基于GC-MS/MS联合HPLC-MS/MS测定大枣禁用农药残留

Determination of Forbidden Pesticide Residues in Jujube by GC-MS/MS Combined with HPLC-MS/MS

目的:建立QuEChERS结合气相色谱-串联质谱法(Gas Chromatography-tandem Mass Spectrometry,GC-MS/MS)联合高效液相色谱-串联质谱法(High Performance Liquid Chromatography-tandem Mass Spectrometry,HPLC-MS/MS)检测大枣禁用农药残留的方法。方法:样品以体积比为1%的乙酸乙腈为溶剂,高速匀浆,采用QuEChERS法净化处理样品,分别以气质法和液质法进行分析,气质法采用外标法定量,液质法采用内标法定量。结果:气相色谱-串联质谱法检测的35种农药线性关系良好,相关系数均≥0.9972,定量限为0.0001~0.0055 mg·kg^(-1),回收率为65.54%~101.03%,相对标准偏差为0.38%~11.54%。高效液相色谱-串联质谱法测定的30种农药线性关系良好,相关系数均≥0.9896,定量限为0~0.00049mg·kg^(-1),回收率为62.92%~109.96%,相对标准偏差为0.04%~3.71%。结论:该方法操作简便、高效、定量定性准确、灵敏度高、重现性和稳定性良好,适用于大枣禁用农药残留的快速检测。

Objective:The method of QuEChERS combined with gas chromatography-tandem mass spectrometry(GC-MS/MS)and high-performance liquid chromatography-tandem mass spectrometry(HPLCMS/MS)for the determination of forbidden pesticide residues in jujube was established.Method:The samples were purified by QuEChERS method using acetonitrile with 1%volume ratio as solvent and homogenized at high speed.The samples were analyzed by temperament method and liquid mass method respectively.The temperament method was quantified by external standard method,and the liquid mass method was quantified by internal standard method.Result:The linear relationship of 35 pesticides detected by gas chromatography-tandem mass spectrometry was good.The correlation coefficients were all greater than 0.9972,the limits of quantitation were 0.0001~0.0055 mg·kg^(-1),the recoveries were 65.54%~101.03%,and the relative standard deviations were 0.38%~11.54%.The 30 pesticides determined by high-performance liquid chromatography tandem mass spectrometry have good linear relationships.The correlation coefficients were all greater than 0.9896,the limits of quantification were 0~0.00049 mg·kg^(-1),the recoveries were 62.92%~109.96%,and the relative standard deviations were 0.04%~3.71%.Conclusion:This method is simple and efficient,with accurate quantitative and qualitative analysis,high sensitivity,good reproducibility and stability,and is suitable for the rapid detection of prohibited pesticide residues in jujube medicinal materials.