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人参中农药多残留的超高效液相色谱-串联质谱分析方法研究
引用本文:陈丽娜,宋凤瑞,郑重,邢俊鹏,刘志强,刘淑莹. 人参中农药多残留的超高效液相色谱-串联质谱分析方法研究[J]. 化学学报, 2012, 70(7): 843-851. DOI: 10.6023/A1110262
作者姓名:陈丽娜  宋凤瑞  郑重  邢俊鹏  刘志强  刘淑莹
作者单位:a 中国科学院长春应用化学研究所 长春质谱中心 长春 130022;b 中国科学院研究生院 北京 100049
基金项目:“十一五”国家科技支撑计划,国家科技部创新方法工作专项
摘    要:以传统中药人参为研究对象, 建立一种同时检测人参中46 种农药多残留的基质固相分散-超高效液相色谱-串联质谱(MSPD-UPLC-MS/MS)方法. 前处理方法分别采用N-丙基乙二胺(PSA)和乙腈作为MSPD的分散剂和洗脱剂, 检测方法采用正负离子同时扫描, 利用超高效液相色谱-串联质谱在分时段多反应监测模式下进行定量和定性分析. 大部分农药在5~500 μg/kg 范围内线性关系良好, 在低(10 μg/kg)、中(50 μg/kg)、高(100 μg/kg)三个浓度水平上的添加回收率平均值在70%~110%之间, 相对标准偏差(RSD)小于15% (n=3), 定量限小于0.01 mg/kg, 能够满足农药多残留分析要求. 该方法通用性强、选择性好、灵敏度高、简单廉价.

关 键 词:基质固相分散法  超高效液相色谱-串联质谱  人参  多农药残留  

Studies on the Determination Method of Pesticide Multi-residues in Ginseng by Ultra Performance Liquid Chromatography Tandem Mass Spectrometry
Chen Lina,Song Fengrui,Zheng Zhonga,Xing Junpeng,Liu Zhiqiang,Liu Shuying. Studies on the Determination Method of Pesticide Multi-residues in Ginseng by Ultra Performance Liquid Chromatography Tandem Mass Spectrometry[J]. Acta Chimica Sinica, 2012, 70(7): 843-851. DOI: 10.6023/A1110262
Authors:Chen Lina  Song Fengrui  Zheng Zhonga  Xing Junpeng  Liu Zhiqiang  Liu Shuying
Affiliation:a Changchun Institute of Applied Chemistry Chinese Academy of Sciences, Changchun Centre of Mass Spectrometry, Changchun 130022;b Graduate School of Chinese Academy of Sciences, Beijing 100049
Abstract:Taking the traditional herbal,ginseng,as the object in the paper,a comprehensive analytical method based on matrix solid-phase dispersion-ultra performance liquid chromatography tandem mass spec-trometry(MSPD-UPLC-MS/MS) has been developed for the simultaneous determination of 46 pesticide residues in Ginseng.The sample was prepared by MSPD.Primary secondary amine(PSA) was used as dis-persant,and acetonitrile was used as eluant.Both positive and negative ionization modes were used in the detection.Qualitative and quantitative analysis was carried out by UPLC-MS/MS under multiple reaction monitoring mode(MRM).The linear range of this method was 5~500.0 μg/kg.The limits of quantification(LOQ) for the 46 pesticides were less than 0.01 mg/kg.The mean recoveries at the three spiked levels of 10~100 μg/kg were 70%~110%,with relative standard deviations(RSD) better than 15%(n=3).The method is robust,selective,sensitive,rapid and cheap.
Keywords:matrix solid-phase dispersion  ultra performance liquid chromatography tandem mass spec-trometry  ginseng  multi-residue pesticides
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