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Background <p>In the present study, a new and sensitive UPLC method for stability-indicating study has been established and validated as per the ICH guidelines. To date, no work has been reported on the forced degradation studies of alpelisib using the UPLC technique. Box–Behnken design was used to study the response surface for method optimisation to achieve a good separation with a minimum number of experimental trials. Three independent parameters selected were mobile phase ratio, flow rate of the mobile phase and temperature of the column. Retention time and tailing factor were taken as two responses to obtain mathematical models.</p> Results <p>The chromatography was executed using Waters BEH C<sub>18</sub> UPLC column (2.1 × 50&#xa0;mm, 1.7micron) at wavelength detection of 246&#xa0;nm. The optimised assay conditions predicted were isocratic mobile solvent system using 0.1% formic acid buffer solution and acetonitrile in the ratio of 50:50 (V/V), with a flow rate of 0.25&#xa0;mL per min and injection volume of 4&#xa0;µL. The method has shown a good response with a total run time of 4&#xa0;min, retention time was found to be 1.49&#xa0;min and tailing factor was 0.99 for alpelisib, showing good peak symmetry. The linearity of the method developed is at a range of 10–50&#xa0;µg/mL with R<sup>2</sup> 0.9955, while the percentage mean recovery for accuracy was of 99.25%. The method developed was precise as % RSD of inter-day and intra-day precision was 0.3 and 0.1, respectively, meeting the specified limits.</p> Conclusion <p>The developed UPLC work is quick and simple with an&#xa0;increased&#xa0;level&#xa0;of&#xa0;linearity, precision, specificity and accuracy as per the ICH criteria and can find application in industries as a regular method for quantification of alpelisib.</p>

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Stability-indicating UPLC method for quantification of alpelisib in bulk and tablet formulation by QbD approach

  • 期刊论文

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  • 发表日期：

    2025年4月28日

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  • Tandrima Majumder,
  • Shiva Kumar Gubbiyappa,
  • Padmini Iriventi

摘要

Background

In the present study, a new and sensitive UPLC method for stability-indicating study has been established and validated as per the ICH guidelines. To date, no work has been reported on the forced degradation studies of alpelisib using the UPLC technique. Box–Behnken design was used to study the response surface for method optimisation to achieve a good separation with a minimum number of experimental trials. Three independent parameters selected were mobile phase ratio, flow rate of the mobile phase and temperature of the column. Retention time and tailing factor were taken as two responses to obtain mathematical models.

Results

The chromatography was executed using Waters BEH C18 UPLC column (2.1 × 50 mm, 1.7micron) at wavelength detection of 246 nm. The optimised assay conditions predicted were isocratic mobile solvent system using 0.1% formic acid buffer solution and acetonitrile in the ratio of 50:50 (V/V), with a flow rate of 0.25 mL per min and injection volume of 4 µL. The method has shown a good response with a total run time of 4 min, retention time was found to be 1.49 min and tailing factor was 0.99 for alpelisib, showing good peak symmetry. The linearity of the method developed is at a range of 10–50 µg/mL with R2 0.9955, while the percentage mean recovery for accuracy was of 99.25%. The method developed was precise as % RSD of inter-day and intra-day precision was 0.3 and 0.1, respectively, meeting the specified limits.

Conclusion

The developed UPLC work is quick and simple with an increased level of linearity, precision, specificity and accuracy as per the ICH criteria and can find application in industries as a regular method for quantification of alpelisib.