SYNTHESIS OF PHENYL MODIFIED SILICA AND ITS APPLICATION AS A LIQUID CHROMATOGRAPHIC COLUMN

• Main Author: Lifia Yulianti, Fifi
• Format: Final Project
• Language: Indonesia
• Subjects: Kimia
• Online Access: https://digilib.itb.ac.id/gdl/view/65028
• Institution: Institut Teknologi Bandung

High Performance Liquid Chromatography (HPLC) is one type of chromatography that is widely applied in the pharmaceutical industry. One of the applications is for simultaneous determination of paracetamol and caffeine in drugs. In pharmaceutical formulations, paracetamol can be found alone or combined with other substances such as caffeine. Therefore, analysis is needed to ensure that the drug has appropriate content. One analytical method that can be used for simultaneous analysis of paracetamol and caffeine is HPLC with phenyl-modified silica column. The phenyl group was chosen because it can interact ?-? with double bond electrons in the analyte. This study, successfully synthesis a phenyl modified silica using phenyltriethoxysilane (PTES) and tetraethylorthosilicate (TEOS) as precursors, isopropanol as a solvent, water as a hydrolyzing agent, and ammonia as a catalyst. Characterization of modified silica particles was carried out by Scanning Electron Microscope (SEM) and Fourier Transform Infrared (FTIR) spectroscopy. Based on FTIR data, silica particles have been successfully synthesized and obtained new peaks such as Si-O-Si and Si-O peaks in siloxane (1087 cm-1, 808 cm-1, and 478 cm-1) and O-H peak (3373 cm-1). Then, silica has also been successfully modified by phenyl group from a new peak at the aromatic C=C peak (1440 cm-1) and aromatic C-H peak (945 cm-1). Based on SEM measurements, silica and phenyl-modified silica have a spherical shape with a size of about 3-5 ????m, so that it can be packed in 4,6 x 150 mm column using GALAK GLK2000 for HPLC. A mixture of methanol and water (30:70, v/v) as mobile phase, under isocratic elution mode with a flow rate of 1 mL/min, and ultraviolet (UV) detection at 280 nm gave the best measurement results. This method shows good linearity with coefficient correlation of paracetamol and caffeine are 0,9987 on concentration 2-100 ppm and 0,9996 on concentration 1-100 ppm, respectively. Relative standard deviation (RSD) values for paracetamol and caffeine respectively are 1,05% and 1,53% for standard 100 ppm and 3,25% and 2,70% for standard 2 ppm. Quantitative analysis of drug showed that the method used haved good accuracy for analysis of paracetamol and caffeine with % recovery 90-110% for both analytes.