药用辅料检验用磷脂酰胆碱对照品的研制

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。

Preparation of Reference Substances of Phosphatidylcholine for Pharmaceutical Excipients Inspection

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 ¹³C 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 ¹³C 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.