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Purpose <p>This study aimed to develop and validate a robust, stability-indicating, and environmentally sustainable RP-HPLC method for quantifying silibinin in electrospun nanofibrous scaffolds using an Analytical Quality by Design (AQbD) approach.</p> Methods <p>An Analytical Target Profile (ATP) was defined to ensure reliable quantification of silibinin in complex matrices. Critical Method Attributes (CMAs), including retention time, tailing factor, and theoretical plates, were selected, while Critical Method Parameters (CMPs), such as methanol composition and flow rate, were optimized using Central Composite Design (CCD). Chromatographic separation was achieved on a Phenomenex Luna C18 column with a mobile phase of methanol: 0.1% formic acid (95:5, v/v) at a flow rate of 0.9&#xa0;mL/min, and detection at 288&#xa0;nm. Method validation was performed in accordance with International Council for Harmonisation Q2(R1) guidelines. The Method Operable Design Region (MODR) was established using response surface analysis. Environmental sustainability was assessed using AGREE, Complex GAPI, and BAGI tools.</p> Results <p>The method showed excellent linearity (R<sup>2</sup> = 0.999) over 100–500&#xa0;µg/mL. The limits of detection and quantification were 13.34&#xa0;µg/mL and 40.44&#xa0;µg/mL, respectively. Precision (%RSD &lt; 2%) and accuracy (99.51–100.16%) met ICH acceptance criteria. Forced degradation studies confirmed the method’s stability-indicating capability with no interference from degradation products. The MODR ensured robust performance within the design space. Greenness evaluation demonstrated high environmental compatibility (AGREE score 0.79; BAGI score 75).</p> Conclusion <p>The developed AQbD-based RP-HPLC method is rapid, reliable, and eco-friendly, making it suitable for routine quality control and advanced drug delivery applications.</p> Graphical abstract <p></p>

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Development and validation of a quality by design assisted green stability indicating RP- HPLC UV method for quantification of silibinin in nanofibrous scaffolds

  • 期刊论文

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  • 发表日期：

    2026年7月21日

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  • Melvin Vincent Dsouza,
  • Suneel Dodamani,
  • Bhaskar Kurangi,
  • Priya Shetti,
  • Shalaka Gaonkar,
  • Rahul Koli,
  • Vijay Kumbar

摘要

Purpose

This study aimed to develop and validate a robust, stability-indicating, and environmentally sustainable RP-HPLC method for quantifying silibinin in electrospun nanofibrous scaffolds using an Analytical Quality by Design (AQbD) approach.

Methods

An Analytical Target Profile (ATP) was defined to ensure reliable quantification of silibinin in complex matrices. Critical Method Attributes (CMAs), including retention time, tailing factor, and theoretical plates, were selected, while Critical Method Parameters (CMPs), such as methanol composition and flow rate, were optimized using Central Composite Design (CCD). Chromatographic separation was achieved on a Phenomenex Luna C18 column with a mobile phase of methanol: 0.1% formic acid (95:5, v/v) at a flow rate of 0.9 mL/min, and detection at 288 nm. Method validation was performed in accordance with International Council for Harmonisation Q2(R1) guidelines. The Method Operable Design Region (MODR) was established using response surface analysis. Environmental sustainability was assessed using AGREE, Complex GAPI, and BAGI tools.

Results

The method showed excellent linearity (R2 = 0.999) over 100–500 µg/mL. The limits of detection and quantification were 13.34 µg/mL and 40.44 µg/mL, respectively. Precision (%RSD < 2%) and accuracy (99.51–100.16%) met ICH acceptance criteria. Forced degradation studies confirmed the method’s stability-indicating capability with no interference from degradation products. The MODR ensured robust performance within the design space. Greenness evaluation demonstrated high environmental compatibility (AGREE score 0.79; BAGI score 75).

Conclusion

The developed AQbD-based RP-HPLC method is rapid, reliable, and eco-friendly, making it suitable for routine quality control and advanced drug delivery applications.

Graphical abstract