ABSTRACT
This work offers preparation of surfactant-modified amorphous carbon and its application in dispersive solid phase extraction of metronidazole and clarithromycin from plasma samples. The extraction procedure was combined with dispersive liquid-liquid microextraction for further preconcentration of the analytes for sensitive determination of the analytes followed by high performance liquid chromatography-diode array detector. In this work, first, the sorbent was added to the sample and the mixture vortexed to adsorb the analytes. Then, the obtained supernatant after centrifuging is discarded and the loaded analytes onto the sorbent surface were eluted with a water-miscible organic solvent. In the following, to further enrichment of the analytes the microextraction step was done. For this purpose, the eluate is taken, mixed with a water-immiscible organic solvent, and injected into deionized water. After centrifuging, an aliquat of the sedimented phase is taken and injected into the analytical instrument for the quantitative analysis. Under the optimum extraction conditions, high extraction recoveries (79 and 89% for metronidazole and clarithromycin, respectively), low limits of detection (2.1 and 1.9 ng mL-1 for metronidazole and clarithromycin, respectively) and quantification (7.0 and 6.3 ng mL-1 for metronidazole and clarithromycin, respectively), good repeatability (relative standard deviations less than 4.3% for intra- and 6.3% inter-day precisions), and wide linear ranges (7.3-1000 and 6.3-1000 ng mL-1 for metronidazole and clarithromycin, respectively) were obtained. At the end, the introduced method was applied on the plasma samples of the patients treated with metronidazole and clarithromycin successfully.
Subject(s)
Clarithromycin , Metronidazole , Humans , Chromatography, High Pressure Liquid , Surface-Active Agents , Solvents , Water , CarbonABSTRACT
In this work, for the first time, a polymeric composite based on ß-cyclodextrin grafted with polyethylene has been prepared through ball milling and used as an efficient sorbent for dispersive solid phase extraction of metronidazole and clarithromycin from plasma samples. The prepared sorbent was characterized using Fourier transform infrared spectrophotometry, X-ray diffraction, and scanning electron microscopy. In the extraction process, after precipitating the proteins, the sorbent was added into the sample solution, and the mixture was vortexed to facilitate and speed up the sorption of the analytes onto the sorbent surface. After centrifuging, the sorbent particles were contacted with methanol to elute the analytes under the vortexing process. After this step, an aliquot of the eluate was taken and injected into high-performance liquid chromatography-diode array detector for quantitative analysis. Under the optimum extraction conditions, the extraction recoveries for metronidazole and clarithromycin were 76 and 83%, respectively. The limits of detection were 2.6 and 2.2 ng/ml for metronidazole and clarithromycin, respectively. The repeatability of the offered approach, expressed as relative standard deviation, was equal to or less than 4.7%. Finally, the method was successfully applied to plasma samples of the patients treated with metronidazole and clarithromycin.