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使用UPLC-Q-Exactive Orbitrap-MS/MS和NMR对6-阿米诺尼基兰酸相关物质的表征

Jiajie Wu¹, Jing Lu¹, Ju Liu¹

¹China State Institute of Pharmaceutical Industry Co., Ltd., Shanghai 200120, China.

Journal of pharmaceutical and biomedical analysis

|September 20, 2025

概括

在各种条件下研究了6-Aminopenicillanic酸 (6-APA) 的降解. 青胺二硫化物被确定为一种新的氧化降解产物,有助于理解半合成青素合成中的杂质形成.

科学领域:

制药化学制药化学制药化学
分析化学分析化学
有机化学有机化学

背景情况:

6-阿米诺尼西兰酸 (6-APA) 是半合成青素抗生素的关键组成部分.
了解6-APA的稳定性和降解途径对于确保抗生素质量和安全至关重要.
强制降解研究对于识别潜在杂质和开发稳定性指示分析方法至关重要.

研究的目的:

在各种压力条件下调查6-aminopenicillanic acid (6-APA) 的强制降解.
识别和描述由此产生的降解产品,并阐明降解途径.
发现新的降解产品,包括氧化和还原物种.

主要方法:

在热性,性,酸性,氧化和光解应激下强制降解6-APA.
使用超高压液态染色学四极-精确轨道质量/质谱法 (UPLC-Q-精确轨道质量-MS/MS) 识别降解产品.
使用核磁共振 (NMR) 光谱和半准备性液体色谱 (半Prep-LC) 的结构阐明.

主要成果:

总共有18种相关物质被确定,包括与工艺相关的杂质和降解产品.
西二硫化物被确定为一种新的氧化降解产物 (RS7).
为6-APA提出了降解途径,在降解产品中确定了几对异构体对.

结论:

这项研究首次成功地确定了6-APA的氧化和还原降解产物.
这些发现为6-APA的稳定性概况和潜在的杂质形成提供了关键的见解.
这项研究有助于质量控制和开发半合成青素抗生素.

关键词:

6 - 氨基尼基兰酸 (6-APA)核磁共振 (NMR) 是一种核磁共振技术.相关物质相关物质超高压液体色谱-四极-精确轨道质量/质量谱 (UPLC-Q-精确轨道质量-MS/MS)

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