QuEChERS-超高效液相色谱-串联质谱法测定鱼和虾中苯巴比妥残留

Determination of phenobarbital residues in fish and shrimp by QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  苯巴比妥  鱼  虾  QuEChERS  超高效液相色谱-串联质谱法

英文关键词:phenobarbital  fish  shrimp  QuEChERS  ultra performance liquid chromatography-tandem mass spectrometry

中文摘要:

      目的 建立QuEChERS样品前处理结合超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)测定鱼和虾中苯巴比妥残留的方法。方法 样品采用乙腈提取, 经乙二胺-N-丙基硅烷(primary secondary amine, PSA)、C18、石墨化碳黑(graphitized carbon black, GCB)和无水硫酸镁(MgSO4)净化, 使用Agilent Eclipse Plus C18 色谱柱(50 mm×2.1mm, 1.8 μm)分离, 以甲醇(A)-水(B)为流动相进行梯度洗脱, 在UPLC-MS/MS多反应监测模式下进行定性和定量分析。结果 方法在0.5~100.0 μg/L的质量浓度范围内线性关系良好, 相关系数(r2)为0.9999, 检出限和定量限分别是0.5、1.5 μg/kg。草鱼、鲈鱼、罗非鱼和南美白对虾4种常见鲜活水产品经QuEChERS前处理, 有效降低基质干扰, 表现为可忽略的弱基质效应。对以上4种样品进行加标回收实验, 平均回收率为72.1%~96.7%, 相对标准偏差为1.2%~12.3% (n=6)。结论 该方法操作简便快速、灵敏度高、准确性和精密度好, 可满足水产品鱼和虾中苯巴比妥残留快速筛查和定量分析的需求。

英文摘要:

      Objective To develop a method for the determination of phenobarbital residues in fish and shrimp by pre-treatment of QuEChERS combined with ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods The samples were extracted by acetonitrile solution, purified with primary secondary amine (PSA), C18, graphitized carbon black (GCB), anhydrous magnesium sulfate (MgSO4), and separated by Agilent Eclipse Plus C18 column (50 mm×2.1 mm, 1.8 μm) by gradient elution using methanol (A)-water (B) as mobile phase. The qualitative and quantitative analyses were carried out under the multiple reaction monitoring modes of UPLC-MS/MS. Results This method had good linear relationship in the range of 0.5?100.0 μg/L, and the correlation coefficient (r2) was 0.9999. The limits of detection and quantitation were 0.5 and 1.5 μg/kg, respectively. Four kinds of common fresh aquatic products including Ctenopharyngodon idellus, Lateolabrax japonicus, Oreochroms mossambcus and Litopenaeus Vannamei pre-treated with QuEChERS could effectively reduce matrix interference, showing a negligible weak matrix effect. The average recoveries of the above 4 kinds of samples were 72.1%?96.7%, and the relative standard deviations were 1.2%?12.3% (n=6). Conclusion The proposed method is simple, fast, sensitive, accurate and precise, which is suitable for rapid and quantitative analysis of phenobarbital residues in fish and shrimp samples.