Preparation and Characterization of Glycidyl Polymethacrylate Monolith Column and its Application for Simultaneous Deter
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Preparation and Characterization of Glycidyl Polymethacrylate Monolith Column and Its Application for Simultaneous Determination of Paracetamol and Chlorzoxazone in Their Combined Pharmaceutical Formulations Mutaz E. Saliha, b, *, Ahmad Aqelc, Babiker Y. Abdulkhaira, d, Munir S. Obbedc, Zeid A. ALOthmanc, Yacine Badjah-Hadj-Ahmedc, and Mohamad A. Abdulaziza aChemistry
Department, College of Science, Sudan University for Science and Technology, Khartoum, 11111 Sudan of Chemistry-Hurrymilla, College of Science and Humanities, Shaqra University, Shaqra, 11962 Saudi Arabia c Department of Chemistry, College of Science, King Saud University, P.O. Box 2455, Riyadh, 11451 Saudi Arabia dChemistry Department, College of Science, Al-Imam Mohammad Ibn Saud Islamic University (IMSIU), Riyadh, 11432 Saudi Arabia *e-mail: [email protected] bDepartment
Received April 20, 2018; revised November 14, 2018; accepted May 21, 2020
Abstract—A home-made column (3.2 mm i.d., 100 mm length) was prepared in which glycidyl polymethacrylate was used. The optimum value of the initiator corresponded to 5 mg/mL. The column morphology was characterized by scanning electron microscopy. The permeability was evaluated using acetonitrile and water as a mobile phase and uracil as an unretained substrate. A simple and economical reversed-phase HPLC method has been developed for the simultaneous estimation of paracetamol and chlorzoxazone in their pharmaceutical formulations. Components were determined using a UV detector at 270 nm. The mobile phase was composed of 1% formic acid solution and acetonitrile (65/35, v/v); 0.7 mL/min flow rate and 5.0 μL injection volume were used. Peak resolution was 1.96. All findings allow concluding that the prepared stainless steel conventional HPLC column and the novel validated method are applicable for quality control and routine analysis. Keywords: liquid chromatography, monolith, glycidyl methacrylate, paracetamol, chlorzoxazone 10.1134/S1061934820110106
Monolithic columns use separation media composed of one large particle that has no inter-particular voids. Consequently, the mobile phase flows through the stationary phase. Such flow causes a great acceleration of the mass transfer rate. Unlike diffusion, the major cause for mass transfer within the pores of the particles of the stationary phase during chromatographic separation, enhancement of the separation speed takes place by convective flow [1]. Monolithic phases have higher external porosity arising from the structure of the network of macropores. The networks of meso and macropores twist around each other and provide the intricate structure of the monolithic medium. These two structural characteristics allow the combination of low hydraulic resistance of the column to the stream of the mobile phase (low backpressure) and provide the surface area needed for analyte retention. Since monoliths possess no interstitial void volume, all the mobile phase has to flow through the pore channels of the support. This results in enhancing the rate of mass transf
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