自动QuEChERS结合液相色谱-串联质谱法测定香叶中的212种农药残留

Detection of 212 kinds of pesticide residues in Laurus nobilis by automatic QuEChERS combined with liquid chromatography-tandem mass spectrometry

中文关键词:  自动QuEChERS  香叶  农药残留  液相色谱-三重四极杆串联质谱法

英文关键词:automatic QuEChERS  Laurus nobilis  pesticide residues  liquid chromatography-triple quadrupole tandem mass spectrometry

中文摘要:

      目的 建立自动QuEChERS结合液相色谱-三重四极杆串联质谱法测定香叶中212种农药残留。 方法 香叶样品用乙腈提取, 使用300 mg十八烷基硅烷键合硅胶(C18)+75 mg Nano-Carb、4.0 g无水硫酸镁和1.0 g氯化钠进行净化, 经自动样品制备系统进行制备后, 应用液相色谱-三重四极杆串联质谱法进行检测, 在电喷雾电离正离子模式下扫描, 动态多反应监测(dynamic multiple reaction monitoring, DMRM)模式下检测, 基质匹配外标法定量分析。结果 212种目标农药在各自线性范围内线性关系良好, 线性相关系数(r2)均大于0.995, 检出限(limits of detection, LODs)范围为1~5 μg/kg, 定量限(limits of quantitation, LOQs)范围为2~20 μg/kg, 在10、50和100 μg/kg的添加水平, 212种农药的平均回收率范围分别为70.35%~112.49%、70.30%~107.02%和72.39%~95.87%, 相对标准偏差均小于14.1%。结论 该方法快速、准确、灵敏度高, 能够应用于香叶中多农药残留的高通量定性筛查和准确定量, 并可扩展到其他香辛料多农药残留检测中。

英文摘要:

      Objective To establish a method for the detection of 212 kinds of pesticide residues in Laurus nobilis by automatic QuEChERS method combined with liquid chromatography-triple quadrupole tandem mass spectrometry. Methods Laurus nobilis samples were extracted by acetonitrile, purified with 300 mg C18+75 mg Nano-Carb, 4.0 mg anhydrous magnesium sulfate and 1.0 g sodium chloride. Then the samples were prepared by automatic extraction equipment, detected by liquid chromatography-triple quadrupole tandem mass spectrometry, scanned in electrospray ionized ion mode, and quantified by matrix matching external standard method with the dynamic multiple reaction monitoring (DMRM) mode. Results Two hundred and twelve kinds of target pesticides exhibited great linear relationships within their respective linear ranges, and linear correlation coefficients (r2) were all greater than 0.995, the limits of detection (LODs) were in the range of 1?5 μg/kg and the limits of quantification (LOQs) were in the range of 2-20 μg/kg, at 10, 50 and 100 μg/kg addition levels, the recoveries of 212 kinds of pesticides were 70.4%?112.5%, 70.3%?107.0% and 72.4%?95.9%, respectively, the relative standard deviations (RSDs) were all less than 14.1%. Conclusion This method is fast, accurate and sensitive, can be applied to the high-throughput qualitative screening and accurate quantification of multi-pesticide residues in Laurus nobilis, and can be extended to the high-throughput screening of multi-pesticide residues in other spices.