超高效液相色谱-串联质谱法测定牛乳中6种兽药残留

Determination of 6 Kinds of Veterinary Drug Residues in Milk by Ultra Performance Liquid Chromatography-tandem Mass Spectrometry

目的:建立高效液相色谱-串联质谱法(high performance liquid chromatography-tandem mass spectrometry,HPLC-MS/MS)测定牛奶样品中6种兽药残留(硝碘酚腈、碘醚柳胺、氯氰碘柳胺、托曲珠利、三氯苯达唑、水杨酸钠)的检测方法。方法:样品经过乙腈溶液提取,以MAX固相萃取柱净化,采用Waters X Bridge BEH C_(18)色谱柱分离,流动相以乙腈和0.1%甲酸水溶液梯度洗脱,并使用电喷雾离子源,正负离子切换扫描模式进行检测,外标法定量。结果:6种兽药在0~10 ng/mL范围内呈现良好的线性关系,决定系数(R2)均大于0.995。6种兽药方法的检出限为0.06~0.18μg/kg,方法的定量限为0.5~2.0μg/kg。在添加量为0.5~8.0μg/kg的加标回收实验下,6种兽药加标回收率为67.1%~105.5%,相对标准偏差均小于10%。结论:该方法前处理操作简便,分析速度快,灵敏度高,可用于牛奶样品中的兽药残留测定。

Objective:To establish a high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)method for the determination of six veterinary drug residues in milk samples.Methods:The sample was extracted with acetonitrile solution,purified with MAX solid phase extraction column,and separated by Waters X Bridge BEH-C_(18)chromatographic column.The mobile phase was eluted with a gradient of acetonitrile and 0.1% formic acid aqueous solution,and electrospray ion source was used,positive and negative ion switching scanning mode for detection,external standard method for quantification.Results:The 6 veterinary drugs showed a good linear relationship in the range of 0~10 ng/mL,and the coefficient of determination(R^(2)) was greater than 0.995.The detection limit of the 6 veterinary drugs was 0.06~0.18 μg/kg.The limit of quantification of the method was 0.5~2.0 μg/kg.With the addition of 0.5~8.0 μg/kg in the standard recovery experiment,the recovery rates of the 6 veterinary drugs were 67.1%~105.5%,and the relative standard deviations were all less than 10%.Conclusion:This method is easy to operate,fast in analysis,and high in sensitivity.It can be used for the determination of veterinary drug residues in milk samples.