Abstract
A monolithic imprinted atenolol column was constructed by in situ polymerisation using a methacrylic acid monomer and a 1 : 1 (v/v) porogen of propanol: toluene with two template: monomer: crosslinker combinations, namely, MIP 1 (1 : 4 : 20) and MIP 2 (1 : 5 : 20). Physical characterisation of the monolithic columns consisted of permeability testing, Fourier transform infrared (FTIR) testing, surface area analysis (SAA), and scanning electron microscopy (SEM). The permeability value of four monolithic columns was in the good category: MIP 1 (24.01 mD), NIP 1 (56.43 mD), MIP 2 (23.03 mD), and NIP 2 (14.47 mD). The polymerisation process of these four monolithic imprinted columns was carried out perfectly, as shown by the absence of vinyl groups (1000 cm−1 and 900 cm−1) during FTIR testing. Based on SAA testing, the pores of the four polymers were classified as mesopores. The best monolithic column was MIP 1, as seen from the intercolumn and intracolumn reproducibility values and a % RSD <2.0%. The MIP 1 column was selective towards atenolol, as seen from the selectivity factor, imprinting factor (IF), and resolution (Rs) values. The IF values of MIP 1 were atenolol (204.62), metoprolol (3.36), and propranolol (1.27). The Rs value between atenolol and the analogue compounds was 7.23. The MIP 1 column can be used for the analysis of atenolol in blood serum samples with an average percentage recovery rate of 94.88 ± 4.43%.
Highlights
Beta blockers have become the first choice for hypertension treatment over the past four decades [1] to reduce blood pressure, heart rates, anxiety, and muscle tremors
E components used for the construction of imprinted monolithic columns are functional monomers, crosslinkers, porogens, and initiators. e functional monomer used in the present study was methacrylic acid (MAA), which is a universal monomer most often used for the manufacture of monolithic columns [18]
Materials. 3-(Trimethoxysilyl)-propyl methacrylate (MAPS) (Tokyo Chemical Industry), atenolol (Tokyo Chemical Industry), metoprolol tartrate hydrochloride (Tokyo Chemical Industry), propranolol hydrochloride (Tokyo Chemical Industry), acetic acid, phosphoric acid, hydrochloric acid (HCl), acetone (Merck), benzoyl peroxide (BPO), ethanol proanalysis, sodium hydroxide, pyridine, and propanol were from Merck
Summary
Beta blockers have become the first choice for hypertension treatment over the past four decades [1] to reduce blood pressure, heart rates, anxiety, and muscle tremors. Conventional HPLC still uses particle columns as stationary phases, which require large amounts of mobile phase. Monolithic columns can be constructed using molecularly imprinted polymer (MIP) technology to increase selectivity. E components used for the construction of imprinted monolithic columns are functional monomers, crosslinkers, porogens, and initiators. E functional monomer used in the present study was methacrylic acid (MAA), which is a universal monomer most often used for the manufacture of monolithic columns [18]. A research study about the monolithic column for beta blockers based on imprinted technology was only published by Zhang et al [22] for propranolol. An imprinted monolithic column was constructed using methacrylate acid (MAA) as a functional monomer and propanol as a porogen. Analytical performance for atenolol selectivity with respect to analogue compounds, reproducibility testing, and application of atenolol analysis in serum using HPLC was carried out
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