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Background <p>Alogliptin is a selective dipeptidyl peptidase-4 (DPP-4) inhibitor used to treat type 2 diabetes mellitus. Accurate measurement of alogliptin in plasma is crucial for analytical and research purposes, especially in labs without access to LC-MS/MS systems.</p> Objective <p>To develop and validate a cost-effective, DoE-optimised RP-HPLC method for quantifying alogliptin in human plasma using a simple protein-precipitation extraction approach.</p> Methods <p>Plasma samples were processed by protein precipitation with acetonitrile and analysed on a C18 column using an isocratic mobile phase of acetonitrile and 0.1% formic acid (20:80 v/v) at 0.7 mL/min. Detection was performed at 224&#xa0;nm. The method was validated in accordance with ICH M10 guidelines for selectivity, linearity, accuracy, precision, recovery, sensitivity, and robustness. Method parameters were optimised using a two-factor DoE model based on mobile phase composition and flow rate.</p> Results <p>The method demonstrated excellent linearity over the range of 2–10&#xa0;µg/mL (r² = 0.9998). Recovery values remained high and consistent (99.7–101.8%) with %CV &lt; 0.5%. Precision results at LQC, MQC, and HQC levels showed intra- and inter-day variation within accepted limits (%CV ≤ 15%). The validated LOQ was 0.2297&#xa0;µg/mL, sufficient for detecting alogliptin within the established calibration range, although not as sensitive as LC-MS/MS methods reported in the literature. Robustness testing confirmed that small variations in chromatographic conditions did not affect method performance.</p> Conclusion <p>This work presents a practical and cost-effective RP-HPLC method optimised through a DoE approach for the quantification of alogliptin in human plasma. While less sensitive than the LC-MS/MS technique, the method offers reliable performance, simple sample preparation and good reproducibility, making it suitable for routine analytical use in laboratories where advanced instrumentation is not available.</p>

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Development and Validation of a Cost-Effective, DoE-Optimized RP-HPLC Method for the Quantification of Alogliptin in Human Plasma

  • 期刊论文

  • 发表日期：

    2026年2月20日

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  • Kajal S. Bansode,
  • Paresh R. Mahaparale,
  • Pratiksha R. Rajguru,
  • Kiran K. Mali

摘要

Background

Alogliptin is a selective dipeptidyl peptidase-4 (DPP-4) inhibitor used to treat type 2 diabetes mellitus. Accurate measurement of alogliptin in plasma is crucial for analytical and research purposes, especially in labs without access to LC-MS/MS systems.

Objective

To develop and validate a cost-effective, DoE-optimised RP-HPLC method for quantifying alogliptin in human plasma using a simple protein-precipitation extraction approach.

Methods

Plasma samples were processed by protein precipitation with acetonitrile and analysed on a C18 column using an isocratic mobile phase of acetonitrile and 0.1% formic acid (20:80 v/v) at 0.7 mL/min. Detection was performed at 224 nm. The method was validated in accordance with ICH M10 guidelines for selectivity, linearity, accuracy, precision, recovery, sensitivity, and robustness. Method parameters were optimised using a two-factor DoE model based on mobile phase composition and flow rate.

Results

The method demonstrated excellent linearity over the range of 2–10 µg/mL (r² = 0.9998). Recovery values remained high and consistent (99.7–101.8%) with %CV < 0.5%. Precision results at LQC, MQC, and HQC levels showed intra- and inter-day variation within accepted limits (%CV ≤ 15%). The validated LOQ was 0.2297 µg/mL, sufficient for detecting alogliptin within the established calibration range, although not as sensitive as LC-MS/MS methods reported in the literature. Robustness testing confirmed that small variations in chromatographic conditions did not affect method performance.

Conclusion

This work presents a practical and cost-effective RP-HPLC method optimised through a DoE approach for the quantification of alogliptin in human plasma. While less sensitive than the LC-MS/MS technique, the method offers reliable performance, simple sample preparation and good reproducibility, making it suitable for routine analytical use in laboratories where advanced instrumentation is not available.