HPLC-Q-TOF-MS分析注射用泮托拉唑钠中降解杂质

Analysis of Degradation Impurities in Pantoprazole Sodium for Injection by HPLC-Q-TOF-MS

关键词:  泮托拉唑钠  杂质  高效液相色谱-四级杆飞行时间质谱法  鉴定

Key words:  pantoprazole sodium  impurities  HPLC-QTOF-MS  determination

摘要:

目的 优化注射用泮托拉唑钠有关物质检查方法，并用高效液相色谱-四级杆飞行时间质谱法(HPLC-QTOF-MS)对注射用泮托拉唑钠中降解杂质进行结构鉴定。方法 采用色谱柱 Waters Symmetry C₁₈(250 mm×4.6 mm，5 μm)；流动相：10 mmol·L^-1乙酸铵(用乙酸调节pH至4.5)(A)-乙腈(B)，梯度洗脱(0~20 min，B相20%；20~30 min，B相20%→40%；30~45 min，B相40%→30%；45.01~65 min，B相20%)；流速：1.0 mL·min^-1；检测波长：289 nm；进样量：20 μL；柱温：35 ℃；离子源：ESI源；扫描模式：正离子模式。结果 优化后有关物质测定方法可有效分离各降解杂质。根据各降解杂质的二级质谱图以及高分辨数据，推测出了4个降解杂质的结构式。结论 所建立的色谱条件可有效检测注射用泮托拉唑钠中的有关物质，降解杂质结构式的确定为该产品稳定性研究提供了技术支持。

Abstract:

OBJECTIVE To improve the method for the examination of related substances in pantoprazole sodium for injection and establish an HPLC-Q-TOF-MS method for the structure determination of the degradation impurities. METHODS The analysis was performed on Waters Symmetry C₁₈(250 mm×4.6 mm, 5 μm) with the mobile phase consisting of 10 mmol·L^-1 ammonium acetate (adjusted to pH 4.5 by acetic acid)-acetonitrile in gradient mode. The detection wavelength was 289 nm and the flow rate was 1.0 mL·min^-1. The compound was ionized in the electrospray ionization(ESI) and operated in positive mode. RESULTS The improved method for the examination of related substances could separate the major degradation impurities effectively. According to the mass spectrum and high resolution data of degradation impurities in pantoprazole sodiu the structure of four degration impurities could be infered. CONCLUSION The chromatographic condition can detect the related substances in pantoprazole sodium for injection effectively. And the structure identification of the degradation impurities can provide technical support for stability study of this medicine.