scholarly journals Permanganometric determination of etamsylate in bulk drug and in tablets

2009 ◽  
Vol 15 (3) ◽  
pp. 149-157 ◽  
Author(s):  
K.B. Vinay ◽  
H.D. Revanasiddappa ◽  
Zenita Okram ◽  
Kanakapura Basavaiah
Keyword(s):  
Molar Absorptivity ◽  
Molar Ratio ◽  
Spectrophotometric Methods ◽  
Fixed Concentration ◽  
Bluish Green ◽  
Bulk Drug ◽  
Direct Spectrophotometry ◽  
Assay Conditions ◽  
Drug Solution

One titrimetric and two spectrophotometric methods which are simple, selective, sensitive, accurate, precise and economical for the determination of etamsylate (ETM) in bulk drug and in tablets employing permanganate as the oxidimetric reagent are described. In titrimetry, ETM is titrated directly with permanganate in sulphuric acid medium. A direct spectrophotometry (method A) involves treating the aqueous solution of the drug with permanganate in alkaline medium and measuring the bluish green product at 610 nm. In indirect spectrophotometry (method B), the drug solution was treated with a fixed concentration of permanganate in H2SO4 medium, and after a specified time, the unreacted permanganate was measured at 545 nm. The molar combining ratio in titrimetry and the optimum assay conditions were studied. Titrimetry is applicable over 1-10 mg range and the calculations are based on a 1:4 (ETM:KMnO4) molar ratio. In spectrophotometry, Beer's law is obeyed over 0.5- 5.0 and 1.5-15 ?g ml-1 for method A and B, respectively. The molar absorptivity values are calculated to be 2.79?104 and 4.17?104 l mol-1 cm-1 for method A and B, respectively and the corresponding sandell sensitivity values are 0.0094 and 0.0063 ?g cm-2. The limits of detection (LOD) and quantification (LOQ) are also reported for spectrophotometric methods. The applicability of the developed methods was demonstrated by the determination of etamsylate in pure drug as well as in commercial dosage forms.

scholarly journals Application of Oxidizing Properties of Permanganate to the Determination of Famotidine in Pharmaceutical Formulations

2019 ◽  
Vol 54 (4) ◽  
Author(s):  
Kanakapura Basavaiah ◽  
Okram Zenita Devi
Keyword(s):  
Pharmaceutical Formulations ◽  
Molar Absorptivity ◽  
Alkaline Media ◽  
Molar Ratio ◽  
Spectrophotometric Methods ◽  
Fixed Concentration ◽  
Bluish Green ◽  
Direct Spectrophotometry ◽  
Assay Conditions

One titrimetric and two spectrophotometric methods are described for the determination of famotidine (FMT) in either pure form or in its pharmaceutical formulations. The methods are based on redox reaction between FMT and KMnO4 in acid and alkaline media. In titrimetry, an acidified solution of FMT is titrated directly with permanganate. Direct spectrophotometry (method A) involves treating the alkaline solution of the drug with permanganate and measuring the bluish green product at 610 nm. In indirect spectrophotometry (method B), the drug solution is treated with a fixed concentration of permanganate in H2SO4 medium, and after a specified time, the unreacted permanganate is measured at 545 nm. The molar combining ratio in titrimetry and the optimum assay conditions are studied. Titrimetry is applicable over 1-10 mg range and the calculations are based on a 1:3 (FMT: KMnO4) molar-ratio. In spectrophotometry, Beer’s law is obeyed over 0.75-7.5 and 2.5-20 μg mL-1 for method A and method B, respectively. The molar absorptivity values are calculated to be 2.79 Å~ 104 and 1.62 Å~ 104 L mol-1 cm-1 for method A and method B, respectively, and the corresponding Sandell sensitivity values are 0.012 and 0.021 μg cm-2. The limits of detection (LOD) and quantification (LOQ) are also reported for the spectrophotometric methods. The applicability of the developed methods was demonstrated by the determination of FMT in pure drug as well as in commercial dosage forms

scholarly journals Cerimetric determination of simvastatin in pharmaceuticals based on redox and complex formation reactions

2018 ◽  
Vol 33 (2) ◽  
pp. 21
Author(s):  
Kanakapura Basavaiah ◽  
Okram Zenita Devi
Keyword(s):  
Limit Of Detection ◽  
Reference Method ◽  
Standard Addition ◽  
Molar Absorptivity ◽  
Experimental Conditions ◽  
Spectrophotometric Methods ◽  
Fixed Quantity ◽  
Bulk Drug ◽  
Student’S T

