ABSTRACT
A validated, reliable and accurate reversed-phase high performance liquid chromatographic method using pre-column derivatization was adopted for the simultaneous determination of two ternary mixtures containing omeprazole, tinidazole and doxycycline hyclate or clarithromycin. Separation was achieved on a C18 column, through a gradient elution system using acetonitrile-methanol-water adjusted to pH = 6.60. Drugs were detected at 277 nm over concentration ranges of 1-112, 5-125, 2.5-550 and 2.5-100 µg/mL for omeprazole, tinidazole, doxycycline hyclate and clarithromycin, respectively. This is the first method that has isolated and identified clarithromycin derivative by infrared and mass spectroscopy. This method is the first study for the simultaneous determination of omeprazole, tinidazole, doxycycline hyclate and clarithromycin in combined mixtures and pharmaceutical formulations.
Subject(s)
Chromatography, High Pressure Liquid/methods , Clarithromycin/analysis , Doxycycline/analysis , Omeprazole/analysis , Tinidazole/analysis , Chromatography, Reverse-Phase/methods , Clarithromycin/chemistry , Clarithromycin/isolation & purification , Doxycycline/chemistry , Doxycycline/isolation & purification , Drug Stability , Least-Squares Analysis , Omeprazole/chemistry , Omeprazole/isolation & purification , Reproducibility of Results , Tablets/chemistry , Tinidazole/chemistry , Tinidazole/isolation & purificationABSTRACT
A polymethacrylate-based molecularly imprinted monolithic column bearing mixed functional monomers, using non-covalent imprinting approach, was designed for the rapid separation of nitroimidazole compounds. The new monolithic column has been prepared via simple in situ polymerization of 2-hydroxyethyl methacrylate, dimethylaminoethyl methacrylate and ethylene dimethacrylate, using (S)-ornidazole ((S)-ONZ) as template in a binary porogenic mixture consisting of toluene and dodecanol. The composition of the polymerization mixture was systematically altered and optimized by altering the amount of monomers as well as the composition of the porogenic solvent. The column performance was evaluated in pressure-assisted CEC mode. Separation conditions such as pH, voltage, amount of organic modifier and salt concentration were studied. The optimized monolithic column resulted in excellent separation of a group of structurally related nitroimidazole drugs within 10 min in isocratic elution condition. Column efficiencies of 99 000, 80 000, 103 000, 60 000 and 99 000 plates/m were obtained for metronidazole, secnidazole, ronidazole, tinidazole and dimetridazole, respectively. Parallel experiments were carried out using molecularly imprinted and non-imprinted capillary columns. The separation might be the result of combined effects including hydrophobic, hydrogen bonding and the imprinting cavities on the (S)-ONZ-imprinted monolithic column.
Subject(s)
Antiprotozoal Agents/isolation & purification , Capillary Electrochromatography/methods , Nitroimidazoles/isolation & purification , Chromatography, High Pressure Liquid , Dimetridazole/isolation & purification , Metronidazole/isolation & purification , Ornidazole/isolation & purification , Permeability , Pressure , Ronidazole/isolation & purification , Tinidazole/isolation & purificationABSTRACT
The main objective of the present study was to analyze the efficacy of technologies based on ozone and activated carbon in dynamic regime to remove organic micropollutants from waters, using the antibiotic tinidazole (TNZ) as a model compound. Results obtained in static regime show that the presence of activated carbon (GAC) during tinidazole ozonation: (i) increases its removal rate, (ii) reduces oxidation by-product toxicity, and (iii) reduces the concentration of dissolved organic matter. Study of the ozone/activated carbon system in dynamic regime showed that ozonation of tinidazole before the adsorption process considerably improves column performance, increasing the volume of water treated. It was observed that the efficacy of the treatment considerably increased with a shorter contact time between TNZ and O(3) streams before entering the column allowing a much higher volume of TNZ solution to be treated compared with the use of activated carbon alone, and reducing by 75% the amount of activated carbon required per unit of treated water volume. TNZ removal by the O(3)/GAC system is lower in natural waters and especially in wastewaters, than in ultrapure water. The toxicity results obtained during TNZ treatment with O(3)/GAC system showed that toxicity was directly proportional to the concentration of TNZ in the effluent, verifying that oxidation of the organic matter in the natural waters did not increase the toxicity of the system.
