超高效液相色谱-串联质谱法检测畜禽肉中199种药物及代谢物残留

The Research of 199 Drugs and Metabolites Residues in Livestock And Poultry Muscle by UPLC-MS/MS

建立了一种可检测猪肉、鸡肉、牛肉和羊肉四种畜禽肉中199种药物及代谢物残留的超高效液相色谱-串联质谱法。样品经Mcllvaine-Na_(2)EDTA缓冲液和2%甲酸乙腈溶液提取后,高速离心去除蛋白质等杂质,用captiva EMR-Lipid小柱净化。以0.1%甲酸乙腈溶液和0.1%甲酸溶液为流动相洗脱,在C_(18)色谱柱上分离。ESI离子源正负离子模式同时扫描,并采用多反应监测模式(MRM)检测,基质匹配标准溶液外标法定量。结果表明:各药物及代谢物在空白猪肉、鸡肉、牛肉和羊肉基质匹配系列浓度范围内均呈现良好的线性关系,相关系数(r)均大于0.990;在4种基质中的定量限范围在0.5~20μg/kg之间;在定量限~200μg/kg添加浓度上的回收率范围为60%~120%,批内与批间相对标准偏差均小于20%。该方法具有简便快捷、选择性好、定性准确,重复性好等特点,可进行多种类药物及代谢物残留的同步处理和同时检测。对提高实际样品检测工作效率,更好的确保动物性食品安全,保护人类健康具有重要意义。

A UPLC-MS/MS method was established for the determination of 119 drugs and metabolites residues in livestock and poultry muscle.The samples were extracted with Mcllvaine-Na_(2)EDTA buffer and acetonitrile(2%formic acid),and the protein was deposited by high-speed centrifugation.Then the sample solutions were purified with EMR-Lipid extraction column.The mobile phase were water(0.1%formic acid)and acetonitrile(0.1%formic acid),and the samples were separated by C_(18) chromatography column.Ionization was performed using both positive and negative ion electrospray ionization(ESI^(+)/ESI^(-))at the same time,applying the detection mode of multiple reaction monitoring(MRM).The method was quantified by matrix matched standard curves.Good linearities of the calibration curves were obtained with the range of matrix matched standard curves in blank pig,chicken,cattle and sheep muscle,the correlation coefficients(r)>0.990.The limits of detection of the method were 0.5~20μg/kg.The recoveries were 60%~120%at the concentrations of LOQ~200μg/kg.The intra-and inter-batch variation coefficients were both less than 20%.With good selectivity,accuracy and repeatability,the method can be used for simultaneous treatment and simultaneous detection of various drug residues.It will be of great significance to improve the efficiency of actual sample detection,better ensure the safety of animal food and protect human health.