Beaulieu N, Curran N M, Gagné C, Gravelle M, Lovering E G
Health and Welfare Canada, Bureau of Drug Research, Ottawa, Ontario.
J Assoc Off Anal Chem. 1989 Mar-Apr;72(2):247-54.
Liquid chromatographic screening procedures have been developed for the estimation of vitamins A and D in multivitamin-mineral tablet, capsule, gelatin capsule, and syrup formulations. The procedure can be used for measuring vitamin A present as either retinyl acetate or retinyl palmitate, and also for measuring the contribution to total vitamin A activity from 13-cis retinyl esters. The retinyl esters and their isomers are resolved from each other and their oxidation products. Ergocalciferol and cholecalciferol are not resolved from each other but they are resolved from other vitamin D isomers and from vitamins A, E, and K and their degradation products. Both assays use a 3 microns amino column, with a mobile phase of hexane for vitamin A and 1% isopropanol in hexane for vitamin D. The precision of replicate injections for vitamins A and D is better than 1% and the recovery from spiked syrups is better than 98%. The coefficient of variation for both assay methods is about 5%. Twenty formulations were analyzed for vitamin A and 24 were analyzed for vitamin D.
已开发出液相色谱筛选程序,用于测定多种维生素 - 矿物质片剂、胶囊、明胶胶囊和糖浆制剂中的维生素A和D。该程序可用于测定以醋酸视黄酯或棕榈酸视黄酯形式存在的维生素A,也可用于测定13 - 顺式视黄酯对总维生素A活性的贡献。视黄酯及其异构体可彼此分离,并与它们的氧化产物分离。麦角钙化醇和胆钙化醇不能彼此分离,但它们可与其他维生素D异构体以及维生素A、E和K及其降解产物分离。两种测定均使用3微米氨基柱,维生素A的流动相为己烷,维生素D的流动相为己烷中1%的异丙醇。维生素A和D重复进样的精密度优于1%,加标糖浆的回收率优于98%。两种测定方法的变异系数约为5%。对20种制剂进行了维生素A分析,对24种制剂进行了维生素D分析。