تطوير طريقة جديدة وفعاله لتحليل مركبات السلفاكوينولين صوديوم ، وفيتامين ك ? صوديوم ثنائي السلفايت ، والامبروليوم هيدروكلورايد مجتمعة معا في المستحضر البيطري والمصنع في شركة دار الشفاء A.S.K Validated HPLC Method to Simultaneously Determine Amprolium Hydrochloride, Sulfaquinoxaline Sodiumand Vitamin K3 in A.S.K Powder Manufactured byPharmacare-PLC

Date
2011-09-10
Authors
مشهور محمد 'فريد اسماعيل 'غانم
mashhour mohammad farid ismaiel ghanem
Journal Title
Journal ISSN
Volume Title
Publisher
AL-Quds University
جامعة القدس
Abstract
A new HPLC method that is based on zwitterionic hydrophilic interaction liquid chromatography (ZIC-HILIC) coupled with ultraviolet detection was developed, optimized and validated for simultaneous determination of Amprolium hydrochloride, Sulfaquinoxaline Sodium , and Vitamin K3 (as menadione sodium bisulfite) in A.S.K Powder. The separation was carried out using ZIC-HILIC column (250 mm×4.6 mm, 5 µm) and a mobile phase of 0.2 M Ammonium acetate (NH4AC) buffer and acetonitrile (ACN) (15:85; v/v) with pH adjusted to 5.7 by glacial acetic acid (G.A.A) at a flow rate of 0.5 ml/min. The analytes were monitored by UV detection at 263 nm. The effects of the operational chromatographic conditions on the separation and column efficiency were thoroughly investigated, including the concentration of the organic solvent (ACN) in the aqueous-organic mobile phase, the ionic strength of the NH4AC buffer and pH of the mobile phase. The optimized method was finally subjected to full analytical validation by examining specificity, accuracy, precision, linearity, range, ruggedness, robustness and stress conditions. The results were evaluated according to the International Conference on Harmonization (ICH) and United States Pharmacopoeia (USP33/NF28) guidelines and the method fulfilled validation criteria. In addition, the assay was shown to indicate stability and can be used to analyze for degradation products; for example; sulfaquinoxaline impurity A. The developed method is sensitive, specific, fast, accurate and requires minimum sample manipulation. The analysis time requires only 18 minutes. The new optimized HPLC method was applied on three commercial A.S.K batches for analysis of amprolium hydrochloride, sulfaquinoxaline sodium and vitamin K3. All the active ingredients were separated from excipients according to the authentic specifications.
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Keywords
ماجستير كيمياء, Master In Chemistry
Citation