In this work, a simple and very sensitive cloud point extraction (CPE) process was developed for the determination of trace amount of metoclopramide hydrochloride (MTH) in pharmaceutical dosage forms. The method is based on the extraction of the azo-dye results from the coupling reaction of diazotized MTH with p-coumaric acid (p-CA) using nonionic surfactant (Triton X114). The extracted azo-dye in the surfactant rich phase was dissolved in ethanol and detected spectrophotometrically at λmax 480 nm. The reaction was studied using both batch and CPE methods (with and without extraction) and a simple comparison between the two methods was performed. The conditions that may be affected by the extraction process and the sensitivity of methods were carefully studied. Using optimal conditions, the linearity of calibration curves was in the range of 0.4-13 and 0.05-4µg/mL and limits of detection of 0.044 and 0.028 µg/mL of MTH for batch and CPE methods respectively. Average recoveries for samples were detected to be between 97-101 %for both methods, with the relative standard deviation (RSD %) best than 2.7 % and 4.5 % for both methods, respectively. The suggested methods were applied successfully for assay of MTH in commercial pharmaceutical tablets.
a simple accurate and sensitive spectrophotometric method for the determination of promethazine HCI has been developed the method is based on the oxidative coupling reaction of promethazine
A sensitive, accurate, and affordable colorimetric method was developed for assaying prednisolone (PRZ) in various medicinal forms. The procedure involves the oxidation of PRZ by ferric ions, followed by complexation of the resulting ferrous ions with ferricyanide to produce a greenish-blue product. Common complexation conditions were thoroughly investigated. The mole ratio of FeCl₃·6H₂O to K₃Fe(CN)₆ was 8:1. The proposed mechanism of complexation was suggested and considered. Various parameters were optimized, including the reduction of the colorimetric reaction temperature to 50°C and the duration of heating and analysis to 20-30 minutes. The calibration curve was linear over the range of 1-60 µg/mL. The limit of detection (LOD
... Show MoreThe present work establishes and validates HILIC strategies simple, accurate, exact and precise in pure form and inpharmaceutical dosage for separating and determining theophylline. These methods are developed on HILIC theophyllineseparation in columns ZIC2 and ZIC3. The eluent was prepared by mixing buffer (20% sodium acetate-40 mM, pH 5.5), 80%acetonitrile. The flow rate is 0.8 mL/min, with gradient elution and UV detection at 270 nm. In the ZIC2 and ZIC3 columns oftheophylline determining, the concentration range was 0.01-4μg.ml-1. The lower limit of detection and quantification fortheophylline were determined as 0.130, 0.190 μg.ml-1 and accuracy were 99.70%, 99.58% on ZIC2 and ZIC3, respectively. TheHILIC methods developed and validat
... Show MoreAn easy, eclectic, precise high-Performance Liquid Chromatographic (HPLC) procedure was evolved and validated to estimate of Piroxicam and Codeine phosphate. Chromatographic demarcation was accomplished on a C18 column [Use BDS Hypersil C18, 5μ, 150 x 4.6 mm] using a mobile phase of methanol: phosphate buffer (60:40, v/v, pH=2.3), the flow rate was 1.1 mL/min, UV detection was at 214 nm. System Suitability tests (SSTs) are typically performed to assess the suitability and effectiveness of the entire chromatography system. The retention time for Piroxicam was found to be 3.95 minutes and 1.46 minutes for Codeine phosphate. The evolved method has been validated through precision, limit of quantitation, specificity,
... Show MoreA simple, rapid and sensitive spectrophotometric method has been developed for the determination of captopril in aqueous solution. The method is based on reaction of captopril with 2,3-dichloro 1,4- naphthoquinon(Dichlone) in neutral medium to form a stable yellow colored product which shows maximum absorption at 347 nm with molar absorptivity of 5.6 ×103 L.mole-1. cm-1. The proposed method is applied successfully for determination of captopril in commercial pharmaceutical tablets.
A sensitive spectrofluorimetric method for the determination of glibenclamide in its tablet formulations has been proposed. The method is based on the dissolving of glibenclamide in absolute ethanol and measuring the native fluorescence at 354 nm after excitation at 302 nm. Beers law is obeyed in the concentration of 1.4 to 10 µg.ml-1 of glibenclamide with a limit of detection (LD) of 0.067 µg.ml-1 and a standard deviation of 0.614. The range percent recoveries (N=3) is 94 - 103.
Beta-lactam medications are among the commonly used antibiotics that share the presence of a beta-lactam ring in their chemical formation. A modern, rapid, highperformance liquid chromatography technique was advanced and validated according to FDA and EMA rules for the concurrent determination of medications in their pharmaceutical and pure forms This study deals with the determination of beta-lactam drugs )Amoxicillin, Ampicillin Cephalexin, Cefotaxime, Cefoxitin, Cefamandole, Cephalothin, Piperacillin, Penicillin, Oxacillin, Cloxacillin Nafcillin, Carbenicillin, Mezlocillin and Dicloxacillin) which is a RP-HPLC technique with an UV detector using a column NEUCLEODUR C-18 (4.0 mm × 100 mm, 5µm particle size), The heat of the chr
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