Aspirin—A national survey III: Determination of impurities in bulk aspirin and aspirin formulations by high-pressure liquid chromatography and spectrophotometry

Autor: Kirchhoefer, Ross D., Reepmeyer, John C., Juhl, William E.
Zdroj: Journal of Pharmaceutical Sciences; May 1980, Vol. 69 Issue: 5 p550-553, 4p
Abstrakt: A quantitative high-pressure liquid chromatographic method, using a reversed-phase column and an aqueous acetic acid-methanol solution as the mobile phase, was employed for the determination of O-acetyl-O-salicylsalicylic acid and O-salicylsalicylic acid in pharmaceutical aspirin preparations. The aspirin was dissolved, filtered, and injected into the chromatograph. The absorbance of the impurities was measured at 254nm. Acetylsalicylic anhydride was determined by a spectrophotometric method. The aspirin was dissolved in pH 11.3 buffer and extracted with benzene. An aliquot of the benzene was evaporated, and the residue was dissolved in α-benzamidocinnamate-pyridine reagent. The acetylsalicylic anhydride was measured using the difference between the absorbance at 362 and 372nm. Possible interference of aspirin with the procedure is discussed. Thirty-four bulk aspirin and 172 tablet formulations were examined. Results for O-acetyl-O-salicylsalicylic acid, O-salicylsalicylic acid, and acetylsalicylic anhydride are given.
Databáze: Supplemental Index