QuEChERS结合超高效液相色谱-串联质谱法同时检测水产品中49种农兽药残留
目的 建立QuEChERS结合超高效液相色谱-串联质谱(ultra performance liquid chromatography- tandem mass spectrometry, UPLC-MS/MS)同时检测水产品中23种农药和26种兽药残留的方法。方法 样品用QuEChERS方法进行前处理, 经5%甲酸乙腈溶液提取, 用EMR-Lipid除脂萃取盐包净化去除脂质。用乙腈和0.1%甲酸水溶液作为流动相进行梯度洗脱, ZORBAX Eclipse Plus C18色谱柱进行色谱分离, 电喷雾正离子模式扫描, 多反应监测(multiple reaction monitoring, MRM)。结果 49种农兽药在2.0~100 μg/L浓度范围内线性关系良好, 相关系数大于0.990, 平均加标回收率为70.5%~109.6%。结论 该方法操作简单、灵敏度高, 可以同时分析性质差别较大的农药和兽药, 适用于水产品中49种农兽药残留的测定。
Objective To establish a method for simultaneous determination of 23 kinds of pesticide residues and 26 kinds of veterinary drug residues in aquatic products by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) with QuEChERS. Methods The samples were pretreated with QuEChERS method, extracted with 5% formic acid in acetonitrile and purified by EMR-Lipid. The purified liquid was separated by ZORBAX Eclipse Plus C18 chromatographic column with gradient elution of acetonitrile and 0.1% formic acid solution. The mass spectrometry was carried out by electrospray iron source in positive mode and multiple reaction monitoring (MRM). Results Forty-nine kinds of pesticide and veterinary drug residues showed good linear relationships in the concentration range of 2.0-100 μg/L, with the correlation coefficients above 0.990, and the average recoveries were 70.5%-109.6%. Conclusion This method is easy to operate and has high sensitivity, which can analyze pesticides and veterinary drugs with different properties at the same time, and can be used in the analysis of the residues of 49 kinds of pesticides and veterinary drugs in aquatic products.
标题：QuEChERS结合超高效液相色谱-串联质谱法同时检测水产品中49种农兽药残留
英文标题：Simultaneous determination of 49 kinds of pesticide and veterinary drug residues in aquatic products by ultra performance liquid chromatography-tandem mass spectrometry with QuEChERS
作者：
臧国栋 惠州市农产品质量安全监督检测中心
黄子敬 惠州市农产品质量安全监督检测中心
陈孟君 惠州市农产品质量安全监督检测中心
符靖雯 惠州市农产品质量安全监督检测中心
杨钦沾 惠州市农产品质量安全监督检测中心
刘战花 惠州市农产品质量安全监督检测中心
中文关键词:QuEChERS,农药残留,兽药残留,超高效液相色谱-串联质谱法,水产品,
英文关键词:QuEChERS,pesticide residues,veterinary drug residues,ultra performance liquid chromatography- tandem mass spectrometry,aquatic products,
发表日期：2018-03-01
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