ren Jin;Gu Lihong;Li Jianming;Hou Huichan

机构地区：[1]广州市药品检验所国家药品监督管理局中成药质量评价重点实验室,广州510160

出　　处：《中国药师》2022年第3期537-543,共7页China Pharmacist

基　　金：国家药品医疗器械审评审批制度改革子课题(中药)项目(编号:ZG2016-2-10),国家药典委员会课题(编号:2020Z05)。

摘　　要：目的:建立陈皮中63种农药(含禁用27种)残留的气相色谱质谱联用检测方法。方法:采用乙腈为提取溶剂,经通过式固相萃取小柱Oasis;PRiME HLB净化,气相色谱-三重四极杆串联质谱法检测,电子轰击电离源(EI),多反应监测(MRM)。结果:63种农药线性关系良好,相关系数均大于0.99,平均回收率在53.4%~125.8%(92%农药回收率在65%~120%),RSD在1.9%~13.4%;精密度RSD在0.5%~6.2%,方法检出限在0.001~0.034 mg·kg;。32批陈皮中有24批检出部分农药。结论:本方法能快速有效地检测陈皮63种农药残留,可用于陈皮农药监测,也为中药材的农残检测提供借鉴与参考。Objective: To establish a GC-MS/MS method for the determination of 63 kinds of(including 27 kinds of forbidden) pesticide residues in Citri Reticulatae Pericarpium.Methods: The samples were extracted by acetonitrile and purified by passing mode solid phase extraction(SPE) with Oasis;PRiME HLB cartridge, and the quantitative analysis was carried out by GC-MS/MS in multiple-reaction monitoring(MRM) mode and electron impact(EI)source.Results: The calibration curves of 63 pesticide residues showed good linearity with correlation coefficients above 0.99. The average recoveries of all target pesticides were within the range of 53.4%-125.8% with the RSDs of 1.9%-13.4%, and the recoveries of 92% pesticides ranged from 65% to 120% with the RSDs of precision experiment was within the range of 0.5%-6.2%. The method detection limit(MDL) was within the range of 0.001-0.034 mg·kg;. Some pesticides were detected in 24 of 32 batches in Citri Reticulatae Pericarpium.Conclusion: The method is fast, accurate and highly sensitive for the screening and confirmation of 63 pesticide residues in Citri Reticulatae Pericarpium, which provides basis for the pesticide residues control for other Chinese herbal medicine.

关 键 词：固相萃取 气相色谱-三重四极杆串联质谱 陈皮 农药残留 

分 类 号：R927.1[医药卫生—药学]