ABSTRACT
Tributylphosphine oxide (TBPO) is proposed as an extractant for the extraction of lead(II) and copper(II) from salicylate media. The optimum conditions were evaluated by varying the experimental parameters, such as the pH, sodium salicylate concentration, tributylphosphine oxide (TBPO) concentration, shaking period and various diluents. The probable extracted species, deduced from log-log plots were Pb(HSal)2.2TBPO and Cu(HSal)2.2TBPO. The extraction took place through a solvation mechanism. The method permits the binary separation of lead(II) and copper(II) from commonly associated elements as well as the mutual separation of lead(II) and copper(II). The method is applicable to the determination of lead(II) and copper(II) in various alloys as well as environmental and pharmaceutical samples.
Subject(s)
Aziridines/chemistry , Copper/analysis , Environmental Pollutants/analysis , Epoxy Compounds/chemistry , Lead/analysis , Salicylates/chemistry , Air Pollutants/analysis , Alloys/analysis , Copper/isolation & purification , Drug Combinations , Hydrogen-Ion Concentration , Indicators and Reagents , Lead/isolation & purification , Minerals/analysis , Organic Chemicals , Tablets , Trace Elements/analysis , Vitamins/analysisABSTRACT
A new simple, precise, rapid and selective high-performance thin-layer chromatographic (HPTLC) method has been developed for the simultaneous determination of atenolol (ATL) and amlodipine (AMLO) in tablets, using methylene chloride:methanol:ammonia solution (25% NH3) (8.8:1.3:0.1; v/v) as the mobile phase and Merck HPTLC plates (0.2 mm thickness) precoated with 60F254 silica gel on aluminium sheet as the stationary phase. Detection was carried out densitometrically using a UV detector at 230 nm. The retention factors of ATL and AMLO were 0.33 and 0.75, respectively. Calibration curves were linear in the range 10-500 microg ml(-1) for both. Assays of ATL and AMLO were 49.87 mg per tablet (relative standard deviation (R.S.D.), 1.3%) and 4.90 mg per tablet (R.S.D., 1.38%) for brand I, and 49.27 mg per tablet (R.S.D., 1.12%) and 4.98 mg per tablet (R.S.D., 1.42%) for brand II, respectively. The percentage recoveries for ATL and AMLO for brands I and II were 99.06 and 99.30%, and 99.27 and 99.15%, respectively.
Subject(s)
Amlodipine/analysis , Atenolol/analysis , Chromatography, Thin Layer/methods , Tablets/chemistry , Calibration , Reproducibility of Results , Spectrophotometry, UltravioletABSTRACT
A new, simple, precise, and rapid ion pair reversed-phase high-performance liquid chromatography (RP-HPLC) method has been developed for the simultaneous determination of pyridoxine hydrochloride (PYR) and doxylamine succinate (DOX) in tablets. The stationary phase was a Microbondapak C18 column (10 mu, 300 mm x 3.9 mm i.d.). The mobile phase was water:methanol (60:40) containing 10 mM heptanesulfonic acid and 0.25% triethylamine and adjusted to pH 2.2 with orthophosphoric acid. Detection was carried out at 263 nm using an ultraviolet (UV) detector. The flow rate was 1.0 ml/min, and retention times were 3.65 min and 7.32 min for PYR and DOX, respectively. The linearity was obtained in the concentration range 0.5-500 micrograms/ml for PYR and DOX. Mean percentage recoveries were 100.20% and 101.20% for PYR and DOX, respectively.
