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Objective <p>The objective was to create AQbD approach novel green stability-indicating RP-HPLC method that can measure Evogliptin tartrate (EVO) and Metformin HCl (MET) in their combined dosage form dosage form at the same time and greenness assessment of method by using AGREE and GAPI matrices.</p> Materials and Methods <p>Initial screening experiments, combined with a structured risk assessment, were conducted to identify the critical method attributes (CMAs), specifically the proportion of organic modifier, buffer pH, and flow rate, all of which impact the critical quality attributes (CQAs). A Box-Behnken design was employed within the response surface methodology framework to evaluate the three-level interactions of these parameters. The effects on 5 key response factors—Retention Time of EVO (R1), Retention Time of MET (R2), Tailing Factor of EVO (R3), Tailing factor of MET (R4) and Resolution (R5) were analyzed in detail. The suggested approach was created utilizing an Eclipse C18 column, a mobile phase consisting of 5-mM 1-hexane sulphonic acid sodium salt in water, and 0.2% v/v TEA: Methanol with pH 3.0 adjusted with orthophosphoric acid (OPA). The study investigated at the forced degradation of pharmaceuticals under different stress settings. Using a PDA detector, the degradant products and both drugs demonstrated high peak resolution at 254.4&#xa0;nm.&#xa0;AGREE and GAPI software’s were used for greenness assessment of method.</p> Results <p>With r2 values &gt; 0.999, which demonstrate a strong linear relationship between concentration and peak area, this approach demonstrated good linearity for the concentration range used: 1–5&#xa0;µg/mL for Evogliptin tartrate and 100–500&#xa0;µg/mL for Metformin HCl. Since the recovery percentage falls between 99 and 100%, it was shown to be accurate without interfering. Measurements of intra-day and inter-day precision showed that the medicines' RSD was less than 2%. For Evogliptin tartrate, the LOD and LOQ were 0.047&#xa0;µg/mL and 0.143&#xa0;µg/mL, while for Metformin HCl, they were 5.81&#xa0;µg/mL and 17.61&#xa0;µg/mL. The technique's capacity to identify stability for both medications was confirmed when it was able to distinguish the degradation products. The developed RP-HPLC method has an AGREE score of 0.63 and In GAPI pictogram showing only three red zones which corresponding to Physico-chemical properties, non- greener solvent used and no waste treatment.</p> Conclusion <p>The proposed method effectively optimized by using BBD. After being evaluated by ICH requirements, the proposed method was determined to be robust, straightforward, specific, precise, and accurate. It will be appropriate for regular quality control and stability studies, guaranteeing the product's ongoing safety and effectiveness. The developed method was evaluated using AGREE and GAPI tools and both of which showed excellent green characteristics.</p>

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AQbD-Optimized Green Stability-indicating RP-HPLC Method for Simultaneous Estimation of Evogliptin Tartrate and Metformin HCl

  • 期刊论文

  • 发表日期：

    2025年11月17日

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  • Mochi Nehaben Sudhirkumar,
  • Rajesh Kanubhai Patel

摘要

Objective

The objective was to create AQbD approach novel green stability-indicating RP-HPLC method that can measure Evogliptin tartrate (EVO) and Metformin HCl (MET) in their combined dosage form dosage form at the same time and greenness assessment of method by using AGREE and GAPI matrices.

Materials and Methods

Initial screening experiments, combined with a structured risk assessment, were conducted to identify the critical method attributes (CMAs), specifically the proportion of organic modifier, buffer pH, and flow rate, all of which impact the critical quality attributes (CQAs). A Box-Behnken design was employed within the response surface methodology framework to evaluate the three-level interactions of these parameters. The effects on 5 key response factors—Retention Time of EVO (R1), Retention Time of MET (R2), Tailing Factor of EVO (R3), Tailing factor of MET (R4) and Resolution (R5) were analyzed in detail. The suggested approach was created utilizing an Eclipse C18 column, a mobile phase consisting of 5-mM 1-hexane sulphonic acid sodium salt in water, and 0.2% v/v TEA: Methanol with pH 3.0 adjusted with orthophosphoric acid (OPA). The study investigated at the forced degradation of pharmaceuticals under different stress settings. Using a PDA detector, the degradant products and both drugs demonstrated high peak resolution at 254.4 nm. AGREE and GAPI software’s were used for greenness assessment of method.

Results

With r2 values > 0.999, which demonstrate a strong linear relationship between concentration and peak area, this approach demonstrated good linearity for the concentration range used: 1–5 µg/mL for Evogliptin tartrate and 100–500 µg/mL for Metformin HCl. Since the recovery percentage falls between 99 and 100%, it was shown to be accurate without interfering. Measurements of intra-day and inter-day precision showed that the medicines' RSD was less than 2%. For Evogliptin tartrate, the LOD and LOQ were 0.047 µg/mL and 0.143 µg/mL, while for Metformin HCl, they were 5.81 µg/mL and 17.61 µg/mL. The technique's capacity to identify stability for both medications was confirmed when it was able to distinguish the degradation products. The developed RP-HPLC method has an AGREE score of 0.63 and In GAPI pictogram showing only three red zones which corresponding to Physico-chemical properties, non- greener solvent used and no waste treatment.

Conclusion

The proposed method effectively optimized by using BBD. After being evaluated by ICH requirements, the proposed method was determined to be robust, straightforward, specific, precise, and accurate. It will be appropriate for regular quality control and stability studies, guaranteeing the product's ongoing safety and effectiveness. The developed method was evaluated using AGREE and GAPI tools and both of which showed excellent green characteristics.