Development and validation of a quality by design enabled robust LC method for estimation of daptomycin in pharmaceutical dosage form

Abstract

A simple and new validated liquid chromatography method with stability‐indicating potential was established for quantifying daptomycin in formulations using a quality by design approach. Analytical target profile establishment and earmarking critical analytical attributes helped to control the method performance. Further, the control strategies for critical method variables were defined as per method intent. Youden's robustness test was applied with the dual intent of defining control strategies and evaluating method robustness for continuous method improvement. Chromatography for the purpose constituted of methanol: water (pH 3.5 maintained by o‐phosphoric acid), 90:10, v/v as mobile phase flowing at 1.2 mL/min on a C18 column. Photodiode array detector provided the best results at 367 nm. Results for parameters viz. linearity (5‐200 µg/mL), accuracy (> 99%) and precision (< 1%) advocated method reliability. The detection (2.5 µg/mL) and quantitation limits (5 µg/mL) were quite in agreement with method need. In a nutshell, the hyphenation of Youden's test with quality by design approach ensured the development of a reliable chromatography method for routine estimation of daptomycin throughout its product lifecycle.

Quality by design with design of experiments approach for development of a stability‐indicating LC method for enzalutamide and its impurities in soft gel dosage formulation

“…However, there is no similar reference stability–indicating method for the corresponding dosage form testing. In a recent trend, the QbD (Ashok, Dongala, & Katakam, 2020; Katakam & Dongala, 2020a, 2020b; Katakam, Dongala, & Ettaboina, 2020; Panda, Bera, & Pradhan, 2019) approach was regulated for use in the pharmaceutical industry, with critical process parameters (CPPs) and critical quality attributes (CQAs) established for assessment of risk and design space for (method) operating conditions. A scientific way of explaining the design of experiments (DoE) approach involves performing a series of trails (usually 18) based on the fractional factorial design to evaluate the rapid and straightforward stability‐indicating UPLC method using ultraviolet detection prior to performing method validation studies.…”