色谱

色谱 ›› 2013, Vol. 31 ›› Issue (3): 191-199.DOI: 10.3724/SP.J.1123.2012.12019

• 研究论文 • 上一篇    下一篇

超高效液相色谱-串联质谱法测定中药材中三唑类杀菌剂及三嗪类除草剂的残留量

王菲, 李彤, 马辰*   

  1. 中国医学科学院&北京协和医学院药物研究所分析室, 北京 100050
  • 收稿日期:2012-12-10 修回日期:2013-01-11 出版日期:2013-03-28 发布日期:2013-03-22
  • 通讯作者:
  • 基金资助:

    科技部创新工作专项基金项目(2011 IM 030200).

Determination of triazole fungicide and triazine herbicide residues in Chinese herbs by ultra-performance liquid chromatography-tandem mass spectrometry

WANG Fei, LI Tong, MA Chen*   

  1. Department of Analysis, Institute of Materia Medica, Chinese Academy of Medical Sciences, Beijing 100050, China
  • Received:2012-12-10 Revised:2013-01-11 Online:2013-03-28 Published:2013-03-22

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769

被引次数

61

摘要： 建立了超高效液相色谱-串联质谱(UPLC-MS/MS)同时测定甘草、西洋参、三七、人参、丹参5种中药材中10种三唑类杀菌剂、18种三嗪类除草剂(包括有毒代谢物)残留量的分析方法。采用QuEChERS前处理方法,样品经1%(v/v)醋酸乙腈提取,乙二胺-N-丙基硅烷(PSA)净化处理,以Shim-pack XR-ODSII(75 mm×2.0 mm)为色谱柱,0.05%(v/v)甲酸溶液-乙腈为流动相梯度洗脱,在多反应监测(MRM)模式下测定。25种农药及其3种有毒代谢物的定量限(S/N≥10)为0.20～5.52 μg/kg;检出限(S/N≥3)为0.10～2.57 μg/kg;在各自的考察浓度范围内线性关系良好(r≥0.999);在0.20～55.2 μg/kg添加水平内,平均加标回收率为70.6%～125.7%,RSD为0.7%～14.2%。该方法样品前处理简单、快速、灵敏,可用于中药材中三唑类杀菌剂和三嗪类除草剂农药残留量的快速筛查。

关键词: QuEChERS, 超高效液相色谱-串联质谱法, 三嗪类除草剂, 三唑类杀菌剂, 中药材

Abstract: A method using QuEChERS clean-up followed by UPLC-MS/MS has been established for the quantitative determination of the residues of 10 triazole fungicides and 18 triazine herbicides in Chinese herbs including Radix Glycyrrhizae, Radix Panacis Quinquefolii, Salvia miltiorrhiza, Radix Notoginseng and Panax ginseng C. The pesticide residues were extracted from the samples by acetonitrile containing 1%(v/v) acetic acid, cleaned-up with primary secondary amine (PSA) and then analyzed using UPLC-MS/MS in multiple reaction monitoring (MRM) mode with positive electrospray ionization. The analytical column was Shim-pack XR-ODSII(75 mm×2.0 mm) and the mobile phases were water containing 0.05% (v/v) formic acid and acetonitrile in gradient elution. The limits of quantification (S/N≥10) of the 28 pesticides were 0.20-5.52 μg/kg and the limits of detection (S/N≥3) were 0.10-2.57 μg/kg. All of the pesticides had good linear responses with r≥0.999 and the average recoveries of the pesticides spiked in the Chinese herbs ranged from 70.6%-125.7% with the RSDs of 0.7%-14.2%. The results demonstrated that the method is simple, fast and sensitive to meet the requirements for the triazole fungicide and triazine herbicide residues and can be used for the analysis of the 28 pesticides in the above five Chinese herbs.

Key words: Chinese herbs, triazine herbicides, triazole fungicides, ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS), QuEChERS