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10.87 μg·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%, 10.87 μg·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.
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