Two sensitive spectrophotometric methods are described for the determination of simvastatin (SMT) in bulk drug and in tablets. The methods are based on the oxidation of SMT by a measured excess of cerium (IV) in acid medium followed by determination of unreacted oxidant by two different reaction schemes. In one procedure (method A), the residual cerium (IV) is reacted with a fixed concentration of ferroin and the increase in absorbance is measured at 510 nm. The second approach (method B) involves thereduction of the unreacted cerium (IV) with a fixed quantity of iron (II), and the resulting iron (III) is complexed with thiocyanate and the absorbance measured at 470 nm. In both methods, the amount of cerium (IV) reacted corresponds to SMT concentration. The experimental conditions for both methods were optimized. In method A, the absorbance is found to increase linearly with SMT concentration (r = 0.9995) whereas in method B, the same decreased (r = -0.9943). The systems obey Beer’s law for 0.6-7.5 and 0.5-5.0 μg mL-1 for method A and method B, respectively. The calculated molar absorptivity values are 2.7 X 104 and 1.06 X 105 Lmol-1 cm-1, respectively; and the corresponding sandel sensitivity values are 0.0153 and 0.0039μg cm-2, respectively. The limit of detection (LOD) and quantification (LOQ) are reported for both methods. Intra-day and inter-day precision, and accuracy of the methods were established as per the current ICH guidelines. The methods were successfully applied to the determination of SMT in tablets and the results were statistically compared with those of the reference method by applying the Student’s t-test and F-test. No interference was observed from the common excipients added to tablets. The accuracy and validity of the methods were further ascertained by performing recovery experiments via standard addition procedure.

scholarly journals Spectrophometric Determination of Nelfinavir Mesylate

2006 ◽  
Vol 3 (2) ◽  
pp. 78-82 ◽  
Author(s):  
K. Vanitha Prakash ◽  
Jangala Venkateswara Rao
Keyword(s):  
Ferric Chloride ◽  
Dosage Form ◽  
Potassium Ferricyanide ◽  
Reagent Blank ◽  
Spectrophotometric Methods ◽  
Bluish Green ◽  
Nelfinavir Mesylate ◽  
Bulk Drug ◽  
Tablet Dosage

Two new simple, sensitive, rapid and economical Spectrophotometric Methods (A and B) have been developed for the determination of Nelfinavir Mesylate in pharmaceutical bulk and tablet dosage form. The method A is based on the reaction of Nelfinavir with ferric chloride, potassium ferricyanide and hydrochloric acid to form a bluish green colored chromogen. The Method B is based on the formation of blood red colored chromogen with Ferric chloride and 1,10-phenanthroline. The absorbances of the chromogen were measured at their respective wavelength of maximum absorbance against the corresponding reagent blank. The proposed methods have been successfully applied to the analysis of the bulk drug and its tablet dosage form. The methods have been statistically evaluated and were found to be precise and accurate.

scholarly journals Application of Cerium (IV) as an Oxidimetric Agent for the Determination of Ethionamide in Pharmaceutical Formulations

2016 ◽  
Vol 2016 ◽  
pp. 1-9 ◽  
Author(s):  
Kanakapura Basavaiah ◽  
Nagib A. S. Qarah ◽  
Sameer A. M. Abdulrahman
Keyword(s):  
Quality Control ◽  
Pharmaceutical Formulations ◽  
Molar Absorptivity ◽  
Sample Solution ◽  
Standing Time ◽  
Spectrophotometric Methods ◽  
Ich Guidelines ◽  
Back Titration ◽  
Bulk Drug

Two simple methods are described for the determination of ethionamide (ETM) in bulk drug and tablets using cerium (IV) sulphate as the oxidimetric agent. In both methods, the sample solution is treated with a measured excess of cerium (IV) solution in H2SO4 medium, and after a fixed standing time, the residual oxidant is determined either by back titration with standard iron (II) solution to a ferroin end point in titrimetry or by reacting with o-dianisidine followed by measurement of the absorbance of the orange-red coloured product at 470 nm in spectrophotometry. In titrimetry, the reaction proceeded with a stoichiometry of 1 : 2 (ETM : Ce (IV)) and the amount of cerium (IV) consumed by ETM was related to the latter’s amount, and the method was applicable over 1.0–8.0 mg of drug. In spectrophotometry, Beer’s law was obeyed over the concentration range of 0.5–5.0 μg/mL ETM with a molar absorptivity value of 2.66 × 104 L/(mol·cm). The limits of detection (LOD) and quantification (LOQ) calculated according to ICH guidelines were 0.013 and 0.043 μg/mL, respectively. The proposed titrimetric and spectrophotometric methods were found to yield reliable results when applied to bulk drug and tablets analysis, and hence they can be applied in quality control laboratories.

