食品科学 ›› 2020, Vol. 41 ›› Issue (16): 292-299.doi: 10.7506/spkx1002-6630-20190509-081

• 安全检测 • 上一篇    

QuEChERS-气相色谱-串联质谱法检测鱼腥草中121 种农药残留

苟琰,高驰,邓晶晶,耿昭,袁军,李敏,周娟,郭力,包晓明   

  1. (1.成都中医药大学药学院,四川 成都 611137;2.四川省食品药品检验检测院,国家药品监督管理局中成药质量评价重点实验室,四川 成都 611731;3.岛津企业管理(中国)有限公司,四川 成都 610023)
  • 发布日期:2020-08-19
  • 基金资助:
    国家中医药管理局中药标准化项目(ZYBZH-Y-SC-41)

Determination of 121 Pesticide Residues in Houttuynia cordata Thunb. by QuEChERS-Gas Chromatography Tandem Mass Spectrometry

GOU Yan, GAO Chi, DENG Jingjing, GENG Zhao, YUAN Jun, LI Min, ZHOU Juan, GUO Li, BAO Xiaoming   

  1. (1. College of Pharmacy, Chengdu University of Traditional Chinese Medicine, Chengdu 611137, China;2. Key Laboratory of Quality Evaluation of Chinese Patent Medicines, Sichuan Institute for Food and Drug Control, National Medical Products Administration, Chengdu 611731, China; 3. Shimadzu (China) Co. Ltd., Chengdu 610023, China)
  • Published:2020-08-19

摘要: 建立鱼腥草中121 种农药残留的QuEChERS-气相色谱-串联质谱方法,并应用于68 批样品筛查。对样品前处理和色谱方法进行优化。最终确定样品以乙腈进行提取,QuEChERS法进行净化处理,采用气相色谱-串联质谱在多反应监测模式下进行检测分析。121 种农药在一定含量范围内线性关系良好,相关系数(r)均大于0.997 3;3 个添加水平进行回收率实验表明,回收率在60%~140%范围内的农药数占总数的90.9%,86.8%的农药相对标准偏差小于15%。121 种农药检出限(RSN=3)范围为0.000 1~0.1 mg/kg,绝大多数小于0.01 mg/kg。68 批样品种共检出27 种农药。该方法简便、灵敏、准确,可用于鱼腥草中多农药残留的快速筛查与检测。检测结果为鱼腥草的种植生产和流通监管提供参考依据。

关键词: 鱼腥草;农药残留;气相色谱-串联质谱法;QuEChERS

Abstract: A multi-residue analysis method was developed for the determination of 121 pesticides in Houttuynia cordata Thunb. by the QuEChERS extraction procedure (the abbreviation of quick, easy, cheap, effective, rugged and safe) coupled with gas chromatography-tandem mass spectrometry (QuEChERS-GC-MS/MS). This method was applied for screening of 68 sample batches. The pesticide residues from the samples were extracted with acetonitrile and purified by a modified QuEChERS method before being detected by GC-MS/MS in the multiple reaction monitoring mode. The results showed that all 121 pesticides exhibited good linearity in certain ranges with correlation coefficients (r) higher than 0.997 3. The recoveries of more than 90.9% pesticides ranged from 60% to 140% at three spiked concentration levels, with relative standard deviations of less than 15% for 86.8% of the pesticides. The limits of detection (RSN = 3) of this method ranged from 0.000 1 to 0.1 mg/kg, below 0.01 mg/kg for most of the selected pesticides. A total of 27 pesticide residues were detected from the 68 sample batches. This simple, sensitive and accurate method proved to be suitable for the fast screening and detection of pesticide residues in H. cordata Thunb. in order to provide?a?basis for the cultivation and circulation supervision of H. cordata Thunb..

Key words: Houttuynia cordata Thunb.; pesticide residues; gas chromatography-mass spectrometry; QuEChERS

中图分类号: