scholarly journals Utility of σ and π-Acceptors for the Spectrophotometric Determination of Gemifloxacin Mesylate in Pharmaceutical Formulations

2008 ◽  
Vol 5 (3) ◽  
pp. 493-498 ◽  
Author(s):  
Marothu Vamsi Krishna ◽  
Dannana Gowri Sankar

In this study, four simple, fast, accurate and sensitive spectrophotometric methods have been developed for the determination of gemifloxacin mesylate in pharmaceutical formulations. The methods are based on the charge transfer complexation reaction of the drug as n-electron donor with sigma (σ)-acceptor iodine, and thepi(π)-acceptors 2, 3-dichloro-5, 6-dicyano-p-benzoquinone (DDQ)-7,7,8,8-tetra cyanoquinodimethane (TCNQ) and tetracyanoethylene (TCNE). The obtained charge transfer complexes were measured at 290nm for iodine (in 1, 2-dichloro ethane), at 470, 840 and 420 nm for DDQ, TCNQ and TCNE (in acetonitrile), respectively. Optimization of different experimental conditions is described. Beer's law is obeyed in the concentration range of 6-30, 2-10, 2.5-12.5 and 1-5 μg mL−1for iodine, DDQ, TCNQ and TCNE methods, respectively. The proposed methods were applied successfully to the determination of GFX in pharmaceutical formulations with good accuracy and precision.

2010 ◽  
Vol 7 (4) ◽  
pp. 1507-1513 ◽  
Author(s):  
V. Annapurna ◽  
G. Jyothi ◽  
V. Nagalakshmi ◽  
B. B. V. Sailaja

Simple, accurate and reproducible UV spectrophotometric methods were established for the assay of pyrilamine maleate (PYRA) based on the formation of oxidative coupling and precipitation, charge transfer complexation products. Method A includes the oxidative coupling reaction of PYRA with 3-methyl-2-benzathiazolinone hydrazone (MBTH) in presence of Ce(IV). The formation of oxidative coupling product with 4-amino phenazone (4-AP) in presence of K3Fe(CN)6is incorporated in method B. Precipitation/charge transfer complex formation of the PYRA with tannic acid (TA)/Metol-Cr(VI) in method C were proposed. The optical characteristics such as Beers law limits, molar absorptivity and Sandell’s sensitivity for the methods (A-C) are given. Regression analysis using the method of least squares was made to evaluate the slope (b), intercept (a) and correlation coefficient (r) and standard error of estimation (Se) for each system. Determination of pyrilamine in bulk form and in pharmaceutical formulations were also incorporated.


2012 ◽  
Vol 18 (2) ◽  
pp. 263-272 ◽  
Author(s):  
K.B. Vinay ◽  
H.D. Revenasiddappa

Two simple, rapid and accurate spectrophotometric procedures are proposed for the determination of quetiapine fumarate (QTF) in pharmaceuticals and in spiked human urine. The methods are based on charge transfer complexation reactions of free base form of the drug (quetiapine, QTP), as n-electron donor (D), with either p-chloranilic acid (p-CAA) (method A) or 2,3-dichloro-5,6-dicyanoquinone (DDQ) (method B) as ?-acceptors (A). The coloured charge transfer complexes produced exhibit absorption maxima at 520 and 540 nm, in method A and method B, respectively. The experimental conditions such as reagent concentration, reaction solvent and time have been carefully optimized to achieve the maximum sensitivity. Beer?s law is obeyed over the concentration ranges of 8.0 - 160 and 4.0 - 80.0 ?g ml-1, for method A and method B, respectively. The calculated molar absorptivity values are 1.77 ? 103 and 4.59 ? 103 l mol-1cm-1, respectively, for method A and method B. The Sandell sensitivity values, limits of detection (LOD) and quantification (LOQ) have also been reported. The stoichiometry of the reaction in both cases was accomplished adopting the limiting logarithmic method and was found to be 1: 2 (D: A). The accuracy and precision of the methods were evaluated on intra-day and inter-day basis. The proposed methods were successfully applied for the determination of QTF in pharmaceutical formulations and spiked human urine.


2008 ◽  
Vol 3 ◽  
pp. ACI.S643 ◽  
Author(s):  
Nafisur Rahman ◽  
Sk Manirul Haque

Four simple, rapid and sensitive spectrophotometric methods have been proposed for the determination of enalapril maleate in pharmaceutical formulations. The first method is based on the reaction of carboxylic acid group of enalapril maleate with a mixture of potassium iodate (KIO3) and iodide (KI) to form yellow colored product in aqueous medium at 25 ± 1°C. The reaction is followed spectrophotometrically by measuring the absorbance at 352 nm. The second, third and fourth methods are based on the charge transfer complexation reaction of the drug with p-chloranilic acid (pCA) in 1, 4-dioxan-methanol medium, 2, 3-dichloro 5, 6-dicyano 1, 4-benzoquinone (DDQ) in acetonitrile-1,4 dioxane medium and iodine in acetonitrile-dichloromethane medium. Under optimized experimental conditions, Beer's law is obeyed in the concentration ranges of 2.5-50, 20-560, 5-75 and 10-200 µg mL-1, respectively. All the methods have been applied to the determination of enalapril maleate in pharmaceutical dosage forms. Results of analysis are validated statistically.


2009 ◽  
Vol 7 (4) ◽  
pp. 870-875 ◽  
Author(s):  
Sayed Zayed

AbstractTwo simple, rapid, accurate and sensitive spectrophotometric methods are described for the determination of sulpiride. They are based on charge transfer complexation between the drug as n-electron donor and p-chloranilic acid as π acceptor or iodine as σ-acceptor. These give highly coloured complexes with absorption maxima at 518 and 363, 294 nm, respectively. Beer’s law linear ranges were 13.7–341.4 and 1.7–20.5 µg mL−1 for the p-chloranilic acid and iodine methods. The methods were successfully applied to the determination of the drug in Dogmatil® Fort tablets and the results compared with the official method. The complex association constants and standard free energy changes were calculated using Benesi-Hildebrand plots.


