Quality by Design (Qbd) Approach to Develop HPLC Method for Estimation of Gliclazide and its Impurity (Gliclazide Impurity A) in Bulk Drug

Author(s): Surendran Vijayaraj*, Narahari N. Palei, Thummala Katyayani.

Journal Name: Current Pharmaceutical Analysis

Volume 15 , Issue 7 , 2019

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Graphical Abstract:


Background: Gliclazide Impurity A (GI-A) is one of the gliclazide impurities, as described in the European Pharmacopoeia.

Objective: The objective of this study was to develop and validate simple, robust and accurate Reverse- Phase High-Performance Liquid Chromatography (RP-HPLC) method for estimation of gliclazide along with GI-A in bulk by optimising chromatographic parameters using Box Behnken design in response surface methodology.

Methods & Results: Box Behnken design was employed for optimizing flow rate, injection volume and strength of the buffer in order to minimize retention time of both gliclazide and GI-A. The optimized strength of orthophosphoric acid buffer in a mixture of Acetonitrile (50:50 v/v), flow rate and injection volume were found to be 25mM, 1mL/min, 20 µL respectively. Linearity was observed in concentration range of 25-150 µg/mL (r2=0.999). The retention time of gliclazide and GI-A was found to be 5.799 minutes and 3.819 minutes, respectively. The limit of detection for Gliclazide and GI-A was found to be 0.0066, and 0.0075 µg/mL and the limit of quantification limit was found to be 0.0202, 0.0228 µg/mL, respectively. The developed method was validated as per the ICH guidelines.

Conclusion: The proposed method is useful for best analysis of Gliclazide and GI-A in pharmaceutical dosage forms. QbD approach was found to be an effective tool for optimising chromatographic conditions of the proposed method.

Keywords: Gliclazide, Impurity A, RP-HPLC, Box Behnken design, QbD, bulk drug.

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Year: 2019
Page: [716 - 723]
Pages: 8
DOI: 10.2174/1573412914666180523092012
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