首批N,S-二乙酰半胱氨酸国家药品对照品的研制  

Establishment of the First Batch of National Drug Reference Standard of N,S-diacetylcysteine

作　　者：刘景坤 张斗胜[1] 范慧红[1] 任丽萍[1] 廖海明[1] Liu Jingkun;Zhang Dousheng;Fan Huihong;Ren Liping;Liao Haiming(National Institutes for Food and Drug Control,NMPA Key Laboratory for Quality Research and Evaluation of Chemical Drugs,Beijing 102629,China)

机构地区：[1]中国食品药品检定研究院,国家药品监督管理局化学药品质量研究与评价重点实验室,北京102629

出　　处：《中国药事》2024年第11期1295-1300,共6页Chinese Pharmaceutical Affairs

基　　金：中国食品药品检定研究院化学药品检定所学科建设项目(编号2024HYZX35)。

摘　　要：目的:研制首批N,S-二乙酰半胱氨酸国家药品对照品,用于氨基酸类药品有关物质的检查,控制相关药品质量,保证患者用药安全。方法:采用高效液相色谱、红外吸收光谱、高分辨质谱及核磁共振谱对N,S-二乙酰半胱氨酸化学结构进行确证,检查其水分、炽灼残渣、无机离子、残留溶剂、有关物质等杂质的含量,采用液相色谱法、核磁共振谱定量法及质量平衡法对其含量进行测定和计算,并采用质量平衡法对其含量进行赋值,考察了其引湿性、均匀性和短期稳定性。结果与结论:试验确证了N,S-二乙酰半胱氨酸的分子结构,测得水分为0.05%,无机离子为0.21%,有关物质为0.90%,未检出残留溶剂。以质量平衡法赋值首批N,S-二乙酰半胱氨酸对照品,含量为98.8%。本批次对照品含量分布均匀,试验结果证明N,S-二乙酰半胱氨酸短期内稳定。Objective:To establish the first batch of national drug reference standard of N,S-diacetylcysteine which is used for the inspection for related substances of amino acid drugs to control the drug quality and guarantee the drug safety.Methods:The molecular structure of N,S-diacetylcysteine was confirmed by the methods of HPLC,IR,NMR and high resolution MS.Moreover,the moisture,residual solvents,residual ignition,inorganic ions and related substances of N,S-diacetylcysteine were all determined.HPLC,Mass Balance and NMR were applied to determine and calculate its content,and Mass Balance mehod was used for evaluating its final content.Finally,its hygroscopicity,homogeneity and short-term stability were also observed.Results and Conclusion:The results of experiments showed the structure of N,S-diacetylcysteine was confirmed,and its contents of moisture,inorganic ions and related substances were 0.05%,0.21%and 0.90%,respectively.The residual solvents were not detected in the samples.The final content of N,S-diacetylcysteine reference standard was 98.8%by mass balance method.The content distribution of this batch of N,S-diacetylcysteine reference standard was uniform,and its short-term stability result proved that N,S-diacetylcysteine was stable.

关 键 词：N S-二乙酰半胱氨酸 对照品 结构确证 有关物质 质量平衡法 

分 类 号：R917[医药卫生—药物分析学]