Green Chromatographic Method for Determination of Active Pharmaceutical Ingredient, Preservative, and Antioxidant in an Injectable Formulation: Robustness by Design Expert

Abstract

We report an efficient HPLC method for simultaneous qualitative and quantitative analysis of lincosamide antibiotic injectable formulations containing Clindamycin phosphate (CMN), benzyl alcohol (BA), and ethylenediaminetetraacetic acid (EDTA) as major ingredients. The three components were separated by Phenomenex prodigy C8 (250 mm × 4.6 mm, 5 μm) HPLC column, flow rate 1.1 mL/min, injection volume 30 μL, and column temperature 35 °C, using 0.05 M sodium acetate buffer (pH 4.5) with acetonitrile (ACN) in the ratio of 80:20 (v/v). The detection wavelength was set as 240 nm. The method was validated as per International Conference on Harmonization (ICH) guidelines and was confirmed to be specific, precise, accurate, and linear. Method robustness was executed by utilizing quality in the design of the experiment. Accuracy results were found to be 99.3–100.5% for CMN, 99.3–100.8% for BA, and 99.1–100.3% for EDTA. Precision results were obtained as % relative standard deviation (RSD): 0.6% for CMN, 0.4% for BA, and 0.4% for EDTA. Correlation coefficient ( r 2 ) values were obtained as >0.999 for the three components. Analytical solutions are stable for 48 h at benchtop and refrigerator conditions. The greenness of the analytical method was evaluated by the Green Analytical Procedure Index (GAPI), National Environmental Method Index (NEMI), analytical eco-scale, and Analytical Greenness (AGREE) tools to confirm that the method is eco-friendly.

Engineering an efficient whole‐cell catalyst for d‐allulose production from glycerol

“…All RSM experimental design and statistical analysis were performed using Design-Expert 8.0.6 software (Stat-Ease, Inc., Minneapolis, MI). [39] 3 RESULTS AND DISCUSSION…”

QbD‐based stability‐indicating liquid chromatography (RP‐HPLC) method for the determination of flurbiprofen in cataplasm

“…The quality by design (QbD) concept is newly, officially introduced by regulatory bodies and the International Conference on Harmonization (ICH) (Dandabattina et al, 2022; ICH, Q14, 2022; Reddy Saddala et al, 2022). The current proposed research considered the guidelines and suggestions from the regulatory bodies and utilized the QbD design of experiments (DoE) approach to study the method robustness (Katakam et al, 2021; Konduru, Gundla, et al, 2022; Konduru, Kowtharapu, & Gundla, 2022; Kowtharapu, Katari, Sandoval, Muchakayala, et al, 2022; Kowtharapu, Katari, Sandoval, Rekulapally, et al, 2022; Kowtharapu, Katari, Surekha, et al, 2022; Muchakayala et al, 2021; Subramanian et al, 2020, 2021).…”

Determination and quantification of related substances and degradation products in bictegravir by full factorial design evaluated HPLC and mass spectrometry

“…Hence, LC-MS methods have also been developed to identify and predict other unknown impurities, such as major degraded analytes in the product. Furthermore, to evaluate viable and robust method conditions such as buffer concentration, ow rate, column oven temperature [8][9][10][11][12][13][14][15][16] and chromatographic conditions with the requirement of current regulatory guidelines, multivariate Design of Experiments (DoEs) has been introduced in this study.…”