A simple and highly sensitive cloud point extraction process was suggested for preconcentration of micrograms amount of isoxsuprine hydrochloride (ISX) in pure and pharmaceutical samples. After diazotization coupling of ISX with diazotized sulfadimidine in alkaline medium, the azo-dye product quantitatively extracted into the Triton X-114 rich phase, dissolved in ethanol and determined spectrophotometrically at 490 nm. The suggested reaction was studied with and without extraction and simple comparison between the batch and CPE methods was achieved. Analytical variables including concentrations of reagent, Triton X-114 and base, incubated temperature, and time were carefully studied. Under the selected optimum conditions, the linearity ranges of calibration curves were 1-9 and 0.5-8 µg/mL with detection limits of 0.26 and 0.09 µg/mL of ISX for batch and CPE methods respectively. A relative standard deviation (RSD %) best than 1.98 and 2.67 % with the percentage recoveries range 100.14 and 99.63 % were obtained for both methods respectively. The proposed methods were successfully used in routine analysis of ISX in pharmaceutical forms with high accuracy and reproducibility.
The present study describes employing zero-, 1st - and 2nd -order derivative spectrophotometric methods have been developed for determination of lorazepam (LORA) and clonazepam (CLON) in commercially available tablets. LORA was determined by means of 1st (D1), 2nd (D2) derivative spectrophotometric techniques using zero cross, peak height, and Peak area. D1 used for the determination of CLON by using zero cross and peak height while D2 (zero cross) was used for the determination of CLON. The method was established to be linear in concentration containing different ratios of LORA and CLON range of (20-200 mg/L) and (5-35 mg/L) at wavelength range (250 -370 nm), (210-370nm) respectively. The proposed techniques are highly sensitive, precise a
... Show MoreDetermination of vitamin B6 (pyridoxine hydrochloride) was described using high performance liquid chromatographic method. The analysis was achieved by cosmos IL 5C18-MS-II column (250 mm x 4.6 mm i. d., 5µm particle size) at room temperature. The mobile phase used was Acetonitrile, buffer solution (Citric acid, Na2HPO4 pH4) buffer solution in the ratio (70:30) (V: V). the flow rate was set to 1.25 mL.min-1 and the retention time 1.82 min with UV-detection at 282 nm. Beer's law was obeyed over the concentration range 10-1250 µg.mL-1. The method was accurate (relative error % less than 0.05%), precise (RSD better than ±1.05%), average recovery 100.
... Show MoreThe aim of this work was to develop and validate a rapid and low cost method for estimation of ibuprofen in pharmaceutical suspensions using Reverse-Phase High Performance Liquid Chromatography. The proposed method was conducted and validated according to International Conference on Harmonization (ICH) requirements. The chromatographic parameters were as follows: column of octyldecylsilyl C18 with dimensions (150 × 4.6) mm, mobile phase composed of acetonitrile with phosphoric acid with a ratio of 50 to 50 each using isocratic mode, flow rate of 1.5 mL/min and injection volume of 5 μL. The detection was carried out using UV detector at 220 nm. The method was validated and showed short retention time for ibuprofen peak at 7.651 min, wit
... Show MoreSimple, rapid and sensitive spectrophotometric method was proposed for the analysis of metoclopramide hydrochloride (MPH) in pure form as well as in pharmaceutical tablets. The method is based on the diazotization reaction of MPH with sodium nitrite in hydrochloric acid medium to form diazonium salt, which is coupled with 1-naphthol in sodium hydroxide medium to form azo dye, showing absorption maxima at 550 nm. Beer’s law is obeyed in the concentration range of 0.4 – 18 µg mL-1 of MPH with detection limit 0.5448 µg mL-1. The molar absorptivity and Sandell’s sensitivity are 3.4969 × 104 L mol-1 cm-1 and 0.0101 µg cm-2, respectively. The method was successfully applied to the determination of MPH in pharmaceutical tablets with
... Show MoreA rapid and sensitive method for the determination of amoxicillin trihydrate (AMXT) based on the diazo-coupling reaction was studied. Sulphanilic acid diazotizes with nitrite ion in acidic medium to produce a water soluble, colorless diazonium ion, which subsequently coupled with AMXT to form a colored azo dye in the alkaline medium, having maximum absorption at 455 nm. The calibration graph showed that Beer's law is obeyed over the concentration range of 0.3 – 30.0 μg/mL of AMXT, with the detection limit of 0.15 μg/mL and molar absorptivity was 2.3 × 104 L/mol.cm. The accuracy and the precision were acceptable depending upon the values of error percentage and relative standard deviation. The influence of common interfer
... Show MoreNitroso-R-salt is proposed as a sensitive spectrophotometric reagent for the determination of paracetamol in aqueous solution. The method is based on the reaction of paracetamol with iron(III) and subsequent reaction with nitroso-R-salt to yield a green colored complex with maximum absorption at 720 nm. Optimization of the experimental conditions was described. The calibration graph was linear in the concentration range of 0.1 – 2.0 ?g mL-1 paracetamol with a molar absorptivity of 6.9 × 104 L mol-1 cm-1. The method was successfully applied to the determination of paracetamol in pharmaceutical preparations without any interference from common excipients. The method has been statistically evaluated with British Pharmacopoeia method a
... Show MoreThe main objective of this paper is to develop and validate flow injection method, a precise, accurate, simple, economic, low cost and specific turbidimetric method for the quantitative determination of mebeverine hydrochloride (MbH) in pharmaceutical preparations. A homemade NAG Dual & Solo (0-180º) analyser which contains two identical detections units (cell 1 and 2) was applied for turbidity measurements. The developed method was optimized for different chemical and physical parameters such as perception reagent concentrations, aqueous salts solutions, flow rate, the intensity of the sources light, sample volume, mixing coil and purge time. The correlation coefficients (r) of the developed method were 0.9980 and 0.9986 for cell
... Show MoreA simple, rapid and environmentally friendly dispersive liquid–liquid microextraction method-based spectrophotometric method for the trace determination of folic acid has been developed. The proposed method is based on the formation of a deep yellow product via reaction of folic acid and 1,2-naphthoquine-4-sulfonate at pH = 9. The formed complex was extracted using a mixture of chloroform and ethanol. Then, the tiny organic droplets were measured at λ = 520 nm. At the optimum conditions, linearity was ranged from 0.05 to 1.5 μg/mL for the standard and samples, with a linear correlation coefficient of 0.9996. The detection limits were 0.02, 0.027, 0.03, 0.02 and 0.04 μg/mL for standard, tablet (5 mg), tablet (1 mg), syrup and fl
... Show MoreA simple, accurate, precise, rapid, economical and a high sensitive spectrophotometric method has been developed for the determination of tadalafil in pharmaceutical preparations and industrial wastewater samples, which shows a maximum absorbance at 204 nm in 1:1 ethanol-water. Beer's law was obeyed in the range of 1-7?g/ mL ,with molar absorptivity and Sandell ? s sensitivity of 0.783x105l/mol.cm and 4.97 ng/cm2respectively, relative standard deviation of the method was less than 1.7%, and accuracy (average recovery %) was 100 ± 0. 13. The limits of detection and quantitation are 0.18 and 0.54 µg .ml-1, respectively. The method was successfully applied to the determination of tadalafil in some pharmaceutical formulations
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