Study of the Liquid Chromatography Retention of Some Fibrate-Type Antihyperlipidemic Drugs on C18 and CN Columns: Application for Quantitation in Pharmaceutical Formulations
The 6 antihyperlipidemic agents—bezafibrate, ciprofibrate, clofibrate, clofibric acid, fenofibrate, and gemfibrozil—were separated on octadecyl (C18) and cyano (CN) chemically bonded columns using mobile phases containing phosphate buffer and different amounts of acetonitrile, dioxane, propan-2-ol, methanol, and tetrahydrofuran. Relationships between log k values and mobile phase composition have been examined for these systems. Analysis was performed on a Waters LC system with Merck LichroCART C18 and CN 125 mm columns using a flow rate of 1 mL/min and 227 nm detection. More than one-half of the results fitted Snyder-Soczewinski equations with r > 0.995. Separation of all drugs was achieved on the C18 column with a mobile phase containing 45% propan-2-ol in phosphate buffer (pH = 2.145) and on a CN column with 20% acetonitrile in the same buffer. The best mobile phase, containing 45% propan-2-ol, was used to quantitate bezafibrate, ciprofibrate, fenofibrate, and gemfibrozil in pharmaceutical formulations. The active substances were extracted with methanol. The calibration curve was constructed in the 0.1–0.8 mg/mL range for all drugs and provided satisfactory linearity (Lack-of-Fit test and Mandel's test). The recovery function was sufficiently linear in all cases, with an insignificant intercept and slope very close to 1. Accuracy was tested by quantitating 3 fortified samples (50, 100, and 150%), which gave results without significant differences. None of the excipients interfered in the analysis. The recovery was 99.85% for bezafibrate, 99.02% for ciprofibrate, 99.53% for fenofibrate, and 99.92% for gemfibrozil, with relative standard deviation values of 0.63, 1.61, 1.84, and 0.88%, respectively.
No Reference information available - sign in for access.
No Citation information available - sign in for access.
No Supplementary Data.
No Article Media
Document Type: Research Article
Affiliations: Medical University, Department of Medicinal Chemistry, 6 Chodźki St, 20–093 Lublin, Poland.
Publication date: 2005-03-01
More about this publication?
- The Journal of AOAC INTERNATIONAL publishes refereed papers and reviews in the fields of chemical, biological and toxicological analytical chemistry for the purpose of showcasing the most precise, accurate and sensitive methods for analysis of foods, food additives, supplements and contaminants, cosmetics, drugs, toxins, hazardous substances, pesticides, feeds, fertilizers and the environment available at that point in time. The scope of the Journal includes unpublished original research describing new analytical methods, techniques and applications; improved approaches to sampling, both in the field and the laboratory; better methods of preparing samples for analysis; collaborative studies substantiating the performance of a given method; statistical techniques for evaluating data. The Journal will also publish other articles of general interest to its audience, e.g., technical communications; cautionary notes; comments on techniques, apparatus, and reagents.
- Information for Authors
- Submit a Paper
- Subscribe to this Title
- Information for Advertisers
- Journal Information
- Ingenta Connect is not responsible for the content or availability of external websites