固相萃取-气相色谱-串联质谱法快速监测酸枣仁中有机氯类农药残留

Rapid determination of organochlorine pesticide in Ziziphi Spinosae Semen by Carb/NH2-solid phase extraction-gas chromatography-tandem mass spectrometry

中文关键词:  有机氯农药  固相萃取  气相色谱-串联质谱法  多离子反应监测  酸枣仁

英文关键词:organochlorine pesticide  solid phase extraction  gas chromatography-tandem mass spectrometry  multiple reactions monitoring  Ziziphi Spinosae Semen

中文摘要:

      目的 建立固相萃取柱净化联合气相色谱-串联质谱法(Carb/NH2-solid phase extraction-gas chromatography-tandem mass spectrometric, Carb/NH2-SPE-GC-MS/MS)快速检测79批市售酸枣仁中13种有机氯农药残留, 并结合实际污染水平评估有机氯农药的暴露风险。方法 样品经乙腈提取, Carb/NH2 SPE柱净化后, 采用多离子反应监测模式(MRM)对13种农药残留定量监测。结果 13种有机氯农药在5～400 μg/kg浓度范围内与对应的峰面积呈现良好的线性关系良好(r2＞0.996), 检出限均低于3 μg/kg。本方法应用于79批酸枣仁样品中13种农药的检测, 仅1批检出七氯和反式氯丹残留, 检出浓度均为0.0025 mg/kg, 低于限量规定(0.05 mg/kg), 慢性暴露风险%ADI为3.95E-03、1.96E-02, 表明其无明显健康风险。结论 本法操作简单、快速、灵敏度高, 可准确监控酸枣仁中有机氯类农药残留。

英文摘要:

      Objective To establish a method for rapid determination of 13 kinds of organochlorine pesticide residues in 79 batches of commercial Ziziphi Spinosae Semen based on Carb/NH2-solid phase extraction purification and gas chromatography tandem mass spectrometry (GC-MS/MS), and evaluate the exposure risk of organochlorine pesticides according to the actual pollution level. Methods Ziziphi Spinosae Semen samples were extracted with acetonitrile and purified by Carb/NH2 SPE column. The multiple reactions monitoring (MRM) mode was used to detect 13 organochlorine residues. Results The 13 kinds of organochlorine pesticides and their peak area had good linear relationships in the range of 5-400 g/kg (r2>1.996), and the limits of detection were all below 3 μg/kg. The method was applied for determination of 13 kinds of pesticides in 79 batches of Ziziphi Spinosae Semens. Among the samples, one batch was found contamination with heptachlor and trans-chlordane, and the detected concentrations were 0.0025 mg/kg (below the limit standards of 0.05 mg/kg). Chronic exposure risk %ADI were 3.95E-03 and 1.96E-02, indicating no significant health risk. Conclusion The Carb/NH2-SPE-GC-MS/MS method is simple, rapid and sensitive, which can accurately and quantitatively analyze the multi-component pesticide residues in Ziziphi Spinosae Semen.