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

发布时间：2018-03-23 09:53

  本文选题：中药　切入点：农药多残留　出处：《中国药学杂志》2016年05期

【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·m L~(-1)之间线性良好,相关系数r0.990 0;在质量比为5、20、100μg·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 gas chromatography-tandem mass spectrometry (GC-MS / MS) and liquid chromatography-tandem mass spectrometry (LC-MS / MS) methods for the determination of 187 pesticide residues in Flos Lonicerae (Flos Lonicerae) and Fructus Lycii (Fructus Lycii). It was applied to the preliminary screening of more than 50 batches of 8 kinds of medicinal materials. Methods according to the basic principles of risk control, the banned, highly toxic and common pesticide varieties in China were selected as the detection indexes. The extraction solvent was used in the process of the experiment. The purification conditions and chromatography-mass spectrometry conditions were explored and optimized. The final method was extracted by acetonitrile and purified by solid phase extraction column with graphite carbon black, and separated by gas and liquid chromatography, respectively. Both GC-MS / MS and LC-MS/MS were calculated by internal standard method to improve the accuracy of the results. Results the method was linear with honeysuckle and wolfberry. The linear range of this method was 1100ng / mL ~ (-1). The average recovery rate of above 88% was between 70% and 120% in the three-level standard recovery experiment with a mass ratio of 5 ~ 20100 渭 g 路kg ~ (-1) ~ (-1). Conclusion the detection index of this method has strong pertinence and covers the banned pesticides in most Chinese herbal medicines, and the detection method is rapid. Accurate, suitable for the daily detection of pesticide residues in flowers and fruits.
【作者单位】： 中国食品药品检定研究院;
【基金】：国家十二五“重大新药创制”专项资助项目(2014ZX09304307-002)
【分类号】：R284.1;O657.63
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本文编号：1652943