Graphene oxide-based stationary phase synthesis and separation of drug molecules for liquid chromatography (HPLC) analysis

Abstract

A new graphene oxide-based liquid chromatography stationary phase was synthesized, characterized, and used for the first time in the separation of paracetamol and caffeine in pharmaceutical preparations under reversed phase conditions. For this purpose, graphene oxide was synthesized using the modified Hummers method, and Si-GO stationary phase was obtained by immobilizing graphene oxide on aminopropyl silica. The obtained graphene oxide, Si–GO and aminopropyl silica materials were characterized by XRD, SEM, TEM and FTIR analysis. Different mobile phases were used to separate drug molecules in order to determine the mechanism of interaction between drug molecules and the stationary phase. Once the appropriate solvent system was determined, optimum chromatographic parameters such as mobile phase composition (methanol percentage in water), flow rate and column temperature were determined. The linearity of the method was in the range of 0.989–0.997. The maximum relative standard deviation (% RSD) value was calculated as 0.54. Mean recoveries for paracetamol and caffeine were 98%–99%, respectively, and LOD and LOQ were 6 × 10⁻³ to 6.5 × 10⁻³mg/L and 2 × 10⁻² to 2.2 × 10⁻²mg/L, respectively. The results showed that the new graphene oxide-based stationary phase could be used for the separation of paracetamol and caffeine in pharmaceutical preparations.

Keywords:

• Graphene oxide
• liquid chromatography
• stationary phase
• drug analysis
• validation

Acknowledgment

The authors wish to thank the principal of Konya Technical University and Scientific Research Projects Coordination.

Disclosure statement

The authors would like to certify that the work described has not been published previously and is not under consideration for publication elsewhere. Furthermore, authors have no actual or potential conflict of interest including any financial, personal, or other relationships with other people or organizations within three years of beginning the submitted work that could inappropriately influence, or be perceived to influence their work.

Additional information

Funding

This study, a part of M.Sc. work entitled “Development of Graphene Oxide-Based Liquid Chromatography (HPLC) Stationary Phases and Their Use in The Analysis of Pharmaceutical Molecules”, was supported by Konya Technical University, Coordinators of Scientific Research Projects with BAP 221022062 project numbers.