超高效液相色谱-串联质谱法测定牛乳中6种兽药残留

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...

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

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-C₁₈chromatographic 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(R²) 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.