PERFORMANCE TESTING OF SILICA MODIFIED WITH MYRISTIC AMIDE AND PALMITIC ESTER FOR HIGH PERFORMANCE LIQUID CHROMATOGRAPHY COLUMN

• Main Author: Putra Arrafi, Wisnu
• Format: Final Project
• Language: Indonesia
• Subjects: Kimia
• Online Access: https://digilib.itb.ac.id/gdl/view/75330
• Institution: Institut Teknologi Bandung

One of the components of a High Performance Liquid Chromatography (HPLC) column is the column filler particles. The most commonly used column particles are silica-based that have been modified with specific functional groups. C8 and C18 chromatography columns are standard commercial columns. Fatty acid-modified silica with a carbon chain length of C8–C18 is predicted to have equivalent performance to commercial C8 and C18 chromatography columns. This study has synthesized and tested the performance of silica modified with myristic amide and palmitic ester for HPLC column. Silica was prepared using tetraethylorthosilicate (TEOS) and N1-(3-trimethoxysilylpropyl)diethylenetriamine (N- TMSpen) precursors which were further modified with myristic acid and palmitic acid using N,N'-dicyclohexylcarbodiimide (DCC)/4-dimethylaminopyridine (DMAP) coupling reagents. According to the IR results for silica modified witth with myristic amide, the absorption band at wave number 1625 cm–1 was obtained as C=O amide absorption band. There are also absorption bands at 2927 cm–1 and 2850 cm–1 as C–H stretching vibrations on alkyl groups, C–N amide stretching vibrations at wave number 1400 cm–1, and Si–O–Si absorption band at wave number 1103 cm–1. IR results for silica modified with palmitic ester showed the presence of C=O ester stretching vibrations at wave number 1625 cm–1. There were also C–H alkyl absorption bands at wave numbers 2927 cm–1 and 2850 cm–1, respectively, and Si–O–Si vibrations at wave number 1089 cm–1. The silica modified with myristic amide column was successfully charged and was able to separate a mixture of 40 ppm paracetamol standard and 40 ppm caffeine standard with a resolution of 2.31 and a column selectivity of 13.68 under conditions of 20 µL injection volume, water eluent, 1.0 mL/min flow rate, Diode Array Detector (DAD) at a wavelength of 274 nm, and separation conditions applying gradient elution at a time of 1 min with a composition of water : methanol (80:20 v/v) and a fixed flow rate. The silica modified with palmitic ester column was successfully charged and was able to separate a mixture of 40 ppm paracetamol standard and 40 ppm caffeine standard with a resolution of 4.28 and column selectivity of 3.45 under conditions of 20 µL injection volume, water eluent, 1.0 mL/min flow rate, DAD detector at a wavelength of 274 nm, and isocratic elution separation conditions