A Green and QbD-Optimized Rp-Hplc Method for Simultaneous Estimation of Linagliptin and Dapagliflozin

IF 1.7 4区化学 Q4 CHEMISTRY, PHYSICAL

International Journal of Chemical Kinetics Pub Date : 2026-03-25 Epub Date: 2026-01-27 DOI:10.1002/kin.70032

Sourabh Satapathy, Kuladip barman, Shivam Kumar, Neha Singh, Balak Das Kurmi, Preeti Patel

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引用次数: 0

Abstract

The present study focuses on the development and optimization of a robust reversed-phase high-performance liquid chromatography (RP-HPLC) method for the simultaneous estimation of linagliptin and dapagliflozin in bulk and tablet dosage forms. A Quality by Design (QbD) approach was employed using the Box-Behnken design to systematically optimize critical chromatographic parameters, ensuring efficient separation with high sensitivity and reproducibility. The optimized conditions utilized a mobile phase of methanol: acetonitrile: buffer: triethylamine (80:10:10:0.1 v/v/v/v), with a pH adjusted to 5.0 using orthophosphoric acid and a flow rate of 1.0 mL/min. The method demonstrated excellent linearity (r² > 0.998), precision (%RSD < 2), and accuracy (98.9%–100.5%), complying with ICH guidelines. Additionally, a greenness evaluation was conducted using the AGREE analytical greenness metric tool, giving a score of 0.68, indicating an environmentally sustainable analytical approach. The developed method is rapid, reliable, and suitable for routine quality control analysis of linagliptin and dapagliflozin in pharmaceutical formulations.

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绿色qbd优化反相高效液相色谱法同时测定利格列汀和达格列净的含量

本研究的重点是建立和优化一种反相高效液相色谱（RP-HPLC）同时测定利格列汀和达格列净散装和片剂剂型的方法。采用Box-Behnken设计，采用设计质量法（Quality by Design, QbD）系统优化关键色谱参数，确保高效分离、高灵敏度和高重现性。优化条件为流动相：甲醇：乙腈：缓冲液：三乙胺（80:10:10:0.1 v/v/v/v /v），正磷酸调节pH为5.0，流速为1.0 mL/min。该方法线性良好（r2 > 0.998），精密度（%RSD < 2），准确度（98.9% ~ 100.5%），符合ICH指南。此外，使用AGREE分析绿色度量工具进行了绿色评估，得分为0.68，表明环境可持续的分析方法。该方法快速、可靠，适用于利格列汀和达格列净制剂的常规质量控制分析。

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来源期刊

International Journal of Chemical Kinetics 化学-物理化学

CiteScore

3.30

自引率

6.70%

发文量

审稿时长

3 months

期刊介绍： As the leading archival journal devoted exclusively to chemical kinetics, the International Journal of Chemical Kinetics publishes original research in gas phase, condensed phase, and polymer reaction kinetics, as well as biochemical and surface kinetics. The Journal seeks to be the primary archive for careful experimental measurements of reaction kinetics, in both simple and complex systems. The Journal also presents new developments in applied theoretical kinetics and publishes large kinetic models, and the algorithms and estimates used in these models. These include methods for handling the large reaction networks important in biochemistry, catalysis, and free radical chemistry. In addition, the Journal explores such topics as the quantitative relationships between molecular structure and chemical reactivity, organic/inorganic chemistry and reaction mechanisms, and the reactive chemistry at interfaces.