HPLC Determination of Imidazoles with Variant Anti-Infective Activity in Their Dosage Forms and Human Plasma (original) (raw)
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ABSTRACT A reverse phase high performance liquid chromatography method was developed in this research for separation and assay of antiprotozoal imidazole derivatives (Metronidazole, Tinidazole and Secnidazole). The separation was achieved by C8 column using acetonitrite: water (20:80 v/v) as a mobile phase, a flow rate of 1.5 ml/min. UV detection was carried out at 318 nm. The retention times of metronidazole, secnidazole and tinidazole were 4.140, 5.515 and 6.692 min respectively. The qualitative study of this method included the effect of flow rate and the ratio of the components of mobile phase on the quality of separation. The method was validated for accuracy, precision, selectivity and robustness. Linearity of metronidazole, secnidazole and tinidazole were in the range of 80-120 μg/ml. The relative standard deviation for precision was not more than 2%. The recoveries in accuracy obtained for metronidazole, secnidazole and tinidazole were 99.22%, 99.89 and 99.64% respectively. The developed method was found to be rapid, accurate and precise and was used for the determination of the three compounds in raw materials and tablets. This method was also used for the assay of these three compounds in the spiked human serum (1-30 μg/ml) and recoveries were in the range of 88-96%. Keywords: RP-HPLC, Metronidazole, Tinidazole, Secnidazole.
Eurasian Journal of Analytical Chemistry, 2017
Imidazoles are well known heterocyclic compounds having important feature of a variety of medicinal agents. Studies with imidazole containing compounds are great importance in the clinical use of drugs. The presence of imidazole group in the molecules of lanoconazole (LCZ) and butoconazole (BCZ) is very important for its chemical and analytical behavior. Target analytes were efficiently separated with a Pinnacle DB Cyano column (5 µm, 4.6 x 250 mm I.D.) and oxiconazole (OCZ) used as an internal standard. In this study, correlation between the retention factors of the solutes and pH of the mobile phase was determined at ten pH values in acetonitrile-water binary mixture. In optimization condition, quantification of these drugs were performed in human urine. The linear responses were observed over a wide concentration range (6.25.
Analysis of imidazoles and triazoles in biological samples after MicroExtraction by packed sorbent
Journal of enzyme inhibition and medicinal chemistry, 2017
This paper reports the MEPS-HPLC-DAD method for the simultaneous determination of 12 azole drugs (bifonazole, butoconazole, clotrimazole, econazole, itraconazole, ketoconazole, miconazole, posaconazole, ravuconazole, terconazole, tioconazole and voriconazole) administered to treat different systemic and topical fungal infections, in biological samples. Azole drugs separation was performed in 36 min. The analytical method was validated in the ranges as follows: 0.02-5 μg mL(-1) for ravuconazole; 0.2-5 μg mL(-1) for terconazole; 0.05-5 μg mL(-1) for the other compounds. Human plasma and urine were used as biological samples during the analysis, while benzyl-4-hydroxybenzoate was used as an internal standard. The precision (RSD%) and trueness (Bias%) values fulfill with International Guidelines requirements. To the best of our knowledge, this is the first HPLC-DAD procedure coupled to MEPS, which provides the simultaneous analysis of 12 azole drugs, available in the market, in human pl...
E-Journal of Chemistry, 2010
A novel approach was carried out to develop and validate a rapid, specific, accurate and precise reverse phase ultra performance liquid chromatographic (UPLC) method for the simultaneous separation and quantification of secnidazole, fluconazole and azithromycin in pharmaceutical dosage forms. The developed analytical method is superior in technology to conventional HPLC with respect to time, resolution, solvent consumption and cost of analysis. Elution time for the separation was 10 min and ultra violet detection was carried out at 210 nm. Efficient separation was achieved on BEH C18 sub-2-μm UPLC column using 0.002 M Na2HPO4and acetonitrile as organic solvent in a gradient program. Benzophenone was used as internal standard. Resolutions between secnidazole, fluconazole and azithromycin were found to be more than 4.8. The calibration graphs were linear for secnidazole, fluconazole, benzophenone and azithromycin. The method showed excellent recoveries for all dosage forms. The test s...
Journal of Chromatography B: Biomedical Sciences and Applications, 1997
A rapid, reproducible high-performance liquid chromatographic method for the determination of secnidazole, 5 nitroimidazole class of antiprotozoals from blood is described. Metronidazole was used as an internal standard. A simple extraction step with dichloromethane was done before chromatography on a C,, column with the wavelength fixed at 276 nm on the UV detector. Blood levels up to 500 ng/ml have been measured with good precision in the healthy volunteers after 1 g of secnidazole was administered. The present described method can readily be utilized for routine pharmacokinetic studies.
