液相色谱-质谱联用法检测药品中非法添加的醋酸泼尼松和布洛芬

Detection of Prednisone Acetate and Ibuprofen Mixed Illegally into Drugs by Combined Liquid Chromatography and Mass Spectrometry Method

目的检测制剂中非法掺入的醋酸泼尼松和布洛芬。方法采用液相色谱-质谱联用法,选用Venusil MP C18色谱柱(4.6mm×150mm,5μm),以0.01mol/L醋酸铵(用冰醋酸调pH值至3.0)-乙腈(50∶50)为流动相,对非法制剂的提取液进行液相色谱-质谱联用分析,与对照品的色谱、紫外及质谱行为比较,对此类非法制剂进行定量测定和定性鉴别。结果在这些非法制剂中均检出了醋酸泼尼松和布洛芬,且两者的加样回收率分别为98.95%和98.87%(n=6)。结论方法选择性强、灵敏度高,可分析检测非法制剂中的醋酸泼尼松和布洛芬。

Objective To develop a specific method for prednisone acetate and ibuprofen mixed illegally into drugs, Methods The combined liquid chromatography and mass spectrometry method were used. The Venusil MP C18 column was used with the mobile phase of 0. 01 mol/L ammonium acetate solution（adjusted to pH 3.0 with acetic acidglacial）- acetonitrile（50 ： 50）. Prednisone acetate and ibuprofenmixed illegally into drug was identified according to the chromatographic .behavior and mass spectral data by comparison with those of reference substances. Results Prednisone acetate and ibuprofen were found in illegal drugs, Their average recovery rates were 98.95% and 98.87% （n=6）,respectively. Conclusion The method is highly selective. It sensitive and can be used to detect prednisone acetate and ibuprofen mixed into illegal drug.