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.
Metoclopramide (MCP) ion selective electrodes based on metoclopramide-phosphotungstic acid (MCP-PT) ion pair complex in PVC matrix membrane were constructed. The plasticizers used were tri-butyl phosphate (TBP), di-octyl phenyl phosphonate (DOPP), di-butyl phthalate (DBPH), di-octyl phthalate (DOP), di-butyl phosphate (DBP), bis 2-ethyl hexyl phosphate (BEHP). The sensors based on TBP, DOPP, DBPH and DOP display a fast, stable and linear response with slopes 59.9, 57.7, 57.4, 55.3 mV/decade respectively at pH ranged 2-6. The linear concentration range between 1.0×10-5 – 1.0×10-2 M with detection limit 3.0×10-6 and 4.0×10-6 M for electrodes using TBP, DOPP and DBPH while e
... Show MoreA simple, precise, and sensitive spectrophotometric method has been established for the analysis of doxycycline. The method includes direct charge transfer complexation of doxycycline withp-Bromanil in acetonitrileto form a colored complex. The intensely colored product formed was quantified based on the absorption band at 377 nm under optimum condition. Beer’s law is obeyed in the concentration range of 1–50 μg.mL-1 with molar absorptivity of 1.5725x104 L.mol-1.cm-1, Sandell's sensitivity index (0.0283) μg.cm-2, detection limit of 0.1064 μg.mL-1, quantification limit 0.3224 μg.mL-1 and association constant of the formed complex (0.75x103). The developed method could find application in routine quality control of doxycycline and has
... Show MoreThis work was influenced the separation and preconcentration steps were carried out to determination of metformin (MET) in pharmaceutical preparations and human serum samples. Complex formation method and cloud-point extraction (CPE) coupling with UV-Visible spectrophotometry were used to investigated of study target.The results has showed the best optical characteristic for calibration curve and statistical data which were obtained under optimum conditions. The first method is based on the reaction of MET with nickel (II) in alkaline medium an absorption maximum ?)max) at 434nm. ''Beer's low'' is obeyed in the concentration range (10-100µg.ml-1) with molar absorptivity of 3.9x103 L.mol-1.cm-1.The limit of detection and quantitation valu
... Show MoreA simple reverse-phase high performance liquid chromatographic method for the simultaneous analysis (separation and quantification) of furosemide (FURO), carbamazepine (CARB), diazepam (DIAZ) and carvedilol (CARV) has been developed and validated. The method was carried out on a NUCLEODUR® 100-5 C18ec column (250 x 4.6 mm, i. d.5μm), with a mobile phase comprising of acetonitrile: deionized water (50: 50 v/v, pH adjusted to 3.6 ±0.05 with acetic acid) at a flow rate 1.5 mL.min-1 and the quantification was achieved at 226 nm. The retention times of FURO, CARB, DIAZ and CARV were found to be 1.90 min, 2.79 min, 5.39 min and 9.56 min respectively. The method was validated in terms of linearity, accuracy, precision, limit of detection and li
... Show MoreMetoclopramide HCl (MTB) is a potent antiemetic drug used for the treatment of nausea and vomiting. Many trials were made to prepare a satisfactory MTB orodispersible tablet using direct compression method.Various super disintegrants were used in this study which are croscarmellose sodium (CCS), sodium starch glycolate (SSG) and crospovidone (CP). The latter was the best in terms of showing the fastest disintegration time in the mouth.Among the different diluents utilized, it was found that a combination of microcrystalline cellulose PH101 (MCC 101), mannitol, dicalcium phosphate dihydrate (DPD) and Glycine was the best in preparing MTB orodispersible tablet with fastest disintegration time in the mouth.The physical parameters of the pre
... Show MoreA procedure for the mutual derivatization and determination of thymol and Dapsone was developed and validated in this study. Dapsone was used as the derivatizing agent for the determination of thymol, and thymol was used as the derivatizing agent for the determination of Dapsone. An optimization study was performed for the derivatization reaction; i.e., the diazonium coupling reaction. Linear regression calibration plots for thymol and Dapsone in the direct reaction were constructed at 460 nm, within the concentration range of 0.3-7 μg ml-1 for thymol and 0.3-4 μg ml-1 for Dapsone, with limits of detection 0.086 and 0.053 μg ml-1, respectively. Corresponding plots for the cloud point extraction of thymol and Dapsone were constructed
... Show Morea 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
In this paper, turbidimetric and reversed-phase ultra-fast liquid chromatography (UFLC) methods were described for the quantitative determination of ephedrine hydrochloride in pharmaceutical injections form. The first method is based on measuring the turbidimetric values for the formed yellowish white precipitate in suspension status in order to determine the ephedrine hydrochloride concentration. The suspended substance is formed as a result of the reaction of ephedrine hydrochloride with phosphomolybdic acid which was used as a reagent. The physical and chemical characteristics of the complex were investigated. The calibration graphs of ephedrine were established by turbidity method. While the second method (UFLC) was conducted using the
... Show MoreA 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
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