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  • P-ISSN1225-0163
  • E-ISSN2288-8985
  • SCOPUS, ESCI, KCI

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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
https://doi.org/10.5806/ast.2024.37.4.220
Zahraa Hadi Shareef (Department of Chemistry, College of Science, University of Babylon)
Ahmed Ali Alkarimi (Department of Chemistry, College of Science, University of Babylon)

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-dimethoxy-2-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 ㎍·mL-1 with an r2 value of 0.999. The detection and quantification limits were 0.932 and 2.788 ㎍·mL-1, respectively. The molar absorptivity and Sandells sensitivity were 2.99138 × 106 L·mol-1·cm-1 and 103.1 × 10-3 ㎍·cm-2, respectively.

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

Graphical Abstract

AST-2024-001_R4_P_Graphical Abstract_001.jpg

Received
2024-02-03
Revised
2024-03-03
Accepted
2024-04-17
Published
2024-08-25
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Analytical Science and Technology