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<p>Reported analytical methods for dasatinib often exhibit limited sensitivity, prolonged run times, high solvent consumption, and inadequate adherence to green analytical chemistry principles, thereby restricting their applicability to nanoformulations and biological matrices. To address these limitations, a robust and environmentally sustainable reverse-phase ultra-performance liquid chromatography (RP-UPLC) method was developed using a systematic Quality by Design (QbD) framework. Critical analytical attributes were identified using an Ishikawa cause–effect diagram and prioritized through Risk Priority Number (RPN) assessment. Method screening was conducted using a Taguchi Orthogonal Array (Taguchi OA), followed by optimization with a Box–Behnken Design (BBD). Chromatographic separation was achieved on a Phenomenex Kinetex<sup>®</sup> C18 analytical column (50 × 2.1&#xa0;mm, 1.7&#xa0;μm) using methanol and 0.1% formic acid (65:35, v/v) at a flow rate of 1.0 mL/min and 30&#xa0;°C. Validation was performed in accordance with International Council for Harmonisation (ICH) guidelines. The optimized method demonstrated excellent linearity over 2–10&#xa0;µg/mL (r² = 0.999), with limit of detection (LOD) and limit of quantification (LOQ) values of 0.1696 and 0.5141&#xa0;µg/mL, respectively. High precision <b>(</b>percentage relative standard deviation [%RSD] &lt; 2%<b>)</b> and satisfactory recovery (97.87–99.17%) were achieved in nanosuspensions, plasma, and urine samples. Forced degradation studies confirmed its stability-indicating nature, while greenness and operational efficiency were supported by Complementary Green Analytical Procedure Index (ComplexGAPI), Analytical GREEnness Metric Approach (AGREE), AGREE for sample preparation (AGREEprep), Analytical Eco-Scale, Blue Applicability Grade Index (BAGI) and Lean Six Sigma assessments. Overall, the method is rapid, sensitive, eco-efficient, and suitable for routine pharmaceutical and bioanalytical applications.</p>

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Quality by Design-Driven Green RP-UPLC Method for Quantification of Dasatinib in Nanosuspensions and Biological Matrices

  • 期刊论文

  • 发表日期：

    2026年6月15日

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  • Adarsh C. Umarani,
  • Veerkumar P. Japti,
  • Rahul Koli,
  • Atith Muppayyanamath,
  • Priya P. Shetti

摘要

Reported analytical methods for dasatinib often exhibit limited sensitivity, prolonged run times, high solvent consumption, and inadequate adherence to green analytical chemistry principles, thereby restricting their applicability to nanoformulations and biological matrices. To address these limitations, a robust and environmentally sustainable reverse-phase ultra-performance liquid chromatography (RP-UPLC) method was developed using a systematic Quality by Design (QbD) framework. Critical analytical attributes were identified using an Ishikawa cause–effect diagram and prioritized through Risk Priority Number (RPN) assessment. Method screening was conducted using a Taguchi Orthogonal Array (Taguchi OA), followed by optimization with a Box–Behnken Design (BBD). Chromatographic separation was achieved on a Phenomenex Kinetex® C18 analytical column (50 × 2.1 mm, 1.7 μm) using methanol and 0.1% formic acid (65:35, v/v) at a flow rate of 1.0 mL/min and 30 °C. Validation was performed in accordance with International Council for Harmonisation (ICH) guidelines. The optimized method demonstrated excellent linearity over 2–10 µg/mL (r² = 0.999), with limit of detection (LOD) and limit of quantification (LOQ) values of 0.1696 and 0.5141 µg/mL, respectively. High precision (percentage relative standard deviation [%RSD] < 2%) and satisfactory recovery (97.87–99.17%) were achieved in nanosuspensions, plasma, and urine samples. Forced degradation studies confirmed its stability-indicating nature, while greenness and operational efficiency were supported by Complementary Green Analytical Procedure Index (ComplexGAPI), Analytical GREEnness Metric Approach (AGREE), AGREE for sample preparation (AGREEprep), Analytical Eco-Scale, Blue Applicability Grade Index (BAGI) and Lean Six Sigma assessments. Overall, the method is rapid, sensitive, eco-efficient, and suitable for routine pharmaceutical and bioanalytical applications.