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作 者:程妍 李莉 张佳莉 CHENG Yan;LI Li;ZHANG Jiali(Changzhou Institute for Food,Drug and Fiber Control,Changzhou 213000,China)
机构地区:[1]常州市食品药品纤维质量监督检验中心,常州213000
出 处:《药学与临床研究》2022年第5期409-414,446,共7页Pharmaceutical and Clinical Research
基 金:国家药品监督管理局2021年国家药品抽验计划(序号7)。
摘 要:目的:测定抗栓胶囊中33种禁用农药的残留量,并进行风险评估。方法:收集29批抗栓胶囊,以快速样品处理法(QuEChERS)制备样品后,采用GC-MS/MS和LC-MS/MS法,电喷雾/电子轰击离子源,正离子多反应监测模式,同时测定抗栓胶囊中33种禁用农药的残留量。结果:33种禁用农药在检测质量浓度范围内线性关系良好,相关系数r^(2)≥0.99,平均回收率为67.51%~103.12%,RSD为1.33%~14.05%(n=6)。29批样品中有部分批次检出农药残留,包括水胺硫磷、甲拌磷、氟虫腈、三氯杀螨醇。结论:该方法准确,重复性好,作为农药残留筛查方法为抗栓胶囊标准完善、质量监督提供参考。结果显示,抗栓胶囊中禁用农药残留量极低,无重大健康风险。Objective:To determine the residual amounts of 33 banned pesticides in Kangshuan capsules and to perform risk assessment.Methods:Twenty-nine batches of Kangshuan capsules were collected.Samples were prepared with QuEChERS,then the residual amounts of 33 banned pesticides in Kangshuan capsules were simultaneously determined with LC-MS/MS and GC-MS/MS.For MS detection,ion sources were from electrospray or electron bombardment,positive ion and MRM mode were adopted.Results:For the 33 banned pesticides,all had good linear relationships(r^(2)≥0.99),their recoveries ranged from 67.51%to 103.12%,with RSDs between 1.33%-14.05%(n=6).Some banned pesticides were detected from the twenty-nine batches of Kangshuan capsules,including isocarbophos,phorate,fipronil and dicofol.Conclusion:The method has good stability,high precision and promising repeatability,which provides a reference for standard perfection and quality supervision of Kangshuan capsules.The results showed that the residual amounts of 33 banned pesticides in Kangshuan capsules were extremely low,and there was no significant health risks.
关 键 词:抗栓胶囊 禁用农药残留 液相色谱-串联质谱法 气相色谱-串联质谱法 风险评估
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