scholarly journals Spectrophotometric determination of repaglinide in tablets based on charge-transfer complexation reaction with chloranilic acid and dichloro-dicyano benzoquinone

2011 ◽  
Vol 17 (4) ◽  
pp. 469-476 ◽  
Author(s):  
Madathil Cijo ◽  
Kanakapura Basavaiah ◽  
Sameer Abdulrahman ◽  
K.B. Vinay
Keyword(s):  
Charge Transfer ◽  
Correlation Coefficients ◽  
Molar Absorptivity ◽  
Complexation Reaction ◽  
Chloranilic Acid ◽  
Subsequent Formation ◽  
Spectrophotometric Methods ◽  
Bulk Drug ◽  
Charge Transfer Complexation

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.

scholarly journals Spectroscopic Determination of Two Beta-Blockers – Atenolol and Propanolol by Oxidative Derivatization Using Potassium Permanganate in Alkaline Medium

2020 ◽  
Vol 39 (1) ◽  
pp. 56-64
Author(s):  
Edebi N. Vaikosen ◽  
Jeniffer Bioghele ◽  
Ruth C. Worlu ◽  
Benjamin U. Ebeshi
Keyword(s):  
Alkaline Medium ◽  
Beta Blockers ◽  
Molar Absorptivity ◽  
Pharmaceutical Dosage Forms ◽  
Bluish Green ◽  
Relative Standard ◽  
Colour Changes ◽  
Tablet Formulations ◽  
Assay Conditions

AbstractA simple, rapid, sensitive, cheap and accurate oxidative method for two beta-blockers in pharmaceutical dosage forms was developed and evaluated. The method involved the oxidimetric treatment of atenolol and propanolol with 2 x 10-3 mol L-1 KMnO4 in alkaline medium (pH ≥ 9). Scanned spectra of oxidized complex showed distinctive absorptions at 460, 520, 540 and 570 nm. Arrays of colour changes were observed - from violet to blue; blue to bluish-green and yellow. Exhibited colours were due to ligand-metal charge transfer. An indirect spectrophotometric determination of atenolol and propranolol was done after 12-15 minutes at 520 nm. The optimum assay conditions showed linearity ranged from 0 – 15.0 μg mL-1 for both beta-blockers (R= 0.9997 – 0.9999). Molar absorptivity values were 4.79 x 103 and 4.88 x 103 L mol-1 cm-1 for atenolol and propanolol respectively, with corresponding Sandell’s sensitivity values of 0.056 and 0.053 μg cm-2. Limits of detection and quantification were 0.50 and 1.65 μg mL-1 for atenolol respectively and 0.58 and 1.91 μg mL-1 for propanolol, while relative standard deviation for intra-and inter-day precision were < 2.0%. The applicability, accuracy and reliability of the method were demonstrated by the determination of atenolol and propanolol in tablet formulations. The recovery studies ranged from 93.33 - 103.00% for both beta-blockers and the amounts in brands were from 97.53 ± 2.68 to 100.84 ± 1.82%.

scholarly journals Titrimetric and spectrophotometric assay of diethylcarbamazine citrate in formulations using iodate and iodide mixture as reagents

2015 ◽  
Vol 51 (1) ◽  
pp. 43-52 ◽  
Author(s):  
Nagaraju Swamy ◽  
Kudige Nagaraj Prashanth ◽  
Kanakapura Basavaiah
Keyword(s):  
Molar Absorptivity ◽  
Potassium Iodate ◽  
Spectrophotometric Methods ◽  
Accuracy And Precision ◽  
Ich Guidelines ◽  
Diethylcarbamazine Citrate ◽  
Back Titration ◽  
Bulk Drug ◽  
Reaction Stoichiometry

