Zhejiang University of Technology, Hangzhou 310004, China.
Zhejiang Institute for Food and Drug Control, Hangzhou 310052, China.
J Pharm Biomed Anal. 2019 Oct 25;175:112793. doi: 10.1016/j.jpba.2019.112793. Epub 2019 Jul 25.
A simple and sensitive method was developed for separation and characterization of seventeen impurities from commercial latamoxef sodium for injection by liquid chromatography combined with electrospray ionization and QTOF mass spectrometer (LC-ESI-QTOF MS). The chromatographic separation was performed on a Boston Green ODS-AQ C18 column (250 mm × 4.6 mm, 5 μm) under gradient mode using binary mobile phase: (A) ammonium acetate (10 mM)-methanol (99:1, v/v) and (B) ammonium acetate (10 mM)-methanol (70:30, v/v). Based on tandem multistage MS and high resolution MS data, the molecular formulas and structures of unknown impurities were inferred. A plausible formation mechanism of impurities was also proposed. In addition, the fragmentation regularity of degraded impurities in positive-ion mode was summarized.
建立了一种简单、灵敏的液相色谱-电喷雾串联四级杆飞行时间质谱（LC-ESI-QTOF MS）法，用于分离和结构鉴定注射用拉氧头孢钠中的 17 个杂质。采用梯度洗脱方式，以 Boston Green ODS-AQ C18 柱（250mm×4.6mm，5μm）为色谱柱，流动相 A 为 10mmol/L 乙酸铵-甲醇（99∶1，v/v），流动相 B 为 10mmol/L 乙酸铵-甲醇（70∶30，v/v）。根据串联多级质谱和高分辨质谱数据，推断出未知杂质的分子式和结构，并提出了可能的杂质形成机制。此外，还总结了在正离子模式下降解杂质的碎裂规律。
