超高效液相色谱-串联质谱法测定水果中42种农药残留

Determination of 42 pesticides in fruits by ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  超高液相色谱-串联质谱法  农药残留  QuEChERS  水果

英文关键词:ultra performance liquid chromatography-tandem mass spectrometry  pesticide residues  QuEChERS  fruits

中文摘要:

      目的 建立QuEChERS-超高效液相色谱-串联质谱法检测水果中42种农药残留的分析方法。方法 优化前处理的步骤、质谱参数和流动相组分, 分析水果中检出率较高的42种农药。样品经乙腈提取, 以900 mg MgSO4和150 mg乙二胺-N-丙基硅烷对样品进行净化, 利用ACQUITY UPLC HSS T3色谱柱分离, 在多反应监测模式下监测, 外标法定量。结果 42种农药在10~200 ng/mL线性范围内相关系数均大于0.995, 方法定量限为0.9~3.6 μg/kg, 回收率为70.7%~118.8%, 相对标准偏差为1.2%~13.1%。结论 该方法操作简便、灵敏度高, 适用于水果中农药残留的分析。

英文摘要:

      Objective To develop an analytical method for the determination of 42 pesticides in fruits by QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry. Methods The 42 pesticides with high detection rate in fruits were analyzed through optimizing pretreatment steps, mass spectrum parameters and mobile phase components. The samples were extracted with acetonitrile and cleaned up using 150 mg primary secondary amine (PSA) and 900 mg magnesium sulfate (MgSO4). The target compounds were separated on ACQUITY UPLC HSS T3 column, detected in multiple reaction monitoring mode and quantified by external standard method. Results The correlation coefficients of 42 pesticides in the range of 10?200 ng/mL were larger than 0.995. The limits of quantification (LOQs) were 0.9?3.6 μg/kg. The recoveries were 70.7%?118.8% and the relative standard deviations were 1.2%?13.1%. Conclusion This method is simple, sensitive and suitable for the determination of pesticide residues in fruits