超高效液相色谱-串联质谱法测定虾肉中52种兽药残留

Simultaneous Determination of 52 of Veterinary Drug Residues in Shrimp by Ultra-performance Liquid Chromatography-tandem Mass Spectrometry

试验旨在建立超高效液相色谱-串联质谱(UPLC/MS/MS)同时测定虾肉中6个大类52种兽药残留检测方法。样品经1%甲酸乙腈溶液均质提取,采用QuEChERS EMR-Lipid技术净化后,使用三重四极杆液质联用仪测定,基质曲线外标法定量。目标物在ZORBAX Eclipse plus C_(18)色谱柱上,以0.2%甲酸水溶液和乙腈溶液(含0.2%甲酸)作为流动相,采用梯度洗脱模式进行色谱分离,质谱离子源为电喷雾离子源(ESI),多重反应监测模式(MRM)。结果显示,在5.0~500μg/L质量浓度范围内52种兽药残留线性关系良好,线性相关系数(r^(2))均大于0.99,检出限范围在0.36~14.00μg/kg。向虾肉中添加2.0~100μg/kg药物(n=6),目标化合物回收率为61.2%~119.5%,相对标准偏差为1.0%~13.7%。该方法灵敏高效、准确可靠、重复性稳定,适用于虾类兽药残留的同时筛查检测,具有较高的实际应用价值。

A rapid method was developed for the simultaneous determination of 52 veterinary drug residues, including macrolides, chloramphenicol, nitromidazoles, sulfonamides, tetracyclines and quinolones in shrimp by QuEChERS combined with ultrahigh performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS). The sample was extracted with acetonitrile containing 1% formic acid, and purified with QuEChERS EMR-Lipid. The extract was evaporated under nitrogen stream, and redissolved with 20% acetonitrile. The UPLC separation was performed on ZORBAX SB-C_(18) column by gradient elution. The analysis of target compounds was carried out with electrospray ionization(ESI) under multi-reaction monitoring(MRM) mode. The external standard method was used for quantification. Under the optimal condition, the correlation coefficients for 52 veterinaries were larger than 0.99, and the limits of detection ranged from 0.36 μg/kg to 14.00μg/kg. The recoveries of 52 veterinary at the three spiked levels were between 61.2% and 119.5%, and their relative standard deviations were in the range of 1.0% to 13.7%. The methods were suitable for the determination of veterinary drug residues in shrimp and could be used for residue control programs.