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EN
New, sensitive, rapid, cost-effective, and validated stability-indicating thin layer chromatographic (TLC) method coupled with fluorescence (FL) detection was developed for the quantitative analysis of celecoxib (CEL) and amlodipine besylate (AMLO) in their laboratory prepared binary mixture using the non-fluorescent TLC silica gel 60 plates. Ethyl acetate: diethylamine: 1-propanol (9:1:0.2, V/V) was used as a developing system. The retention factor (Rf) for each drug was 0.80 ± 0.03 and 0.44 ± 0.01 for CEL and AMLO, respectively. The plates were excited at 264 nm for the simultaneous FL measurement of CEL and AMLO, the calibration curves were linear over a concentration ranges of 30.0–300.0 ng/band and 15.0–150.0 ng/band with mean percentage recoveries of 99.80 ± 0.85 and 99.80 ± 0.77 For CEL and AMLO, respectively. The developed method was applied for the stability studies of the cited drugs in their laboratory prepared binary mixture and the forced degradation products were determined when present in presence of the pure drugs so the method can be considered as a stability-indicating one and it was validated as per ICH guidelines and proved to be accurate and precise.
EN
Two sensitive and selective chromatographic methods were developed for determination of finasteride and tamsulosin hydrochloride in bulk powder and a pharmaceutical formulation. The first method was based on high-performance liquid chromatography (HPLC) separation of the cited drugs in the presence of the acid degradation product of finasteride. The separation was achieved using a C18 column (300 mm × 3.9 mm; 10-μm particle size) and a mobile phase consisting of 0.04 M ortho-phosphoric acid (pH 3.5 ± 0.2 adjusted with triethylamine) and acetonitrile (50:50, v/v). Quantification was achieved with ultraviolet (UV) detection at 215 nm. Linearity was in the range of 10.00–110.00 μg/mL and 2.00–44.00 μg/mL for finasteride and tamsulosin hydrochloride, respectively. Thin-layer chromatography (TLC)–densitometric method was achieved on an aluminum plates pre-coated with silica gel 60 F254 using toluene–ethanol–diethylamine (8:2:1.5, by volume) as eluent, and the RF values of tamsulosin hydrochloride and finasteride were 0.57 and 0.64, respectively. Quantification was achieved with UV detection at 250 nm for finasteride and 280 nm for tamsulosin hydrochloride. Linearity was in the range of 1.00–40.00 and 0.2.00–20.00 μg per spot for finasteride and tamsulosin hydrochloride, respectively. The results obtained were validated according to the International Conference on Harmonisation (ICH) guidelines. A statistical comparison between the obtained results and the results of a reported method was carried out.
EN
Two sensitive and selective chromatographic methods have been developed and validated for analysis of idrocilamide in the presence of its degradation products. Forced degradation studies were performed using HCl, NaOH, and 3% H2O2. The first method is based on thin-layer chromatographic separation of the intact drug from its degradation products, followed by densitometric measurement. The second method is based on isocratic reversed phase high-performance liquid chromatographic separation of the drug from its degradation products on a C18 column. The HPLC method was used to investigate the kinetics of alkaline degradation of the drug at different temperatures.
EN
A new simple, precise, accurate, and selective thin-layer chromatographic (TLC) method has been developed for simultaneous analysis of atenolol and lercanidipine hydrochloride in a tablet dosage form. Chromatographic separation was achieved on aluminum foil plates precoated with silica gel 60F 254 , with toluene-methanoltriethylamine 3.5:1.5:0.1 (v/v) as mobile phase. Detection was performed densitometrically at 275 nm. The R F of atenolol and lercanidipine hydrochloride were 0.24 and 0.68, respectively. The reliability of the method was assessed by evaluation of linearity (2000-12000 ng per band for atenolol and 400-2400 ng per band for lercanidipine hydrochloride), accuracy (98.94 š 0.30% for atenolol and 99.75 š 0.69% for lercanidipine hydrochloride), and specificity, in accordance with ICH guidelines. The method can be used for routine simultaneous analysis of atenolol and lercanidipine hydrochloride in pharmaceutical formulations.
EN
A new simple, accurate, precise, rapid, and selective densitometric TLC method has been established for simultaneous analysis of aceclofenac, paracetamol, and chlorzoxazone in tablets. Identification and quantification were performed on 10 cm × 10 cm aluminium-backed TLC plates coated with 0.2 mm layers of silica gel 60 F 254 , previously washed with methanol, and using toluene-2-propanol-ammonia 4:4:0.4 (υ/υ) as mobile phase. Detection was performed at 274 nm. The R F values of aceclofenac, paracetamol, and chlorzoxazone were 0.28 š 0.01, 0.72 š 0.02, and 0.51 š 0.02, respectively. Calibration plots were linear in the range 400-1400 ng per band for aceclofenac, 2000-7000 ng per band for paracetamol, and 1000-3500 ng per band for chlorzoxazone, with correlation coefficients, r , 0.9995, 0.9993, and 0.9996, respectively. Recovery of aceclofenac, paracetamol, and chlorzoxazone were 99.54-100.44, 100.02-100.47, and 99.39-99.84%, respectively. The suitability of densitometric TLC for quantitative analysis of these compounds was proved by validation in accordance with the requirements of ICH Guidelines.
EN
The aim of the presented research was to optimize fluorescence detection conditions for selected biological active organic compounds after their TLC separation using densito-metry. Application of fluorescence to a quantitative analysis of organic compounds requires measuring fluorescence vs. time dependence separately for each determined compound. In this paper, time changes
PL
Celem pracy była optymalizacja warunków pomiarów fluorescencj i wybranych aktywnych biologicznie związków organicznych. Badane związki rozdzielano za pomocąTLC z zastosowaniem densytometrii. Wykorzystanie metody fluorescencyjnej do analizy ilościowej związków organicznych wymaga prowadzenia pomiaru zmian fluorescencji w czasie, oddzielnie w przypadku każdego oznaczanego związku. W pracy przedstawiono wyniki takich pomiarów dla różnych grup związków o własnościach kancerogennych.
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