2021
A novel High-Performance Thin-Layer Chromatography (HPTLC) method was portrayed for the determination of Fenticonazole Nitrate (FTZ) in Bulk and Vaginal Capsules. The estimation of Fenticonazole Nitrate was achieved on aluminium pre-coated sheets of silica gel 60 F(10 cm × 10 cm) using mobile phase Toluene: Methanol: Triethylamine (4:1:0.5 v/v/v). Densitometry detection of Fenticonazole Nitrate was performed at 254nm. Fenticonazole nitrate demonstrated a strong correlation with a coefficient of correlation of 0.999 over the concentration range of 500 – 3000 ng/band. The Rvalue for Fenticonazole Nitrate was found to be 0.65. As per International Conference on Harmonization the established method was successfully validated to various parameters like accuracy, precision, sensitivity, specificity, robustness and shows the satisfactory results for all parameters. The recognized method is simple, accurate, precise, robust, sensitive and economical in nature. This method can be used for qu...
A simple and precise reversed-phase high performance liquid chromatography (HPLC) method for the determination of metronidazole in human plasma was developed and validated. Using tinidazole as an internal standard (IS), separation was achieved on Symmetry shield RP18 column. The mobile phase, sodium acetate 0.05 M (pH=4, adjusted with phosphoric acid), and acetonitrile (85:15,v:v) delivered at flow rate 1.0 ml/min. 0.25ml plasma samples were deproteinized with methanol containing 2% perchloric acid and centrifuged. 100µl supernatant clear solution was injected to HPLC system. The eluent was monitored spectrophotometricly at 320 nm. No interference in blank plasma or of commonly used drugs was observed. The relationship between the concentration of metronidazole in plasma and peak area ratio of metronidazole to the IS was linear over the range of 0.05-15.0 μg/ml. Intra-day and inter-day coefficient of variation (CV) and bias were ≤ 6.2% and ≤ 9.0%, and ≤7.3% and ≤ 11.0%, respectively. Mean extraction recovery of metronidazole and the IS from plasma samples was ≥ 88% using the method, metronidazole was found stable under various conditions generally encountered in the clinical laboratory (≥93% and ≥90% in processed and unprocessed samples, respectively). Further, the method was successfully employed to measure metronidazole levels in plasma samples from healthy volunteers.
Simultaneous determination of metronidazole and miconazole in pharmaceutical dosage forms by RP-HPLC
A reversed-phase high performance liquid chromatography (RP-HPLC) method with UV detection is described for the simultaneous determination of metronidazole and miconazole in pharmaceutical dosage forms. Chromatography was carried out on a C18 reversed-phase column, using a mixture of methanol Á/water (40'/60, v/v) as a mobile phase, at a flow rate of 1.0 ml min (1 . Sulfamethoxazole was used as an internal standard and detection was performed using a diode array detector at 254 nm. The method produced linear responses in the concentration ranges 10 Á/70 and 1 Á/20 mg ml (1 with detection limits 0.33 and 0.27 mg ml (1 for metronidazole and micanozole, respectively. This procedure was found to be convenient and reproducible for analysis of these drugs in ovule dosage forms. # 2002 É ditions scientifiques et médicales Elsevier SAS. All rights reserved. .tr (S.A. Ö zkan). Il Farmaco 57 (2002) 953 Á/957 www.elsevier.com/locate/farmac 0014-827X/02/$ -see front matter # 2002 É ditions scientifiques et médicales Elsevier SAS. All rights reserved. PII: S 0 0 1 4 -8 2 7 X ( 0 2 ) 0 1 2 9 6 -X
Separation of imidazole and its derivatives by capillary electrophoresis
Journal of Chromatography A, 1994
The use of capilla~ cicctrophorcsis (CE) for the separation of imidazole and its derivatives is reported. In the first part of the investigation, efforts were focused on method development, where the effects of buffer pH, types of buffer modifiers and modifier concentration on the separation of these compounds were examined. The second part was focused on method validation, where the ruggedness, selectivity, limits of detection and linearity were investigated. In the final part, the CE method was applied to commercial-grade imidazole. A comparison of the results obtained using the CE system was made with those obtained by HPLC. Good correlation between the two sets of results was obtained and superior efficiencies and better peak shapes for most of the imidazoles were also achieved using the CE system.
2006
A rapid and cost effective method for the analysis of metronidazole in biological samples was developed. The extraction method is a simple single-step liquid-liquid process that has eliminated the need for costly extraction and evaporation equipment. The mobile phase consists largely of water, making the method cheap to run with less than 6 min total analytical time per sample. The calibration curve was linear from 0 to 2.00 µg/ml. The regression coefficient was 0.99. The method is highly sensitive, with limit of detection of 1 ng/ml. The coefficient of variation for within-day run was less than 4% while that of day-to-day run was less than 6%. There were no interfering peaks from endogenous materials in the serum. The method was validated and used for pharmacokinetic studies.