目的 为有效控制复方氨基酸(15)双肽(2)注射液的产品质量,标定甘氨酰-L-酪氨酸的首批国家标准物质的含量,同时揭示肽类药品标准物质标定过程中的一些共性特殊问题。方法 采用紫外光谱、高分辨质谱和一维/二维核磁共振谱对其进行结构确证,利用高效液相色谱法进行有关物质的测定及稳定性考察,采用质量平衡法进行标准物质含量计算,并通过核磁共振定量法对质量平衡法的准确性进行验证。结果 确证了甘氨酰-L-酪氨酸的结构,并测定了首批甘氨酰-L-酪氨酸国家标准物质的含量为88.4%。结论 针对本品的特点,分别采用多种不同方法对本品进行定性与定量研究,确保国家对照品标定结果准确性。
Abstract
OBJECTIVE To verify a new reference standard for N-glycyl-L-tyrosine in order to assure the quality of amino acids (15) and dipeptides (2) injection. METHODS UV, HRMS,1H-NMR,13C-NMR and 2D NMR were used to confirm the structure, and the content of the product was calculated by mass balance method, which was also confirmed by titrimetric method. RESULTS The structure of this product was identified and the content of N-glycyl-L-tyrosine was assigned as 88.4%. CONCLUSION According to the physicochemical properties of the compound, were used multiple methods for the qualitative and quatitative analysis to ensure the calibration results of the national reference standard accurately. The first established N-glycyl-L-tyrosine national reference can be efficiently applied for the assay of amino acids (15) and dipeptides (2) injection.
关键词
甘氨酰-L-酪氨酸 /
质量平衡法 /
标准物质 /
结构确证 /
含量测定
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Key words
N-glycyl-L-tyrosine /
mass balance method /
reference standard /
structure confirmation /
content determination
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中图分类号：
R917
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参考文献
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