QuEChERS前处理技术结合气相色谱-串联质谱法测定药食同源中药材59种农药残留

Determination of 59 pesticide residues in Chinese medicinal materials with homology of medicine and food by QuEChERS pretreatment technology combined with gas chromatography tandem mass spectrometry

目的建立QuEChERS前处理技术结合气相色谱-串联质谱(GC-MS/MS)同时检测药食同源中药材59种农药残留的检测方法。方法中药材样品加水浸泡,精密加入1%醋酸的乙腈溶液10 ml和QuEChERS提取剂进行提取,离心,上清液经QuEChERS净化剂净化,离心后得到上清液,精密量取上清液2 ml至玻璃离心管中,40℃水浴中氮气浓缩至近干,乙酸乙酯溶解残渣,微孔滤膜过滤后进行GC-MS/MS检测,外标法定量。结果59种农药在5 ng/ml~500 ng/ml内线性关系良好,相关系数(r)均>0.99;平均回收率为67.9%~107.8%,相对标准偏差(RSD)为2.8%~8.6%;方法检出限为0.1μg/kg~4.6μg/kg;方法定量限为0.3μg/kg~12.0μg/kg。应用本方法检测温州市部分零售药食同源中药材,对农药残留进行风险监测发现,花类中药材的农药残留污染情况相对较为严重,金银花中共检出10种农药,其中毒死蜱检出率最高,为72.5%。结论本方法灵敏、简便、高效、准确、廉价、环保,可用于药食同源中药材多种农药残留的快速筛查与检测,为药食同源中药材的种植生产和质量管控提供技术支撑。

Objective This paper aims to establish a method for the simultaneous detection of 59 pesticide residues in Chinese medicinal materials with homology of medicine and food using QuEChERS pretreatment technology combined with gas chromatog⁃raphy-tandem mass spectrometry(GC-MS/MS).Methods Chinese medicinal material samples were soaked and accurately added to 10 ml of acetonitrile solution with 1%acetic acid and QuEChERS extraction agent for extraction and centrifugation;the supernatant was purified with QuEChERS purification agent.After centrifugation,the supernatant was obtained.2 ml of the supernatant was precisely measured and stored in a glass centrifuge tube,concentrated in nitrogen at 40℃in a water bath to nearly dry,dissolved in ethyl acetate,filtered with microporous filter membrane for GC-MS/MS detection,and quantified by external standard method.Results The linear ranges of 59 pesticides were within 5 ng/ml-500 ng/ml,with correlation coeffi⁃cients(r)greater than 0.99.The average recovery was within 67.9%-107.8%,and the relative standard deviation(RSD)was within 2.8%-8.6%.The detection limit of the method is within 0.1μg/kg-4.6μg/kg,and the quantitative limit of the method is within 0.3μg/kg-12.0μg/kg.This method is applied to detect some Chinese medicinal materials with homology of medicine and drug in Wenzhou City and monitor the risk of pesticide residues.The pesticide residue pollution of Chinese medic⁃inal materials such as flowers was relatively serious.A total of 10 pesticides were detected in Lonicera japonica,of which the highest detection rate of chlorpyrifos was 72.5%.Conclusion This method is sensitive,simple,efficient,accurate,inexpen⁃sive,and environmentally friendly,and can be used for the rapid screening and detection of multiple pesticide residues in Chinese medicinal materials with homology of medicine and food,providing technical support for the cultivation,production,and quality control of Chinese medicinal materials with homology of medicine and food.