QuEChERS法结合气相色谱-串联质谱法测定贝母类中药中53种农药残留

目的建立基于QuEChERS法结合气相色谱-串联质谱法(GC-MS/MS)对贝母类中药中53种农药残留量的快速检测方法,并应用于193批样品筛查。方法根据调研选择禁限用及常用农药作为检测指标。采用QuEChERS法对样品进行前处理,在气相色谱-串联质谱多反应监测(MRM)模式下进行测定,以3个添加水平测定样品的回收率和RSD。结果 53种农药在一定含量范围内线性关系良好,r均大于0.997 8;在1倍LOD(Limit of Detection)、2倍LOD、10倍LOD 3个添加浓度水平进行回收率试验中,86.8%的农药在60%～140%,RSD均小于15%;各农药检出限均小于0.01 mg/kg。193批贝母类中药种共检出14种农药,91批样品有检出,检出率为47.2%,仅有1批超出即将执行的《中国药典》2020年版限度规定。结论该方法检测指标具有一定针对性,且操作简便快速、灵敏可靠,适用于贝母类中药中农药残留的筛查测定。对于贝母类中药的生产种植和流通监管具有一定的参考意义。

Determination of 53 pesticide residues in different category of Fritillaria by QuEChERS and GC-MS/MS

Objective To establish a method for simultaneous determination of 53 kinds of pesticides residual in different category of Fritillaria by using QuEChERS and gas chromatography tandem mass spectrometry, and applying to 193 batches sample screening. Methods The forbidden, restricted and commonly used pesticides were selected as detecting indexes according to the result of this investigation. The samples were prepared by QuEChERS, and quantitative analysis was carried out by GC-MS/MS multiple-reaction monitoring (MRM) model. There were three supplemental levels for determining recoveries and RSD. Results The results showed that all the 53 pesticides had good linearity in certain ranges with the correlation coefficients (R) higher than 0.997 8. The recoveries of more than 86.8% pesticides were ranged from 60% to 140% at three supplemental levels (1×LOD, 2×LOD, and 10×LOD), with the RSDs less than 15%. The LOD ranged of all pesticides were below 0.01 mg/kg. The result of 193 batches sample screening showed that 91 batches sample were detected 14 pesticides, and the detection rate was 47.2%. Conclusion The detecting indexes is meaningful and the developed method is simple, rapid, sensitive, and reliable for screening multiple pesticide residues in different category of Fritillaria. The result has certain reference value for the cultivation and circulation supervision of different category of Fritillaria.