XÂY DỰNG VÀ THẨM ĐỊNH QUY TRÌNH ĐỊNH LƯỢNG ĐỒNG THỜI ASPIRIN VÀ TẠP C TRONG VIÊN NÉN BẰNG KỸ THUẬT HPLC-DAD

Abstract

Background: Aspirin is an essential medicine included in the current essential medicines lists of the Ministry of Health of Vietnam and the World Health Organization. The determination of aspirin impurity C in tablet dosage forms is a mandatory quality requirement stipulated in the Vietnamese Pharmacopoeia V, the British Pharmacopoeia 2024, and the United States Pharmacopeia 2024. However, the official pharmacopoeial method for impurity C determination relies on a colorimetric technique, which is inherently limited in terms of analytical accuracy, selectivity, and sensitivity. To date, no studies conducted in Vietnam have reported a validated analytical method for the simultaneous quantification of aspirin and impurity C in tablet formulations. Objectives: To develop and validate a simultaneous HPLC-DAD method for determination of aspirin and impurity C in tablets. Materials and methods: Aspirin tablets and reference standard impurity C were used as analytical materials. A simultaneous quantitative method was developed and validated by HPLC-DAD in accordance with the International Council for Harmonisation (ICH) guidelines for analytical method validation. Chromatographic separation was achieved using a Phenomenex Gemini NX column (150 × 4.6 mm, 5 µm). The mobile phase consisted of acetonitrile and phosphoric acid–acidified water in a ratio of 40:60 (v/v), adjusted to pH 1.6 with an ionic strength of 0.5 M. The flow rate was set at 1.0 mL/min, and the column temperature was maintained at 25°C. Results: The developed HPLC-DAD method demonstrated excellent specificity, with complete baseline separation of aspirin and impurity C from the mobile phase and placebo components, and consistent retention times matching those of the reference standards. The method exhibited high precision, with relative standard deviation (RSD) values below 2% for both analytes. Calibration curves showed good linearity within the studied concentration ranges, with regression equations of y = 2733,6x + 28.537 for aspirin and y = 96.578x + 66.842 for impurity C. Method accuracy was confirmed, with recovery values ranging from 98% - 102%. Conclusion: A sensitive, selective, and reliable HPLC-DAD method for the simultaneous quantification of aspirin and impurity C in tablet dosage forms was successfully developed and validated in accordance with ICH guidelines. The proposed method is suitable for routine quality control and regulatory application