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作 者:熊颖[1] 李纯[1] 任晋 朱小媚 钟碧华 顾利红[1] XIONG Ying;LI Chun;REN Jin;ZHU Xiaomei;ZHONG Bihua;GU Lihong(Guangzhou Institute for Drug Control,Guangzhou 510160 Guangdong,China;Guangzhou University of Chinese Medicine,Guangzhou 510006 Guangdong,China)
机构地区:[1]广州市药品检验所,广东广州510160 [2]广州中医药大学,广东广州510006
出 处:《中药新药与临床药理》2020年第5期590-595,共6页Traditional Chinese Drug Research and Clinical Pharmacology
基 金:国家药品医疗器械审评审批制度改革子课题(中药)(ZG2016-2-10)。
摘 要:目的建立陈皮31种禁用农药残留的QuEChERS(Quick,Easy,Cheap,Effective,Rugged and Safe)-GC-MS/MS测定方法。方法采用乙腈为溶剂,匀浆提取,经固相分散萃取管(QuEChERs净化管)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)。结果陈皮31种禁用农药残留线性关系良好,相关系数均大于0.9959,平均回收率为67.3%~127.1%,RSD为1.0%~6.3%;精密度RSD为0.6%~5.8%,方法检出限为0.002~0.010 mg·kg^-1。结论所建立的方法能快速有效地检测陈皮31种禁用农药残留量,可用于陈皮禁用农药监测。Objective To establish a GC-MS/MS method for the determination of 31 forbidden pesticide residues in Citri reticulatae pericarpium. Methods Samples were extracted with acetonitrile by high speed homogenizer and purified with QuEChERs,quantitative analysis was carried out by GC-MS/MS using multiple-reaction monitoring(MRM) mode and electron impact(EI) ion source. Results The calibration curves of 31 forbidden pesticide residues showed good linearities with correlation coefficients above 0.99. The average recoveries for all target compounds were in the range of 67.3%-127.1%, with relative standard deviations of 0.6%-5.8%. The relative standard deviations of precision experiments were in the range of 0.6%-5.8%. Method detection limits(MDL) were in the range of 0.002-0.01 mg·kg^-1. Conclusion The method is fast,accurate and highly sensitive for the screening and confirmation of 31 forbidden pesticide residues in Citri reticulatae pericarpium.
关 键 词:陈皮 禁用农药残留 气相色谱-串联质谱法
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