HPLC-DAD-MS鉴定注射用雷贝拉唑钠杂质及其特征谱研究

目的利用高效液相色谱-二极管阵列检测器-质谱联用方法对注射用雷贝拉唑钠中杂质成分进行分析和结构推断。方法采用CenturySIL C18 BDS色谱柱(250 mm×4.6 mm,5μm),以磷酸盐缓冲液(磷酸氢二钠1.119 g和磷酸二氢钠0.179 g水溶液)-乙腈(体积比60∶40)为流动相,检测波长286 nm,流速1.0 mL·min-1,柱温(35±0.15)℃,进样量10μL,检测雷贝拉唑钠及其杂质;通过DAD检测器和质谱,获得在线紫外光谱图和质谱数据。结果通过在线紫外光谱图和质谱结果推断出可能含有的杂质结构,并测定了主要杂质含量限度。结论高效液相色谱-二极管阵列检测器-质谱联用技术可用于注射用雷贝拉唑钠中杂质的定性推断和定量测定。

Study on the impurities in rabeprazole sodium for injection using HPLC-DAD-MS

Objective To analyze and infer the impurities’ structures in rabeprazole sodium for injection by HPLC-DAD-MS. Methods The operation was carried out on a CenturySIL C₁₈ BDS column (250 mm×4.6 mm, 5 μm), with the mobile phase consisting of a mixture of phosphate buffer (disodium hydrogen phosphate 1.119 g and sodium dihydrogen phosphate 0.179 g)-acetonitrile (V︰V=60︰40). The detection wavelength was set at 286 nm, the flow rate was 1.0 mL·min^-1, the column temperature was（35±0.15）℃ and the injection volume was 10 μL, the rabeprazole sodium and its impurities were detected, the online UV spectrum and MS data were obtained by using DAD detector and MS. Results According to the results of online UV spectra and mass spectrometry, the feasible impurities’ structures were inferred and the limits of the main impurities were determined. Conclusion The method of HPLC-DAD-MS can be used to identify the impurities in rabeprazole sodium for injection.