Abstract
A stable and porous amino-functionalized zirconium-based metal organic framework (Zr-MOF-NH2) containing missing linker defects was prepared and fully characterized by FTIR, scanning electron microscopy, powder X-ray diffraction, and BET surface area measurement. The Zr-MOF-NH2 was then applied as an adsorbent in pipette-tip solid phase extraction (PT-SPE) of carbamazepine. Important parameters affecting extraction efficiency such as pH, sample volume, type and volume of eluent, amount of adsorbent, and number of aspirating/dispensing cycles for sample solution and eluent solvent were investigated and optimized. The best extraction efficiency was obtained when pH of 100 µL of sample solution was adjusted to 7.5 and 5 mg of the sorbent was used. Eluent solvent was 10 µL methanol. Linear dynamic range was found to be between 0.1 and 50 µg L−1 and limit of detection for 10 measurement of blank solution was 0.05 µg L−1. This extraction method was coupled to HPLC and was successfully employed for the determination of carbamazepine in urine and water samples. The strategy combined the advantages of fast and easy operation of PT-SPE with robustness and large adsorption capacity of Zr-MOF-NH2.
Highlights
Carbamazepine (CBZ, 5H-dibenzo [b,f ] azepine-5-carboxamide) often used as anticonvulsant drug for treatment of epilepsy [1, 2]
The peak at 1654 cm−1 is assigned to DMF, while the intense doublet at 1572 and 1386 cm−1 are assigned to the asymmetrical and symmetrical stretching modes of the carboxylate groups
The observed peaks between 1400 and 1500 cm−1 are ascribed to the C=C in aromatic compound of the organic linker
Summary
Carbamazepine (CBZ, 5H-dibenzo [b,f ] azepine-5-carboxamide) often used as anticonvulsant drug for treatment of epilepsy [1, 2]. Whenever a patient consumes CBZ, about 2–3% of this drug will excrete unchanged through his urine and enters into environmental aquatic ecosystems [3]. Biodegradation of CBZ is very difficult in environmental media owing to its low solubility and stability in water. SPE is a prevalent procedure for pre-treatment of various pharmaceutical analytes due to its reproducibility, high recovery and simple operation. Miniaturized SPE has been developed to overcome on the problems raised by conventional SPE processes such as matrix effect, low detection limit, losses of analytes, and environmental problems due to consumption of large amounts of organic solvents
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