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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r>0.990 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。
OBJECTIVE To establish a GC-MS / MS and LC-MS / MS method for the determination of 187 pesticides residues in flower and fruit Chinese medicinal materials with honeysuckle and medlar as representative substrates. MS) detection method, and applied to more than 50 batches of eight herbs samples preliminary screening. Methods Based on the basic principles of risk control, we selected banned, high-risk and common pesticide varieties in our country as test indexes. During the experiment, the extraction solvent, purification conditions and chromatographic conditions were explored and optimized. The final method was extracted by acetonitrile and cleaned up by graphite carbon black solid phase extraction column. The separation was performed by gas phase and liquid chromatography, respectively, and was determined by tandem mass spectrometry in multiple reaction monitoring mode (MRM). Both GC-MS / MS and LC-MS / MS are calculated using internal standard methods to improve the accuracy of the results. Results The results showed that the method was linear between 1 and 100 ng · m L -1 with a correlation coefficient r> 0.990 0. When the mass ratio was 5, 20, 100 μg · kg ~ (-1) -1), the average recoveries of over 88% pesticides ranged from 70% to 120%. Conclusion The method has strong pertinence of detection indexes and covers most of the banned pesticides in Chinese herbal medicine. The detection method is rapid and accurate and is suitable for routine testing of pesticide residues in flowers and fruits.