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  • P-ISSN 1225-0163
  • E-ISSN 2288-8985

Estimation for warfarin in pharmaceutical preparation using monolithic column

Analytical Science and Technology / Analytical Science and Technology, (P)1225-0163; (E)2288-8985
2024, v.37 no.4, pp.220-229
Zahraa Hadi Shareef (Department of Chemistry, College of Science, University of Babylon, Iraq)
Ahmed Ali Alkarimi (Department of Chemistry, College of Science, University of Babylon, Iraq)
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Abstract

This study aims to developing a method for estimating pharmaceutical compounds within a monolith column using high-performance liquid chromatography (HPLC). The monolithic column was prepared using copolymerization of glycidyl methacrylate, co-ethylene dimethacrylate, and co-acrylic acid inside a borosilicate tube of specific dimensions a 60 mm borosilicate tube length with 1.5 mm and 3.5 mm inner and outer diameters, respectively. A UV Ultra violet source with a wavelength of 365 nm was used, and the polymerization process involved mixing glycidyl methacrylate, acrylic acid, ethylene dimethacrylate as a binder, and 2,2-dimethoxy2-phenyl acetate phenone as an initiator in suitable solvents consisting of ethanol and 1-hexanol. The polymerization process formed the monolith column after 4 minutes, and subsequently, the epoxy groups were altered to diol groups using 0.2 M hydrochloric acid HCl, which were pumped through the column for 3 hours at a flow rate of 10 µL·min−1 . Various techniques, such as Scanning Electron Microscope SEM, Brunauer-Emmett-Teller BET, Fourier-transform infrared spectroscopy FT-IR and HNMR, were utilized to characterize and confirm the structure of the monolith. The prepared monolith was employed to estimate and identify the pharmaceutical compound of warfarin using high-performance liquid chromatography HPLC. The analytical curve of warfarin was linear in the range of 3 to 100 µg·mL−1 with an r2 value of 0.999. The detection and quantification limits were 0.932 and 2.788 µg·mL−1 , respectively. The molar absorptivity and Sandells sensitivity were 2.99138 × 106 L·mol−1 ·cm−1 and 103. 1 × 10−3 µg·cm−2 , respectively

keywords
monolith, HPLC, glycidyl methacrylate, warfarin, acrylic acid


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