A novel stability-indicating UPLC method development and validation for the determination of seven impurities in various diclofenac pharmaceutical dosage forms

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• 作者：M. Azougagh^a ; ^{azougaghma@yahoo.fr" class="auth_mail" title="E-mail the corresponding author} ; M. Elkarbane^a ; K. Bakhous^b ; S. Issmaili^b ; A. Skalli^c ; S. Iben Moussad^d ; B. Benaji^c
• 关键词：Method development ; Validation ; Indicating stability ; UPLC ; Diclofenac ; Impurities
• 刊名：Annales Pharmaceutiques Françaises
• 出版年：2016
• 出版时间：September 2016
• 年：2016
• 卷：74
• 期：5
• 页码：358-369
• 全文大小：2747 K

文摘

An innovative simple, fast, precise and accurate ultra-high performance liquid chromatography (UPLC) method was developed for the determination of diclofenac (Dic) along with its impurities including the new dimer impurity in various pharmaceutical dosage forms. An Acquity HSS T3 (C18, 100 × 2.1 mm, 1.8 μm) column in gradient mode was used with mobile phase comprising of phosphoric acid, which has a pH value of 2.3 and methanol. The flow rate and the injection volume were set at 0.35 ml·min⁻¹ and 1 μl, respectively, and the UV detection was carried out at 254 nm by using photodiode array detector. Dic was subjected to stress conditions from acid, base, hydrolytic, thermal, oxidative and photolytic degradation. The new developed method was successfully validated in accordance to the International Conference on Harmonization (ICH) guidelines with respect to specificity, limit of detection, limit of quantitation, precision, linearity, accuracy and robustness. The degradation products were well resolved from main peak and its seven impurities, proving the specificity power of the method. The method showed good linearity with consistent recoveries for Dic content and its impurities. The relative percentage of standard deviation obtained for the repeatability and intermediate precision experiments was less than 3% and LOQ was less than 0.5 μg·ml⁻¹ for all compounds. The new proposed method was found to be accurate, precise, specific, linear and robust. In addition, the method was successfully applied for the assay determination of Dic and its impurities in the several pharmaceutical dosage forms.