Quality by Design Approach for the Development and Validation of Glipizide, an Antidiabetic Drug, by RP-UPLC with Application to Formulated Forms and Urine
Quality by design (QbD) refers to the achievement of certain predictable quality with desired and predetermined specifications. The objective of this study was to develop and demonstrate an integrated multivariate approach to develop and quantify the constituent concentrations of glipizide (GPZ) drug in its pure and tablet forms. The method was developed using Zorbax Extend C-18 (50？mm × 4.6？mm × 1.8？μm) column with mobile phase consisting of a mixture of phosphate buffer of pH 3.5 and acetonitrile (60？:？40？v/v). The method fulfilled validation criteria and was shown to be sensitive, with limits of detection (LOD) and quantitation (LOQ) of 0.001 and 0.005？μg？mL？1, respectively. The percentage relative standard deviations for robustness and ruggedness were observed within the range of 0.1 and 0.99. The calibration graph was linear in the range of 0.005–300？μg？mL？1. The applicability of the method was shown by the analysis of formulated drug and spiked urine samples. The proposed method can be used for routine analysis in quality control laboratories for its bulk and formulated product, and this is the first UPLC method reported for the assay of GPZ in bulk, formulated form and urine. 1. Introduction Quality by design (QbD) is a systematic approach to development that begins with predefined objectives and emphasizes product and process understanding and process control, based on sound science and quality risk management [1, 2]. The objective of the QbD initiative is to demonstrate both understanding and control of pharmaceutical processes to deliver high quality pharmaceutical products while affording opportunities for continuous improvement. QbD delivers a better understanding of method capabilities and limitations and ensures a superior chance of successful downstream method validation and transfer. It has become an important paradigm in the pharmaceutical industry since its introduction by the US Food and Drug Administration [3–8]. The QbD concept can be extended to analytical methods [9–16]. In addition, all international drug administration agencies endorse the QbD approach because it is expected that such performance-based routine methods can be changed within the analytical target profile without regulatory resubmission and approval. Glipizide (GPZ), chemically known as N-[2-[4-[[[(Cyclohexylamino) carbonyl] amino] sulfonyl]phenyl]ethyl]-5-methylpyrazine carboxamide] (Figure 1) is an oral antihyperglycemic agent [17] used in the treatment of noninsulin-dependent diabetes mellitus [18]. It lowers the blood glucose level in humans by stimulating the
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