超高效液相色谱-串联质谱法测定水产品中50种兽药残留

Determination of 50 kinds of veterinary drug residues in aquatic products by ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  水产品  兽药残留  QuEChERS  超高效液相色谱-串联质谱法

英文关键词:aquatic products  veterinary drug residues  QuEChERS  ultra performance liquid chromate graphy-tandem mass spectrometry

中文摘要:

      目的 建立QuEChERS-超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)测定水产品中50种兽药残留(三苯甲烷类、酰胺醇类、硝基咪唑类、磺胺类、喹诺酮类)的方法。方法 样品经过含1%甲酸的乙腈溶液提取, 采用QuEChERS方法净化, 通过相同C18色谱柱分离, 经2个不同流动相系统(0.1%甲酸水溶液-甲醇、5 mmol/L乙酸铵水溶液-甲醇)梯度洗脱后, 采用UPLC-MS/MS电喷雾正离子模式、正负切换模式分别分析测定, 基质添加标准曲线外标或内标法定量。结果 50种药物标准曲线相关系数均>0.997, 检出限为0.032~0.356 μg/kg, 加标回收率为60.7%~114.0%, 相对标准偏差为1.06%~14.10%。结论 本方法快速、高效, 可应用于水产品中多种兽药残留的快速准确筛查和检测。

英文摘要:

      Objective To establish a method for the determination of 50 kinds of veterinary drugs residues (triphenylmethane, amidol, nitroimidazole, sulfonamide and quinolone) in aquatic products by QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods The sample were extracted with 1% formic acid in acetonitrile, purified with QuEChERS, separated by the same C18 chromatographic column, eluted by 2 different mobile phase systems (0.1% formic acid aqueous solution-methanol, 5 mmol/L ammonium acetate aqueous solution-methanol), and then analyzed by UPLC-MS/MS positive ion mode and positive/negative switching mode respectively, and quantified by matrix-added calibration with external or internal standard. Results The correlation coefficients of calibration curves of 50 kinds of veterinary drugs were more than 0.997, the limits of detection were 0.032?0.356 μg/kg, the average recoveries were 60.7%?114.0%, and the relative standard deviations were 1.06%-14.10%. Conclusion The method is quick and efficient, and is suitable for the determination of multi residues of veterinary drug residues in aquatic products.