盐酸法舒地尔有关物质的色谱-质谱结构鉴定

陈月琴; 宋  敏; 杭太俊

盐酸法舒地尔有关物质的色谱-质谱结构鉴定

Identification of the related substances in fasudil hydrochloride with hyphenated techniques

摘要

摘要:
采用WondaSil C₁₈ (250 mm × 4.6 mm ID, 5 μm) 色谱柱, 甲醇−醋酸铵缓冲溶液流动相梯度洗脱, 对盐酸法舒地尔有关物质进行分离; 采用正离子电喷雾−飞行时间质谱法测定准确质量和二级串联质谱分析离子结构特征, 并结合合成制备与波谱解析确证主要有关物质结构。结果显示, 盐酸法舒地尔与其有关物质分离良好, 检测出3个主要有关物质, 并综合分析鉴定了有关物质结构。色谱−质谱联用技术能有效地鉴定盐酸法舒地尔有关物质, 为其工艺和质量控制提供参考依据。

Abstract:
The study aims to identify the related substances in fasudil hydrochloride by hyphenated techniques. A WondaSil C₁₈ (250 mm × 4.6 mm, 5 μm) column was used for the separation of the related substances with a mixture of methanol and ammonium acetate buffer solution as the mobile phase by gradient elution. The structures of the related substances were speculated by electrospray positive ionization LC-TOF/ MS accurate ion mass and MS/MS determination and elucidation, and verified further through synthesis and spectroscopic analysis. Fasudil hydrochloride and the related substances were separated under the established HPLC condition. Three related substances in fasudil hydrochloride were characterized by hyphenated techniques. The hyphenated LC-MS method is useful for the identification of related substances in fasudil hydrochloride and the results obtained are valuable for its manufacturing process and quality control.

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