A simple, sensitive, accurate and low cost effective spectrophotometric method has been developed for the determination of Tetracycline and Doxycycline in pure and pharmaceutical formulations. The method is based on the reaction of methyldopa with 4-aminoantipyren (4-AAP) in presence of potassium ferriecyanide (PFC) in an alkaline medium. Two optimization methods were applied to determine the optimum conditions of oxidizing coupling reaction variables; univariate and design of experiment (DOE) method. The conditions effecting the reaction; pH, buffer Volume, reagent concentration, oxidant concentration, type of buffer, order of addition, time of reaction and stability were optimized . Under univariate and design of experiment (DOE) method; the Tetracycline colored product having (λmax) at 531nm 535nm. Beer’s law was obeyed in concentration range of [two scale (1-18 µg.mL-1) and (15-70µg.mL-1)] with correlation coefficient of 0.9997 and 0.9942 respectively and for second method [two scale (1-30 µg.mL-1) and (40-100µg.mL-1)] with correlation coefficient of 1 and 0.9913. The assay limits of detection quantification were 0.1732, 0.3123µg.mL-1 respectively. Under univariate the Doxycycline colored product having (λmax) at 515nm. Beer’s law was obeyed in concentration range (10-90 µg.mL-1) with correlation coefficient of 0.9995. The assay limits of detection quantification were 1.0724µg.mL-1. The method was successfully applied to the analysis of the drug tablets formulation.
A new simple and sensitive spectrophotometric method for the determination of trace amount of Cu(II) in the ethanol solution have been developed. The method is based on the complexation of Cu(II) with ethyl cyano(2-methyl carboxylate phenyl azo acetate) (ECA) in basic medium of sodium hydroxide givining maximum absorbance at (λmax = 521 nm). Beer's law is obeyed over the concentration range (5-50) (μg / ml) with molar absorptivity of (3.1773 × 102 L mol-1 cm-1) and correlation coefficient (0.9989). The optimum conditions for the determination of Cu(II)-complex and have been studied and applied to determine Cu(II) in synthetic water sample using simple and standard addition methods.
This paper present a simple and sensitive method for the determination of DL-Histidine using FIA-Chemiluminometric measurement resulted from oxidation of luminol molecule by hydrogen peroxide in alkaline medium in the presence of DL-Histidine. Using 70?l. sample linear plot with a coefficient of determination 95.79% for (5-60) mmol.L-1 while for a quadratic relation C.O.D = 96.44% for (5-80) mmol.L-1 and found that guadratic plot in more representative. Limit of detection was 31.93 ?g DL-Histidine (S/N = 3), repeatability of measurement was less that 5% (n=6). Positive and negative ion interferances was removed by using minicolume containing ion exchange resin located after injection valve position.
Rapid, reproducible and accurate method has been developed for the assay for of mebendazol (MBZ) residual assay. The method is based on alkaline hydrolysis of MBZ with sodium hydroxide then oxidation with N-bromosuccinimide (NBS) followed by coupling with 4-Bromoaniline (4-BA) to yield a highly colored product absorbed at maximum 434 nm. Regression analysis of linearity range was found (0.6-2.8) µg.ml-1. The optimum conditions that affect the oxidation were studied. The developed method was found to be precise with mean value of relative standard deviation (1.153- 1.303) and accurate with relative error (-0.5940-1.7821) .The calculated molar absorptivity and sandal sensitivity values of (29825 L.mol-1.cm-1), 0.0099 µg.cm-2 respe
... Show MoreA newly developed FIA-merging zones spectrophotometric system, the method is rapid, accurate and sensitive for metformin hydrochloride determination through the oxidation of 1- naphthol by sodium hypochlorite and coupling with metformin.HCl in the presence of sodium hydroxide to form a blue soluble ion pair and this product was determined using homemade CFIA-Merging zones techniques , at 580 nm. Data treatment shows that linear range is (0.5-35) µg/ ml. The optimization conditions for various chemical and physical conditions of [MTF- NaOCl-α-naphthol-NaOH] system were investigated. The LOD was 0.01µg / ml and LOQ 0.1µg/ml from the lowest concentration of the calibration graph with r2% 99.18 and RSD% did
... Show MoreSimple and sensitive kinetic methods are developed for the determination of Paracetamol in pure form and in pharmaceutical preparations. The methods are based on direct reaction (oxidative-coupling reaction) of Paracetamol with o-cresol in the presence of sodium periodate in alkaline medium, to form an intense blue-water-soluble dye that is stable at room temperature, and was followed spectrophotometriclly at λmax= 612 nm. The reaction was studied kinetically by Initial rate and fixed time (at 25 minutes) methods, and the optimization of conditions were fixed. The calibration graphs for drug determination were linear in the concentration ranges (1-7 μg.ml-1) for the initial rate and (1-10 μg.ml-1) for the fixed time methods at 25 min.
