超高效液相色谱-串联质谱测定猪肉中地塞米松、倍他米松和倍氯米松  

UHPLC-MS/MS Determination of Dexamethasone Betamethasone and Beclomethasone in Pork

作　　者：吴敏[1] 郑向华[1] 齐士林[2] 洪煜琛[1] 周昱[1] 

机构地区：[1]厦门出入境检验检疫局,厦门361026 [2]厦门大学化学化工学院化学系,厦门361005

出　　处：《理化检验（化学分册）》2010年第11期1282-1285,共4页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：国家质量监督检验检疫总局科研计划资助项目(2007IK137)

摘　　要：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1.0～100.0μg.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1,1,2μg.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.

关 键 词：超高效液相色谱 串联质谱 地塞米松 倍他米松 倍氯米松 猪肉 

分 类 号：O652.63[理学—分析化学]