基于保留指数原理结合气相色谱-三重四极杆质谱法快速筛查蔬菜中农药残留的方法研究

Rapid screening of pesticide residues in vegetables by gas chromatography tandem mass spectrometry based on retention index

目的建立气相色谱-三重四极杆质谱联用法快速筛查蔬菜中农药残留的方法。方法利用正构烷烃C9-C33标准溶液,结合气相色谱-三重四极杆质谱联用仪及其Smart Database Pesticides数据库建立仪器数据采集方法。选用9种农药为目标物,试样经QuEChERS方法进行萃取净化后,建立质谱多反应监测(multiple reaction monitoring,MRM)方法,进行定性、定量分析。结果采用空白样品添加标准溶液制得质量浓度为0.01、0.05、0.10mg/kg的样品,基于保留指数所建立的方法准确定性出待测9种农药,并测得方法的平均回收率为72.0%~118.8%。结论该方法简便、快速、成本低,具有较好的适用性,对监测农产品中农药的使用种类,更加全面合理地制定农产品中农残限量范围具有参考价值。

Objective To establish a method for rapid screening pesticide residues in vegetables by gas chromatography tandem mass spectrometry. Methods By using C9-C33 n-alkanes standard solution, combined with gas chromatography tandem mass spectrometry and its Smart Database Pesticides to establish the instrument data acquisition method. Nine pesticides were selected as the target, the samples were extracted and purified by QuEChERS method, and multiple reaction monitoring(MRM) method was established for qualitative and quantitative analysis. Results The 0.01, 0.05 and 0.10 mg/kg samples were prepared by adding standard solution to the blank sample. The method based on retention index was used to determine nine pesticides to be tested accurately. The average recovery of the method was 72.0%-118.8%. Conclusion This method is simple, rapid, low cost, and has good applicability. It is of reference value for monitoring the use of pesticides in agricultural products and formulating more comprehensive and reasonable limits of agricultural residues in agricultural products.