2011 ◽  
Vol 17 (4) ◽  
pp. 469-476 ◽  
Author(s):  
Madathil Cijo ◽  
Kanakapura Basavaiah ◽  
Sameer Abdulrahman ◽  
K.B. Vinay

Two simple, accurate, precise, inexpensive, selective and sensitive spectrophotometric methods are described for the determination of repaglinide (RPG) in bulk drug and its tablets. The methods were based on the charge- transfer complex reaction between RPG in acetonitrile with p-chloranilic acid (CAA) or 2,3-dichloro-5,6-dicyano-1,4-benzoquinone (DDQ) in dioxane and subsequent formation of intensely colored radical anions of the reagents which were measured at 520 nm (CAA) or 590 nm (DDQ). Several experimental variables affecting the complex formation, stability of the colored species and sensitivity of the reaction were optimized. Under the optimized conditions, Beer?s law was obeyed over the concentration ranges of 20-400 and 5-80 ?g ml-1 RPG for CAA and DDQ methods, respectively, and the corresponding correlation coefficients were 0.9995 and 0.9998. The apparent molar absorptivity values were 1.02x103 and 4.60x103 for CAA and DDQ methods respectively, with corresponding Sandell sensitivity values of 0.4438 and 0.0984 ?g cm-2. Limits of detection (LOD) were calculated to be 7.07 and 2.42 ?g ml-1 and the limits of quantification (LOQ) were 21.43 and 7.33 ?g ml-1 RPG, for CAA method and DDQ method, respectively. Validation results demonstrated that the inter day and intra day accuracy were up to 97.56%. The precision determined did not exceed 2.5% of RSD. The methods were successfully used for the determination of RPG in tablet form and the results were in good agreement with the label claims as shown by the recoveries which were in the range of 99.22- 102.8% with standard deviation values < 2%. The accuracy of the method was confirmed by recovery studies via standardaddition procedure with excellent recovery 98.24-104.0 ? 1.08-3.35.


2003 ◽  
Vol 86 (1) ◽  
pp. 1-7 ◽  
Author(s):  
Lories I Bebawy ◽  
Yosry M Issa ◽  
Kamal M Abdel Moneim

Abstract Simple, rapid, accurate, and sensitive spectrophotometric methods are described for the determination of dicyclomine hydrochloride. The methods are based on the reaction of this drug as an n-electron donor with 2,3-dichloro-5,6-dicyano-p-benzoqunione (DDQ), p-chloranilic acid (p-CA), and chloranil (CL) as Π-acceptors to give highly colored complex species. The colored products are measured spectrophotometrically at 456, 530, and 650 nm for DDQ, p-CA, and CL, respectively. Optimization of the different experimental conditions were studied. Beer's law was obeyed in concentration ranges of 20–100, 50–250, and 80–600 μg/mL for DDQ, p-CA, and CL, respectively. Colored complexes are produced in organic solvents and are stable for at least 1 h. The methods were applied to Spasmorest™ antispasmotic tablets and ampoules with good accuracy and precision.


2009 ◽  
Vol 6 (s1) ◽  
pp. S397-S405 ◽  
Author(s):  
R. Singh Gujral ◽  
S. Manirul Haque ◽  
P. Shanker

A simple and sensitive spectrophotometric method has been proposed for the determination of flucloxacillin sodium. The determination method is based on charge transfer complexation reaction of the drug with iodine in methanol-dichloromethane medium. The absorbance was measured at 362 nm against the reagent blank. Under optimized experimental conditions, Beer's law is obeyed in the concentration ranges 1-9 μg/mL for flucloxacillin. The method was validated for specificity, linearity, precision, accuracy. The degree of linearity of the calibration curves, the percent recoveries, limit of detection and quantitation for the spectrophotometric method were determined. No interferences could be observed from the additives commonly present in the pharmaceutical formulations. The method was successfully applied forin vitrodetermination of human urine samples with low RSD value. This is simple, specific, accurate and sensitive spectrophotometric method.


2012 ◽  
Vol 2012 ◽  
pp. 1-12 ◽  
Author(s):  
Kudige N. Prashanth ◽  
Kanakapura Basavaiah

Rizatriptan is a new selective 5-HT1B/1D agonist which is used in the treatment of migraine headaches. Two simple, rapid, accurate, and economical spectrophotometric methods are described for the determination of rizatriptan benzoate (RTB) in its pure form and pharmaceutical preparations. These methods are based on the charge-transfer complexation reaction between rizatriptan benzoate as n-electron donor and p-chloranilic acid (p-CA) or 2,3-dichloro-5,6-dicyano-1,4-benzoquinone (DDQ) as π-acceptor to form highly colored chromogens. The chromogens formed by the reaction between RTB and p-CA peaked at 530 nm (method A) and that formed by the reaction between RTB and DDQ peaked at 590 nm (method B). Under the optimum conditions Beer’s law is obeyed in the concentration range of 14–245 μg mL−1 for method A and 4–70 μg mL−1 for method B. The coefficient of correlation was found to be 0.9999 for both methods. The molar absorptivity, Sandell sensitivity, limits of detection, and quantification are also reported. The stoichiometric relationship determined by Job’s continuous method was found to be 1 : 1 (drug : reagent) for both methods. Both methods were applied to determination of RTB in the pharmaceutical formulations. Results of the analysis were validated statistically.


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