首批L-甲硫氨酸亚砜国家药品对照品的研制  

Establishment of the first batch of national drug reference standard of L-methionine sulfoxide

作　　者：刘景坤 张斗胜[1] 范慧红[1] 廖海明[1] LIU Jing-kun;ZHANG Dou-sheng;FAN Hui-hong;LIAO Hai-ming(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：《药物分析杂志》2024年第8期1373-1378,共6页Chinese Journal of Pharmaceutical Analysis

基　　金：中检院化药所学科建设项目(2024HYZX35)。

摘　　要：目的:建立首批L-甲硫氨酸亚砜国家药品对照品。方法:采用红外吸收光谱仪、核磁共振波谱仪及高分辨质谱仪对L-甲硫氨酸亚砜对照品原料进行结构确证,并检查其水分、炽灼残渣、金属元素含量、残留溶剂、有关物质,采用质量平衡法、液相色谱法及定量核磁法对其含量进行测定和计算,采用质量平衡法对其含量进行赋值,最后考察了其引湿性、均匀性和稳定性。结果:试验结果确证了L-甲硫氨酸亚砜的结构,水分为0.23%,炽灼残渣为0.20%,金属元素含量为10.87μg·g^(-1),有关物质为5.09%,未检出残留溶剂。以质量平衡法赋值首批L-甲硫氨酸亚砜对照品的含量为94.5%。本批次对照品含量均匀,短期稳定性试验结果证明L-甲硫氨酸亚砜短期内稳定。结论:首批L-甲硫氨酸亚砜国家药品对照品的研制成功,可用于氨基酸类药品有关物质的检查,规范相关药品质量,保证用药安全。Objective:To establish the first batch of national drug reference standard of L-methionine sulfoxide.Methods:The molecular structure of methionine sulfoxide was confirmed by the methods of IR,NMR and high resolution MS.Moreover,the moisture,residual solvents,residual ignition and related substances of L-methionine sulfoxide were determined,and then,its hygroscopicity,homogeneity and stability were also observed.Finally,mass balance method,HPLC and quantitative NMR were applied to determine and calculate its contents.Results:The results of experiments showed the structure of L-methionine sulfoxide were confirmed,its contents of moisture,residual ignition,metal elements and related substances were 0.23%,0.20%,10.87μg·g^(-1)and 5.09%.The residual solvents were not detected in the samples.The final content of methionine sulfoxide was 94.5%by mass balance method.The contents of this batch of L-methionine sulfoxide were uniform,and it is stable in short-terms.Conclusion:The first batch of national drug reference standard of L-methionine sulfoxide was established,and it is used for the inspection for related substances of amino acid drug,which is helpful in normalizing drug quality and guaranteeing drug safety.

关 键 词：L-甲硫氨酸亚砜 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]