提出了猪肉中糖皮质激素类药物地塞米松、倍他米松、倍氯米松同时测定的超高效液相色谱-串联质谱法(UHPLC-MS/MS),采用串联四极杆质谱仪及超高效液相色谱仪联用.质谱离子源为电喷雾电离,检测方式为多反应监测正离子模式.超高压反相C18色谱柱分离,以不同比例配成的甲酸-水(1+999)溶液及乙腈的混合溶液作流动相进行梯度洗脱.上述3种药物的质量浓度在1.0~100.0 μg·L-1范围内呈线性.方法的回收率在83%~96%之间,地塞米松、倍他米松和倍氯米松的测定下限(10S/N)分别为1,1,2 μg·kg-1.

A method of determination of residual amounts of dexamethasone,betamethasone and beclomethasone in pork by hyphenation of UHPLC with MS/MS (in tandem) was proposed.The temdem quadripole mass spectrometer in hyphenation with ultra high performance liquid chromatography with ionization source of ESI+ and detection mode of MRM was used in the analysis.The C18 column was used as stationary phase,and mixtures of dil.formic acid (1+999) and acetonitrile in different proportions were used as mobile phase in the gradient elution of chromatographic separation.Linear relationships between values of analytical signal and mass concentration of the 3 drugs were obtained in the range from 1.0 to 100.0 μg·L-1.Results of recovery test were found in the range from 83% to 96%,and values of lower limit of determination (10S/N) found were 1 μg·kg-1 for dexamethasone and betamethasone,and 2 μg·kg-1 for beclomethasone.