高效毛细管电泳法/液质联用分离与测控硫酸卷曲霉素各组分

Separation and determination of components of capreomycin sulfate

目的建立分离硫酸卷曲霉素组份的高效毛细管电泳法(HPCE)和液质联用(LC-MS),定性定量分析各组分。方法通过环糊精的种类及浓度、缓冲液的pH及浓度、温度及电压的优化,选择最佳的HPCE分离条件,并建立适合于LC-MS的分析条件。结果最佳的HPCE缓冲液为30mmol/L磷酸盐缓冲液(pH 2.5,内含8 mmol/L羧甲基-β-环糊精);检测波长为214nm;电压为30kV;温度为30℃,基线分离了卷曲霉素4个组分;采用XBP-C18色谱柱,电喷雾ESI为电离源,分析检测了卷曲霉素的各组分。结论建立的HPCE法和LC-MS法可用于为该产品的质量控制提供了可靠的分析方法。

Objective Qualitatively and quantitatively analyses were employed to establish HPCE and LC-MS methods for the separation of each component of capreomycin sulfate. Methods By optimizing factors which affect separation, the kinds and concentration of cyclodextrin, the pH value and concentration of buffer, the voltage and temperature, the optimum conditions for separation were selected. By choosing chromatography condition, LC-MS methode was established. Results Using phosphoric buffer containing carboxymethyl-β-cyclodextrin, the base-line separation of each component was achieved. By using XBP-Cls column, electrospray ionization and positive ion monitoring, components of capreomycin were analysed. Conclusion The new established HPCE and LC-MS methods were useful to quality control of capreomycin sulfate.