液相色谱-四极杆飞行时间质谱法分析头孢拉定中的主要杂质
HPLC-Q-TOF-MS identification of major impurities in cefradine
分类号:
出版年·卷·期(页码):2013,33 (1):0-0
DOI:
10.16155/j.0254-1793.2017.01.01
-----摘要:-------------------------------------------------------------------------------------------
目的: 采用液相色谱-四极杆飞行时间串联质谱法(HPLC-Q-TOF-MS)分析头孢拉定中主要杂质并对其结构进行鉴定。方法: 色谱柱为Kromasil 100-5C18(250 mm×4.6 mm,5 μm),流动相为甲醇-10 mmol·L-1醋酸铵溶液(30:70);离子源:ESI离子源;扫描模式:正离子扫描。结果: 本方法通过四极杆-飞行时间二级质谱图特征碎片的分析确定了头孢拉定中1.32%的未知杂质为双氢头孢拉定,同时推测该杂质可能是中间体双氢苯甘氨酸中的杂质(四氢苯甘氨酸)参与合成引进的。结论: 本方法鉴定了头孢拉定中的1个未知杂质,进而可以对药品杂质控制和工艺优化提供参数。
-----英文摘要:---------------------------------------------------------------------------------------
Objective: To establish an HPLC-Q-TOF-MS method for the identification of major impurities in cefradine. Methods: The HPLC was performed on a Kromasil 100-5C18 column (250 mm×4.6 mm, 5 μm) with methanol-10 mmol·L-1 a mmonium acetate (30:70) as mobile phase.Data was collected under positive ion modes with ESI as ion resource. Results: The method identified an impurity with the content of 1.32% as dihydrocefradine based on analysis the feature fragmentation from Q-TOF.It was speculated that the impurity was introduced by intermediate dihydrophenylglycine impurities involved in the synthesis process. Conclusion: The method identified an unknown impurity in cefradine, and thus provide reference to its quality control and process optimization.
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