花类、果实类中药材中禁限用及常用农药多残留检测方法的建立

王莹,金红宇,魏赫,孙磊,马双成

中国药学杂志 ›› 2016, Vol. 51 ›› Issue (5) : 404-412.

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中国药学杂志 ›› 2016, Vol. 51 ›› Issue (5) : 404-412. DOI: 10.11669/cpj.2016.05.014
论 著

花类、果实类中药材中禁限用及常用农药多残留检测方法的建立

  • 王莹,金红宇,魏赫,孙磊,马双成*
作者信息 +

Determination of Forbidden and Restrictted Pesticides in Flowers and Fruits of Traditional Chinese Medicines

  • WANG Ying, JIN Hong-yu, WEI He, SUN Lei, MA Shuang-cheng*
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文章历史 +

摘要

目的 以金银花、枸杞子为代表性基质,建立了花和果实类中药材中187种农药多残留的气相色谱-串联质谱(GC-MS/MS)及液相色谱-串联质谱(LC-MS/MS)检测方法,并应用于8种药材50余批次样品初步筛查。方法 依据风险控制的基本原则选择我国禁限用、高毒高风险及常用农药品种作为检测指标。实验过程中对提取溶剂、净化条件及色谱质谱条件都进行了探索和优化。最终方法经乙腈超声提取,石墨炭黑固相萃取柱净化,分别以气相和液相色谱分离,在串联质谱多反应监测模式(MRM)下进行测定。GC-MS/MS和LC-MS/MS皆采用内标法计算以提高结果 的准确性。结果 以金银花、枸杞子作为考察对象,本方法在1~100 ng·mL-1之间线性良好,相关系数r>0.990 0;在质量比为5、20、100 μg·kg-1的三水平加标回收实验中,88%以上的农药平均回收率在70%~120%之间。结论 该方法检测指标针对性强,涵盖大部分中草药中的禁限用农药,检测方法快速、准确,适用于花类、果实类中药中农药残留的日常检测。

Abstract

OBJECTIVE To establish a method for simultaneous determination of 187 kinds of pesticides in flowers and fruits of traditional Chinese medicine (TCM) by using gas and liquid chromatography tandem mass spectrometry, taking medlar and honeysuckle as examples. METHODS The forbidden, restrictted and commonly used pesticides were picked out as detecting indexes according to the principals of risk management. The factors affecting the extraction, purification, and detection were optimized, and the final condition was established as follows: the samples were extracted with acetonitrile, and cleaned-up by carb solid phase extraction column. The separation of target compounds were performed by capillary or liquid column, and quantitative analysis was carrid out by GC-MS/MS or LC-MS/MS with MRM model. Internal standard was used to improve the accuracy of this method. RESULTS Honeysuckle flower and Wolfberry were used to evaluate the accuracy of this method. The calibration curves were linear in the range of 1-100 ng·mL-1 with correction coefficients of greater than 0.99. The recoveries of more than 88% pesticides were ranged from 70% to 120% at three spiked levels (5,20 and 100 μg·kg-1). CONCLUSION The detecting indexes in this method cover most forbidden and restricted pesticides, which is meaningful for the safety supervision of TCM. With the advantage of rapidness and accuracy, this method can be used for routine determination of multi-pesticides in flowers and fruits of TCM.

关键词

中药 / 农药多残留 / 禁限用农药 / 果实 / / 气相色谱串联质谱法 / 液相色谱串联质谱法

Key words

traditional Chinese medicine / multi-pesticide residue / forbidden and restricted pesticide / fruit / flower / gas chromatography tandem mass spectrometry / liquid chromatography tandem mass spectrometry

引用本文

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王莹,金红宇,魏赫,孙磊,马双成. 花类、果实类中药材中禁限用及常用农药多残留检测方法的建立[J]. 中国药学杂志, 2016, 51(5): 404-412 https://doi.org/10.11669/cpj.2016.05.014
WANG Ying, JIN Hong-yu, WEI He, SUN Lei, MA Shuang-cheng. Determination of Forbidden and Restrictted Pesticides in Flowers and Fruits of Traditional Chinese Medicines[J]. Chinese Pharmaceutical Journal, 2016, 51(5): 404-412 https://doi.org/10.11669/cpj.2016.05.014
中图分类号: R284   

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基金

国家十二五“重大新药创制”专项资助项目(2014ZX09304307-002)
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