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.
The present study combines UV-Vis spectrophotometry and dispersive liquid-liquid microextraction (DLLME) for the preconcentration and determination of trace level clidinium bromide (Clid) in pharmaceutical preparation and real samples. The method is based on ion-pair formation between Clid and bromocresol green in aqueous solution using citrate buffer (pH = 3). The colored product was first extracted using a mixture of 800 µL acetonitrile and 300 µL chloroform solvents. Then, a spectrophotometric measurement of sediment phase was performed at λ = 420 nm. The important parameters affecting the efficiency of DLLME were optimized. Under the optimum conditions, the calibration graphs of standard -1 (Std.), drug, urine and serum were ranged
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Charge transfer complex formation method has been applied for the spectrophotometric determination of cimetidine, in bulk sample and dosage form. The method was accurate, simple, rapid, inexpensive and sensitive depending on the formed charge- transfer complex between cited drug and, 2,3-Dichloro-5,6-dicyano-p- benzoquinone (DDQ) as a chromogenic reagent. The formed complex shows absorbance maxima at 587 nm against reagent blank. The calibration graph is linear in the ranges of (5.0 - 50.0) µg.mL-1 with detection limit of 0.268µg.mL-1. The results show the absence of interferences from the excipients on the determination of the drug. Therefore the proposed method has been successfully applied for the determination of cimetid
... Show MoreIt is generally accepted that there are two spectrophotometric techniques for quantifying ceftazidime (CFT) in bulk medications and pharmaceutical formulations. The methods are described as simple, sensitive, selective, accurate and efficient techniques. The first method used an alkaline medium to convert ceftazidime to its diazonium salt, which is then combined with the 1-Naphthol (1-NPT) and 2-Naphthol (2-NPT) reagents. The azo dye that was produced brown and red in color with absorption intensities of ƛmax 585 and 545nm respectively. Beer's law was followed in terms of concentration ranging from (3-40) µg .ml-1 For (CFT-1-NPT) and (CFT-2-NPT), the detection limits were 1.0096 and 0.8017 µg.ml-1, respec
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A rapid high sensitive and inexpensive economic method has been developed for the Determination of phenoxazine by using molecular spectrophotometry. The method is based on the oxidation of phenoxazine by potassium (meta)periodate in acidic medium. The oxidation conditions were selected to enhance the sensitivity and the stability of the pink colored species which shows an absorption maximum at 530 nm. The Beer’s law was obeyed for phenoxazine concentration range from 1 to 6 µg mL-1 with 0.003 µg mL-1 detection limit and provided variation coefficients between 0.4 to 1.7 %. This method was successfully applied for the determination of phenoxazine in aqueous samples
A new method for determination of allopurinol in microgram level depending on its ability to reduce the yellow absorption spectrum of (I-3) at maximum wavelength ( ?max 350nm) . The optimum conditions such as "concentration of reactant materials , time of sitting and order of addition were studied to get a high sensitivity ( ? = 27229 l.mole-1.cm-1) sandal sensitivity : 0.0053 µg cm-2 ,with wide range of calibration curve ( 1 – 9 µg.ml-1 ) good stability (more then24 hr.) and repeatability ( RSD % : 2.1 -2.6 % ) , the Recovery % : ( 98.17 – 100.5 % ) , the Erel % ( 0.50 -1.83 % ) and the interference's of Xanthine , Cystein , Creatinine , Urea and the Glucose in 20 , 40 , 60 fold of analyate were also studied .
A spectrophotometric reliable, rapid and sensitive method has been developed and validated for the determination Ketotifen fumarate . A method was described for the determination of Ketotifen Fumarate in pure form or pharmaceutical formulations, a colored ion-pair complex formation reaction among ketotifen fumarate and acid-dye bromophenol blue at pH 3.0 was used for the colorimetric determination of the drug. The complex formed was extracted into chloroform and the maximum absorbance of the solution was measured at 413 nm against blank. The calibration curve calculated obey Beer's law over the concentration range of 0.4-16 μg/ml and the regression equation was A=0.069
... Show MoreIsocratic high performance liquid chromatography on reversed phase a (150x 4.6 mm I.D), 5 ?m ?-Bondapak RP-8 column (with acidic mobile phase allow the separation of doxcycycline hydrochloride with low detection limit of 0.2 µg/ml detected by UV set at 226 nm. The method was validated for Doxycycline between 0.156- to 5 µg/ml. The concentration of doxycycline was assessed in two single dose randomized crossover studies with intervals of one week between two period. In sera of 20 adults healthy male volunteers with average age of (42 + 10) year, body weight 48-85 kg, body height of (160-185cm) after a single dose of doxycycline hydrochoride 100 mg in form of capsules were orally administrated for both formulations. The blood sa
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A 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
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A new simple and sensitive spectrophotometric method for the determination of trace amount of Co(II) in the ethanol absolute solution have been developed. The method is based on the reaction of Co(II) with ethyl cyano(2-methyl carboxylate phenyl azo acetate) (ECA) in acid medium of hydrochloric acid (0.1 M) givining maximum absorbance at ((λmax = 656 nm). Beer's law is obeyed over the concentration range (5-60) (μg / ml) with molar absorptivity of (1.5263 × 103 L mol-1 cm-1) and correlation coefficient (0.9995). The precision (RSD% ˂ 1%). The stoichiometry of complex was confirmed by Job's method which indicated the ratio of metal to reagent is (2:1). The studied effect of interference elements Zn(II), Cu(II), Na(I), K(I), Ca(II) and Mg
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