HPLC-MS法同时测定北细辛药材中30种禁用农药残留  

Detection 30 kinds of Banned Pesticide Residues in Asarum heterotropoides by HPLC-MS

作　　者：杜连云 张慧娥 周蕖 张涛 黄鑫 刘芳鑫 李东飞 王恩鹏 陈长宝 DU Lianyun;ZHANG Huie;ZHOU Qu;ZHANG Tao;HUANG Xin;LIU Fangxin;LI Dongfei;WANG Enpeng;CHEN Changbao(Jilin Ginseng Academy,Changchun University of Chinese Medicine,Changchun 130117,China;Jilin Zixin Pharmaceutical Industrial Co.,Ltd.,Tonghua 135300,China;National Center for Quality Testing of Traditional Chinese Medicine(North),Changchun 130117,China)

机构地区：[1]长春中医药大学吉林省人参科学研究院,吉林长春130117 [2]吉林紫鑫药业股份有限公司,吉林通化135300 [3]国家中药质量检测(北方)中心,吉林长春130117

出　　处：《特产研究》2023年第6期132-138,共7页Special Wild Economic Animal and Plant Research

基　　金：国家重点研发计划项目(2019YFC1710704);吉林省科技发展计划项目(20200404042YY,20210401108YY);长春市科技局重点研发计划关键技术攻关专项项目(21ZGY10)。

摘　　要：建立北细辛药材中30种禁用农药残留的高效液相色谱质谱联用(High performance liquid chromatography-mass spectrometry,HPLC-MS)检测方法。采用直接提取固相萃取法对产自吉林省和辽宁省的33批次北细辛样品经净化处理后进液相色谱质谱测定,以外标法进行定量检测。结果显示,采用直接提取固相萃取的前处理方法简便,回收率高,30种禁用农药的线性关系良好,相关系数R^(2)>0.99,方法检出限为0.004~0.020 mg/kg,定量限为0.010~0.200 mg/kg。高、中、低3个水平的平均加标回收率为81.35%~104.35%,相对标准偏差为2.1%~7.6%。该方法具有操作简便、灵敏度高、准确可靠和重现性强等优点,适用于北细辛30种禁用农药残留量的同时测定。A high performance liquid chromatography-mass spectrometry(HPLC-MS)method was developed for the determination of 30 kinds of banned pesticide residues in Asarum heterotropoides.33 batches of A.heterotropoides samples from Jilin and Liaoning province were purified by direct extraction-solid phase extraction,and then determined by HPLC-MS.The results showed that the pretreatment method of direct extraction-solid phase extraction was simple with a high recovery rate.The linear relationships of 30 kinds of banned pesticides were good with correlation coefficient R^(2)>0.99.The limits of detection of the method were 0.004~0.020 mg/kg,and the limits of quantitative were 0.010~0.200 mg/kg.The average recoveries of the three additions spiked at high,medium and low levels were 81.35%~104.35%,and the relative standard deviations were 2.1%~7.6%.The method has the advantages of simple operation,high sensitivity,accurate and reliable and strong reproducibility,which is suitable for the simultaneous determination of 30 kinds of banned pesticide residues in A.heter-otropoides.

关 键 词：液相色谱质谱联用 禁用农药残留 北细辛 固相萃取 

分 类 号：R284.1[医药卫生—中药学]