色谱

色谱 ›› 2015, Vol. 33 ›› Issue (8): 869-877.DOI: 10.3724/SP.J.1123.2015.04005

• 研究论文 • 上一篇    下一篇

气相色谱-三重四极杆串联质谱法测定白芍中99种农药残留

刘小勤1, 佟玲2, 孟文婷2, 孙国祥1   

  1. 1. 沈阳药科大学药学院, 辽宁 沈阳 110016;
    2. 天士力控股集团研究院药物分析所, 天津 300402
  • 收稿日期:2015-04-03 出版日期:2015-08-08 发布日期:2015-07-27
  • 通讯作者: 孙国祥
  • 基金资助:

    国家"重大新药创制"科技重大专项(2013ZX09402202).

Determination of 99 pesticide residues in Paeoniae Radix Alba by gas chromatography-triple quadrupole tandem mass spectrometry

LIU Xiaoqin1, TONG Ling2, MENG Wenting2, SUN Guoxiang1   

  1. 1. School of Pharmacy, Shenyang Pharmaceutical University, Shenyang 110016, China;
    2. Tasly R. &D. Institute, Tasly Holding Group, Tianjin 300402, China
  • Received:2015-04-03 Online:2015-08-08 Published:2015-07-27

PDF

154

被引次数

11

摘要：

采用固相萃取技术(SPE)结合气相色谱-三重四极杆质谱(GC-MS/MS)建立了白芍中99种农药同时检测的分析方法。试样用乙酸乙酯提取,采用氨基固相萃取柱净化后,在GC-MS/MS多反应监测(MRM)模式下进行检测,基质匹配标准曲线内标法定量。结果表明,99种农药在0.001~0.25 mg/L范围内线性关系良好,相关系数(r2)大于0.99,方法定量限为0.001~0.050 mg/kg。加标水平为0.05、0.10和0.20 mg/kg时,99种农药的平均回收率为66.7%~128.0%,相对标准偏差(RSD, n=6)小于18.3%。对市售的13批样品进行测定,其中4批样品中检出微量的毒死蜱和p,p'-滴滴伊。实验证明,建立的SPE净化和GC-QqQ-MS相结合的检测方法具有准确可靠、灵敏度高等优点,适用于白芍中多农药残留的同时筛查测定。

关键词: 白芍, 固相萃取, 农药残留, 气相色谱-三重四极杆质谱

Abstract:

A method was established for the simultaneous determination of 99 pesticide residues with combination of solid-phase extraction technique (SPE) and gas chromatography-triple quadrupole tandem mass spectrometry (GC-QqQ-MS). The sample was extracted with ethyl acetate, and cleaned-up by an amino SPE column. The extract was determined by GC-MS/MS in multi-reaction monitoring (MRM) mode, and matrix-matched internal standard method was applied to quantify the pesticides. The results of all the 99 pesticides showed good linearity in the range of 0.001-0.25 mg/L, with correlation coefficients (r2) > 0.99. The limits of quantification (LOQs) were between 0.001-0.050 mg/kg. The recoveries were between 66.7% and 128.0% with RSD values typically lower than 18.3% at three spiked levels of 0.05, 0.10 and 0.20 mg/kg. This method has been applied to determine thirteen batches of commercially available samples, chlorpyriphos-ethyl and p,p'-DDE were detected in four batches of Paeoniae Radix Alba. The method is highly accurate, reliable and sensitive for monitoring the 99 pesticide residues in Paeoniae Radix Alba.

Key words: Paeoniae Radix Alba, gas chromatography-triple quadrupole tandem mass spectrometry (GC-QqQ-MS), pesticide residues, solid-phase extraction (SPE)

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