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1 2024

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A stationary phase of tetraethylene glycol-modified silica for separation of phenolic acids

Linda Roza, Mustika Wida Maya, Rafi Mohamad, Rohaeti Eti, Lim Lee Wah

Acta Chromatographica

2024

Vol. 36, no. 3

196--205

Silica, as a stationary phase, has low separation efficiency accompanied by overlapping, broadened, and tailed peaks, so it needs to be modified to improve its efficiency. This study aims to develop a silicabased stationary phase modified by tetraethylene glycol (TEG) to separate phenolic compounds. Silica was modified by a chemical bond between silanol groups on the silica surface and TEG through a 3-glycidyloxypropylmethoxysilane reaction. The modified silica was packed into a capillary column and used to separate simple phenolic compounds consisting of phenol, pyrocatechol, and pyrogallol. A sample of 0.2 μL was injected into the capillary liquid chromatography and the mobile phase employed was acetonitrile 98% with a flow rate of 3 μL min1. Elution was also done isocratically in this process and detection was carried out at a wavelength of 254 nm. The mixture of simple phenolic compounds was successfully separated in less than 7 min. The asymmetry factor and resolution were 1.43–2.12 and 1.72–5.43 respectively. The number of the theoretical plates ranged from 213 to 7,857. Columns containing Si-TEG stationary phase also separate phenolic compounds, which consist of gallic acid, syringic acid, ferulic acid, and caffeic acid. A sample of 0.2 μL was injected into the capillary liquid chromatography and successfully separated the mixture in less than 12 min. The samples were eluted isocratically using a mixture of methanol and 50mM phosphate buffer pH 2.5 (8:92) with a flow rate of 3 μL min1. The phenolic acids compounds were detected at a wavelength of 280 nm. The chromatogram showed four separate peaks. The asymmetry factor and resolution were 1.53–1.63 and 1.14–1.74, respectively, but the number of the theoretical plates was low, ranging from 190 to 796.