二维超高效液相色谱质谱联用技术测定注射用头孢替唑钠的杂质谱

Study on the Impurity Profile of Ceftezole Sodium for Injection by 2D-UPLC-MS

建立了二维超高效液相色谱质谱联用法(2D-UPLC-MS)研究注射用头孢替唑钠的杂质谱。一维色谱采用Waters BEH C18色谱柱,以枸橼酸溶液∶乙腈(90∶10)为流动相A,乙腈为流动相B,梯度洗脱,检测波长254nm;二维色谱采用Waters HSS T3 C18色谱柱,以0.1%甲酸水溶液为流动相A,0.1%甲酸的乙腈溶液为流动相B,梯度洗脱;质谱采用电喷雾离子源,正离子模式检测。对注射用头孢替唑钠中的10个杂质进行结构推断。本研究建立的方法可用于注射用头孢替唑钠杂质谱的分析,为更好地控制本品的质量提供帮助,也为同类药物杂质谱的研究提供思路。

A two-dimensional ultra high performance liquid chromatography-mass spectrometry (2D-UPLCMS) method was established to investigate the impurity profile of ceftezole sodium for injection. One-dimensional chromatographic conditions were listed. A Waters BEH C18 column was adopted. Citrate solution∶acetonitrile (90∶10) was used as the mobile phase A and acetonitrile as the mobile phase B. Gradient elution was used and the detection wavelength was 254 nm. Two-dimensional chromatographic conditions were summarized. A Waters HSS T3 C18 column was adopted, with water containing 0.1% formic acid as the mobile phase A and acetonitrile containing 0.1% formic acid as the mobile phase B. Gradient elution was used. Electrospray ionization (ESI) source was used at positive ion detection mode. Ten impurities of ceftezole sodium were characterized. This method can be used to study the impurity profile of ceftezole sodium for injection, which is helpful to control the drug quality effectively. It also provides ideas for the research of impurity profile of the similar drugs.