化学学报 ›› 2012, Vol. 70 ›› Issue (07): 843-851 .DOI: 10.6023/A1110262 上一篇    下一篇

研究论文

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

陈丽娜a,b, 宋凤瑞a, 郑重a, 邢俊鹏a, 刘志强a, 刘淑莹a   

  1. 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
  • 收稿日期:2011-10-26 修回日期:2011-11-30 出版日期:2012-04-14 发布日期:2012-01-05
  • 通讯作者: 刘志强 E-mail:liuzq@ciac.jl.cn
  • 基金资助:

    “十一五”国家科技支撑计划(No. 2009ZX09308-006)和国家科技部创新方法工作专项(No. 2010IM030400)资助项目.

Studies on the Determination Method of Pesticide Multi-residues in Ginseng by Ultra Performance Liquid Chromatography Tandem Mass Spectrometry

Chen Linaa,b, Song Fengruia, Zheng Zhongaa, Xing Junpenga, Liu Zhiqianga, Liu Shuyinga   

  1. 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
  • Received:2011-10-26 Revised:2011-11-30 Online:2012-04-14 Published:2012-01-05
  • Supported by:

    Project supported by the National Key Technology R&D Program in the 11th Five year Plan of China (No. 2009ZX09308-006) and Innovation Method Fund of China (No. 2010IM030400).

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

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 spectrometry (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 dispersant, 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.

Key words: matrix solid-phase dispersion, ultra performance liquid chromatography tandem mass spectrometry, ginseng, multi-residue pesticides