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目的:建立中药材中20种农药残留同时检测方法,为中药材安全使用标准的建立提供科学依据。方法:20种农药残留同时检测方法中样品以丙酮超声提取,并采用凝胶渗透色谱(GPC)的方法进行净化,选用气相色谱-质谱串联技术(GC/MS)在DB-17MS毛细管柱上用程序升温技术分离,采用选择离子检测方式,以保留时间和特征离子进行目标成分的定性定量测定,以内标法对样品进行测定。结果:20种农药可在34 min内完全分离,工作曲线在10～1000μg.L-1的范围内有良好的线性关系,相关系数在0.9970～0.9999的范围内,检测限为0.5～2.4μg.kg-1,3个水平添加回收率在70%～120%之间,相对标准偏差小于11%(n=9)。结论:本方法灵敏度高,重现性好,可用于中药材中20种农药的残留检测。
Objective: To establish a method for simultaneous determination of 20 pesticide residues in Chinese herbal medicines, and provide a scientific basis for the establishment of standards for safe use of Chinese herbal medicines. Methods: The samples of 20 pesticide residue simultaneous detection methods were extracted by acetone and purified by gel permeation chromatography (GPC). The samples were separated on a DB-17MS capillary column by gas chromatography-mass spectrometry tandem mass spectrometry (GC / MS) Programmed temperature technology separation, the use of selected ion detection method, the retention time and characteristic ions of the qualitative and quantitative determination of the target component to the internal standard method for the determination of the sample. Results: The 20 pesticides could be completely separated within 34 min. The working curve had a good linear relationship in the range of 10 ~ 1000 μg.L-1 with the correlation coefficient of 0.9970 ~ 0.9999 and the detection limit of 0.5 ~ 2.4 μg. kg-1, 3 levels of recovery between 70% to 120%, the relative standard deviation of less than 11% (n = 9). Conclusion: The method has high sensitivity and good reproducibility, and can be used for the residue detection of 20 kinds of pesticides in traditional Chinese medicine.