高效液相色谱-串联质谱法快速测定鸡肉中多种兽药残留

Rapid Determination of Veterinary Drug Residues in Chicken by High Performance Liquid Chromatography Tandem Mass Spectrometry

目的:本方法建立了鸡肉中磺胺类、喹诺酮类、大环内酯类、抗病毒类、镇定剂、糖皮质激素等40种兽药的高效液相色谱-串联质谱快速测定方法。方法:样品采用乙腈提取、ECS固相萃取柱净化,经C18柱分离,以甲醇-乙腈和甲酸-甲酸铵水溶液为流动相进行梯度洗脱,通过多反应监测模式检测,外标法定量。结果:40种化合物在2.0~50.0 ng·mL^(-1)范围内均呈现良好的线性关系,相关系数(R2)均大于0.99;空白样品添加浓度为2.0μg·kg^(-1)、5.0μg·kg^(-1)和10.0μg·kg^(-1)水平下,回收率为61.3%~116.2%,相对标准偏差(RSD)为0.7%~14.0%,其方法学指标均满足GB/T 27404—2008技术要求。结论:该方法具有操作简便、测定时间短、重复性好和准确度高等优点,可为快速筛查和确证鸡肉中多种兽药残留提供必要的技术支持。

Objective:To establish a method for rapid determination of sulfonamides,quinolones,macrolides,antiviral drugs,sedatives and glucocorticoids in chicken by high performance liquid chromatography tandem mass spectrometry(HPLC-MS/MS).Methods:The samples were extracted by acetonitrile and purified by ECS solid phase extraction column,then separated by C18 column.Methanol acetonitrile and formic acid ammonium formate aqueous solution were used as mobile phases for gradient elution.The samples were detected by multiple reaction monitoring mode and quantified by external standard method.Results:40 compounds showed good linear relationship in the range of 2.0~50.0 ng·mL^(-1),and the correlation coefficients were greater than 0.99;the recoveries were in the range of 61.3%~116.2% with the relative standard deviations of 0.7%~14.0% when the blank samples were added at the concentrations of 2.0μg·kg^(-1),5.0μg·kg^(-1) and 10.0μg·kg^(-1).The methodological indexes met the technical requirements of GB/T 27404—2008.Conclusion:The method has the advantages of simple operation,short determination time,good repeatability and high accuracy,which provides the necessary technical support for rapid screening and confirmation of veterinary drug residues in chicken.