超高效液相色谱-串联质谱法测定6种中药材中110种农药残留

建立了人参、黄芪、紫苏叶、白菊、益母草和五味子6种中药材中110种农药残留的超高效液相色谱-串联质谱(UPLC-MS/MS)分析方法。样品经乙腈提取,PSA固相萃取柱净化,正己烷液液分配,采用UPLC-MS/MS在正离子模式下以多反应监测扫描方式进行检测。结果表明:PSA柱结合正己烷液液分配净化可有效去除杂质干扰;分别在每种农药的定量限(LOQ)、5倍LOQ及20倍LOQ 3种浓度水平下进行添加回收率实验,110种农药的平均回收率在70.1%～95.7%之间,相对标准偏差(RSD)在0.8%～13.7%之间;供试110种农药的线性范围为其各自LOQ值的0.5～50倍,线性相关系数(r)在0.991～0.999之间;110种农药的检出限(LOD)在0.1～8.0 μg/kg之间,LOQ在2.0～100 μg/kg之间。该方法操作简单、净化效果好、灵敏度高,准确度和精密度均符合农药多残留分析的要求。

Determination of 110 pesticide residues in six Chinese herbal medicines by ultra performance liquid chromatography-tandem mass spectrometry

An ultra performance liquid chromatography-tandem mass spectrometric(UPLC-MS/MS) method was developed for the determination of the 110 pesticides in six Chinese herbal medicines.Pesticides were extracted with acetonitrile,cleaned up by PSA solid phase extraction column and then separated with UPLC and detected with MS/MS in multiple reaction monitoring(MRM) mode via positive electrospray ionization(ESI+).The method was validated at three fortification levels(LOQ,5 LOQ and 20 LOQ) in Panax ginseng C.A.Mey.,Astragali radix,Perilla leaf,Chrysanthemum,Motherwort herb and Chinese magnolivine fruit.The average recoveries of the 110 pesticides at three fortification levels were between 70.1%-95.7%,with relative standard deviations(RSDs) between 0.8%-13.7%.The standard calibration curves for 110 pesticides all showed good linearity over the range of 1/2 limit of quantification(LOQ) and 50 LOQ.The LOD of all the 110 pesticides in ginseng were between 0.1 μg/kg and 8.0 μg/kg,LOQ were between 2.0 μg/kg and 100 μg/kg.It was indicated that this method is easy,sensitive and can achieve a good cleanup effect.The sensitivity,accuracy and precision of the method were all acceptable,and it can meet the requirements of the multiple pesticide residues analysis.