Subject(s)
Chromatography, High Pressure Liquid/methods , Doxylamine/analogs & derivatives , Histamine H1 Antagonists/analysis , Pyridoxine/analysis , Doxylamine/analysis , Drug Stability , Linear Models , Reproducibility of Results , TabletsABSTRACT
A new simple, precise, rapid and selective reverse phase ion pair high performance liquid chromatography (HPLC-RP) method has been developed for the simultaneous determination of cinnarizine (CINN) and domepiridone maleate (DOME) from tablets using acetonitrile-methanol-water-0.1 N sulfuric acid (37:10:48:5 v/v/v/v) containing sodium lauryl sulfate (0.01 M), as a mobile phase and a Machery Nagel nitrile column (10 microns, 25 cm x 4.0 mm i.d.) as the stationary phase. The flow of mobile phase through the column was kept at 1.0 ml min(-1) through out the analysis. Detection was carried out using a UV detector at 225 nm. The retention times for CINN and DOME were 4.73 and 9.41 min, respectively. The linearity range and percentage recoveries for CINN and DOME were 4 1000 and 60-750 microg ml(-1) and 99.90 and 99.60%, respectively.
Subject(s)
Calcium Channel Blockers/analysis , Chromatography, High Pressure Liquid/methods , Cinnarizine/analysis , Domperidone/analysis , Dopamine Antagonists/analysis , Tablets/chemistry , Drug Stability , Histamine H1 Antagonists/analysis , Quality ControlABSTRACT
A method is developed for the extraction of lead(II) from an aqueous solution of pH 2.1-8.3 with cyanex 302 [bis(2,4,4-trimethylpentyl monothiophosphinic acid)] in toluene as an extractant. Lead(II) was stripped with 0.1 mol dm(-3) nitric acid and determined spectrophotometrically with PAR. The method is most sensitive and permits the separation of lead(II) from binary mixtures containing commonly associated metal ions. The method is applicable for the separation and determination of lead in alloys and environmental samples.
ABSTRACT
A simple, rapid and precise gas chromatographic method has been developed for the simultaneous determination of pseudoephedrine hydrochloride and diphenhydramine hydrochloride in cough syrup, using a SS column of 10% OV 1 on chromosorb W-HP (80-100 mesh) and nitrogen as a carrier gas at a flow rate of 30 ml min(-1). The oven temperature was programmed at 135 degrees C for 1 min, with a rise of 10 degrees C min(-1) up to 250 degrees C (held for 5 min). The injector and detector port temperatures were maintained at 280 degrees C. Detection was carried out using Flame ionization detector. Guaphenesin was used as an internal standard. Results of assay and recovery studies were statistically evaluated for its accuracy and precision.
ABSTRACT
A new simple, precise, rapid, and selective reversed-phase ion pair high-performance liquid chromatography (RP-HPLC) method has been developed for the simultaneous determination of pseudoephidrine (PSE) and terfanidine (TER) from tablets using 60:15:25 acetontrile:methanol:water (v/v) containing 2.9 g sodium lauryl sulfate/liter, pH adjusted to 3.1 using phosphoric acid as a mobile phase and C18 Spherisorb ODS 2 (3 microns, 5 cm x 4.6 mm i.d.) as stationary phase. Detection was carried out using a UV detector at 254 nm. A constant flow of 1.0 ml/min was maintained throughout the analysis. Retention times for PSE and TER were 1.90 and 7.35 min, respectively. Linearity range and percentage recoveries for PSE and TER were 24-1200 and 12-600 micrograms/ml, and 100.01 and 100.4%, respectively.
Subject(s)
Ephedrine/analysis , Terfenadine/analysis , Calibration , Chromatography, High Pressure Liquid , Solutions , Spectrophotometry, Ultraviolet , TabletsABSTRACT
A new, simple, precise, rapid and stability indicating RP-HPLC method has been developed for the simultaneous determination of mebendazole and pyrantel pamoate from tablets. Chromatography was carried out on a Shodex C8 column using a mixture of 0.05 M monobasic sodium phosphate: acetonitrile: triethylamine (60:40:1.5, v/v), adjusted to pH 6.8 with phosphoric acid. Detection was carried out at 290 nm using a UV detector. Retention times for pamoic acid, pyrantel base and mebendazole were 3.61, 6.41 and 12.81 min, respectively. Linearity was obtained in the concentration range of 20-160 mug and 30-240 mug for pyrantel pamoate and mebendazole, respectively. The method after its application for the assay of pyrantel pamoate and mebendazole from tablets, was statistically evaluated for its accuracy and precision.
