PhD Scientific Days 2026

Pharmaceutical Sciences and Health Technologies 2.

Green Chiral HPLC Method Development for Pharmaceutical Analysis

Előadó neve

Mhammad, Ali, PhD

Neptune code

GFI24E

Előadó munkahelye

Department of Pharmaceutical Chemistry, Semmelweis University, Hőgyes E. u. 9, Budapest, 1092, Hungary

Előadó telefonszáma

+36707754866

Előadó e-mail címe

ali.mhammad@phd.semmelweis.hu

Az előadás címe

Green Chiral HPLC Method Development for Pharmaceutical Analysis

Szerző(k) neve és munkahelye

Ali mhammad¹, Gergely Dombi (Gyógyszeranalitika, HPLC)¹, Gergo Tóth¹

1: Department of Pharmaceutical Chemistry, Semmelweis University, Hőgyes E. u. 9, Budapest, 1092, Hungary

Bemutatás módja

Szóbeli

Szekció

Pharmaceutical Sciences and Health Technologies 2.

Language of the presentation

English

Preferred session

Pharmaceutical Sciences and Health Technologies

Összefoglaló szövege

Introduction
The imperative for sustainable analytical chemistry has catalyzed innovation in green chiral high-performance liquid chromatography (HPLC) for enantiopurity determination of pharmaceuticals. This study presents a comprehensive protocol for developing eco-efficient polar organic and reversed-phase methods using polysaccharide-based chiral stationary phases and environmentally benign eluents, including dimethyl carbonate (DMC), ethanol, and water.
Aims
To devise a tiered workflow—comprising method scouting, design-of-experiments (DoE) optimization (factors: mobile phase composition, flow rate 0.5–1.0 mL/min, temperature 20–40 °C, and organic modifier), and method validation—that systematically maximizes enantioresolution (Rs), column efficiency, and sensitivity for minor enantiomer quantification (LOQ ≤ 0.02% w/w).
Methods
Representative applications included crizotinib on Cellulose-3 with ethanol:water (9:1) and thalidomide on i-Amylose-3 with DMC. All developed methods underwent ICH Q2(R1) validation, with greenness assessed via AGREE, AGSA, and mechanistic analysis of mass transfer kinetics and structural domain interactions.
Results
Crizotinib achieved Rs = 6.3, excellent linearity (r² = 0.9997), precision (RSD = 1.4%), and accuracy (98.9–101.1%); thalidomide yielded Rs = 13.8. DMC-based methods outperformed conventional acetonitrile/methanol systems (AGREE 0.77 ± 0.02 vs 0.56; Δ = 37%) and 2-propanol-based methods (AGREE 0.57), with AGSA scores 84–86. Rigid, polyfunctional analytes preferentially benefited from DMC, enabling predictive CSP–analyte–eluent matching.
Conclusion
This framework reduces solvent consumption, energy demand, and hazardous waste generation, establishing a scalable benchmark for green chiral HPLC in pharmaceutical stereocontrol and regulatory compliance.
Funding
Supported by the 2025-2.1.1-EKÖP-2025-00014 University Research Scholarship Programme of the Ministry for Culture and Innovation from the Source of the National Research, Development and Innovation Fund (G.D.). This work was funded by the National Research, Development, and Innovation Office, Hungary (grant: NKFIH FK 146930 and by the János Bolyai Research Scholarship of the Hungarian Academy of Sciences (G.T).

University

Semmelweis University

Supervisor

Gergo Tóth

Publication of my abstract

I give consent to the publication of my abstract on the website of the congress.

phd.section.field

in doctoral studies before complex exam (PhD)

Kind

Szabad

Status

elfogadva

Accepted presentation method

szóbeli

Előadás fájl jóváhagyás

jóváhagyta

Előadó

8926

Start

10:15

End

10:25