药用辅料检验用磷脂酰胆碱对照品的研制

Preparation of Reference Substances of Phosphatidylcholine for Pharmaceutical Excipients Inspection

目的:建立含量测定用的大豆磷脂酰胆碱、蛋黄磷脂酰胆碱对照品。方法:采用红外光谱、质谱、核磁对原料进行结构确证,卡氏水分测定法测定水分,采用ICP-MS测定金属离子含量,采用HPLCELSD标准曲线法测定纯度,以质量平衡法计算对照品含量。结果:红外光谱、质谱、核磁确证了大豆磷脂酰胆碱、蛋黄磷脂酰胆碱对照品的结构;大豆磷脂酰胆碱、蛋黄磷脂酰胆碱水分测定结果分别为2.2%,2.1%;大豆磷脂酰胆碱、蛋黄磷脂酰胆碱金属离子含量分别为0.03%,0.01%;纯度测定结果分别为99.3%,95.6%;通过质量平衡法计算各对照品含量分别为97.1%,93.6%。结论:建立了大豆磷脂酰胆碱和蛋黄磷脂酰胆碱对照品,可用作药用辅料磷脂含量测定用对照品。

Objective： To determine the reference substances of soybean phosphatidylcholine and egg yolk phosphatidylcholine for content determination. Methods： The structure of raw material was confirmed by IR, HPLC-MS, ~1H NMR, and ^（13） C NMR. The water contents were determined by Karl Fischer method. The contents of metal ion of phosphatidylcholines were measured by ICP-MS. The purity was determined by HPLC-ELSD standard curve method, and the content of reference substance was calculated by mass balance method. Results： The structures of reference substances of soybean phosphatidylcholine and egg yolk phosphatidylcholine were confirmed by IR, HPLC-MS, ~1H NMR, and ^（13） C NMR. The water contents of soybean phosphatidylcholine and egg yolk phosphatidylcholine were 2.2% and 2.1% respectively. The contents of metal ion of soybean phosphatidylcholine and egg yolk phosphatidylcholine were 0.03%, and 0.01% respectively. The purities of soybean phosphatidylcholine and egg yolk phosphatidylcholine were 99.3%, and 95.6% respectively. The contents of reference materials of soybean phosphatidylcholine and egg yolk phosphatidylcholine were 97.1%, and 93.6% respectively. Conclusion： The reference materials of soybean phosphatidylcholine and egg yolk phosphatidylcholine for the content determination of pharmaceutical excipients were successfully provided.