... Show MoreThe drug promethazine hydrochloride (PRZH) forms with rhodium (II) a colored chelate (?max = 472 nm) complex at (pH = 2.1) which is extractable with benzyl alcohol as organic solvent. Under the appropriate experimental conditions a calibration plot was set up from which some analytical parameter were derived and deduced by regression. Standard addition procedure was also adopted. It has been estimated that the concentration of the drug PRZH to be 24.89 mg per unit and 24.19 mg per unit for both calibrations. Under optimal conditions, the developed method has been achieved the following characteristics: LDR (30 – 150 µg ml-1 ) PRZH , RSD % ( 0.6 – 2.47 ) , sandell sensitivity( 0.0844 µg. cm -2 ) , LOD ( 1.66 µgml-1 ) , recovery
... Show MoreSimple, sensitive and economical spectrophotometric methods have been developed for the determination of cefixime in pure form. This method is based on the reaction of cefixime as n-electron donor with chloranil to give highly colored complex in ethanol which is absorb maximally at 550 nm. Beer's law is obeyed in the concentration ranges 5-250 µg ml-1 with high apparent molar absorptivities of 1.52×103 L.mole-1. cm-1.
This research involves an indirect Fluorophotometric method for the determination of microgram amount of oxymetazoline hydrochloride in the concentration range 0.1-5.0 g/ml. The method is based on the oxidation of the drug by cerium sulphate solution which is acidic medium where Ce IV is reduced to Ce III which can be excited at 259 nm to give an emitted light at 377 nm which is directly proportional to the concentration of Ce III which is equivalent to Ce IV that is needed to oxidize the studied drug. The average recovery of the method is 100.19% and relative standard deviation (RSD) < 0.37% . The method have been successfully applied to the determination of the studied drug in its pure and pharmaceutical preparations and it wa
... Show MoreA new simple and sensitive spectrophotometric method is described for quantification of Nifedipine (NIF) and their pharmaceutical formulation. The selective method was performed by the reduction of NIF nitro group to yield primary amino group using zinc powder with hydrochloric acid. The produced aromatic amine was submitted to oxidative coupling reaction with pyrocatechol and ammonium ceric nitrate to form orange color product measured spectrophotometrically with maximum absorption at 467nm. The product was determined through flow injection analysis (FIA) system and all the chemical and physical parameters were optimized. The concentration range from 5.0 to 140.0 μg.mL-1 was obeyed Beer’s law with a limit of detection and quantitatio
... Show MoreComplexes of Co(II),Ni(II),Cu(II)and Zn(II) with mixed ligand of 4- aminoantipyrine (4-AAP) and tributylphosphine (PBu3) were prepared in aqueous ethanol with (1:2:2) (M:L:PBu3). The prepared complexes were characterized using flame atomic absorption, FT.IR and UV-Vis spectroscopic methods as well as magnetic susceptibility and conductivity measurements. In addition biological activity of the two ligands and their complexes against three selected type of bacteria were also examined. The general compositions of the complexes are found to be [M(4-AAP)2(PBu3)2] Cl2 . Where M= Co(II),Ni(II),Cu(II)and Zn(II). Some of the complexes exhibit good bacterial activities. From the obtained data the octahedral structures have suggested for all prepare
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