乙酰水杨酸中免疫原性杂质的比色分析

Colorimetric analysis of immunogenic impurities in acetylsalicylic acid.

作者信息

Bungaard H

出版信息

J Pharm Pharmacol. 1976 Jul;28(7):544-7. doi: 10.1111/j.2042-7158.1976.tb02791.x.

DOI:10.1111/j.2042-7158.1976.tb02791.x

Abstract

A rapid and convenient colorimetric method is described for the quantitative determination of the immunogenic impurities in acetylsalicylic acid, acetylsalicylsalicylic acid and acetylsalicylic anhydride. The method involves initial aminolysis of the compounds by ammonia to give salicylamide and subsequent coupling of this with 4-amino-phenazone in the presence of an oxidizing agent. In conjunction with a previously described method for analysis of the anhydride the method allows a specific determination of acetylsalicylsalicylic acid in concentrations down to 0-005%. Applying the methods to 15 different commercial acetylsalicylic acid samples and formulations, acetylsalicylic anhydride and acetylsalicylsalicylic acid were found to be present in amounts ranging from 0-001 to 0-024% and from 0-006 to 0-58% (w/w), respectively.

摘要

本文描述了一种快速便捷的比色法，用于定量测定乙酰水杨酸、乙酰水杨酸水杨酸酯和乙酰水杨酸酐中的免疫原性杂质。该方法包括先用氨对化合物进行氨解，生成水杨酰胺，然后在氧化剂存在下，将水杨酰胺与4-氨基苯腙偶联。结合先前描述的酸酐分析方法，该方法能够特异性测定低至0.005%浓度的乙酰水杨酸水杨酸酯。将这些方法应用于15种不同的市售乙酰水杨酸样品和制剂，发现乙酰水杨酸酐和乙酰水杨酸水杨酸酯的含量分别为0.001%至0.024%和0.006%至0.58%（w/w）。