One titrimetric and two spectrophotometric methods are proposed for the determination of diethylcarbamazine citrate (DEC) in bulk drug and in formulations using potassium iodate and potassium iodide as reagent. The methods employ the well-known analytical reaction between iodate and iodide in the presence of acid. In titrimetry (method A), the drug was treated with a measured excess of thiosulfate in the presence of unmeasured excess of iodate-iodide mixture and after a standing time of 10 min, the surplus thiosulfate was determined by back titration with iodine towards starch end point. Titrimetric assay is based on a 1:3 reaction stoichiometry between DEC and iodine and the method is applicable over 2.0-10.0 mg range. The liberated iodine is measured spectrophotometrically at 370 nm (method B) or the iodine-starch complex measured at 570 nm (method C). In both methods, the absorbance is found to be linearly dependent on the concentration of iodine, which in turn is related to DEC concentration. The calibration curves are linear over 2.5-50 and 2.5-30 µg mL-1 DEC for method B and method C, respectively. The calculated molar absorptivity and Sandell sensitivity values were 6.48×103 L mol-1 cm-1 and 0.0604 µg cm-2, respectively, for method B, and their respective values for method C are 9.96×103 L mol-1 cm-1 and 0.0393 µg cm-2. The intra-day and inter-day accuracy and precision studies were carried out according to the ICH guidelines. The methods were successfully applied to the analysis of DEC formulations.

scholarly journals Determination of olanzapine by spectrophotometry using permanganate

2009 ◽  
Vol 45 (3) ◽  
pp. 539-550 ◽  
Author(s):  
Nagaraju Rajendraprasad ◽  
Kanakapura Basavaiah
Keyword(s):  
Alkaline Medium ◽  
Standard Addition ◽  
Molar Absorptivity ◽  
Intermediate Precision ◽  
Green Color ◽  
Spectrophotometric Methods ◽  
Ich Guidelines ◽  
Bluish Green ◽  
Optimized Conditions

Two new spectrophotometric methods using permanganate as the oxidimetric reagent for the determination of olanzapine (OLP) were developed and validated as per the current ICH guidelines. The methods involved the addition of known excess of permanganate to OLP in either acid or alkaline medium followed by the determination of unreacted permanganate at 550 nm (method A) or bluish-green color of manganate at 610 nm (method B). The decrease in absorbance in method A or increase in absorbance in method B as a function of concentration of OLP was measured and related to OLP concentration. Under optimized conditions, Beer's law was obeyed over the ranges 2.0 to 20 and 1.0 to 10 μg mL-1 in method A and method B, respectively. The calculated molar absorptivity values were 1.34 x 10(4) and 2.54 x 10(4) l mol-1cm-1 for method A and method B respectively, and the respective Sandell sensitivities were 0.0233 and 0.0123 μg cm-2. The LOD and LOQ for method A were calculated to be 0.37 and 1.13 μg mL-1and the corresponding values for method B were 0.16 and 0.48 μg mL-1. Intermediate precision, expressed as RSD was in the range 0.51 to 2.66 %, and accuracy, expressed as relative error ranged from 0.79 to 2.24 %. The proposed methods were successfully applied to the assay of OLP in commercial tablets with mean percentage recoveries of 102 ±1.59 % (method A) and 101 ±1.53 % (method B). The accuracy and reliability of the methods were further confirmed by performing recovery tests via standard addition procedure.

scholarly journals Sensitive Spectrophotometric Determination of Lamotrigine in Bulk Drug and Pharmaceutical Formulations using Bromocresol Green

2018 ◽  
Vol 35 (1) ◽  
pp. 55
Author(s):  
N. Rajendraprasad ◽  
K. Basavaiah ◽  
K. B. Vinay
Keyword(s):  
Potassium Hydroxide ◽  
Pharmaceutical Formulations ◽  
Molar Absorptivity ◽  
Ion Pair ◽  
Bromocresol Green ◽  
Spectrophotometric Methods ◽  
Base Form ◽  
Bulk Drug ◽  
The Stability

Two new, simple, rapid and reproducible spectrophotometric methods have been developed for the determination of lamotrigine (LMT) both in pure form and in its tablets. The first method (method A) is based on the formation of a colored ion-pair complex (1:1 drug/dye) of LMT with bromocresol green (BCG) at pH 5.02±0.01 and extraction of the complex into dichloromethane followed by the measurement of the yellow ion-pair complex at 410 nm. In the second (method B), the drug-dye ion-pair complex was dissolved in ethanolic potassium hydroxide and the resulting base form of the dye was measured at 620 nm. Beer’s law was obeyed in the concentration range of 1.5-15 μg mL-1 and 0.5-5.0 μg mL-1 for method A and method B, respectively, and the  = corresponding molar absorptivity values are 1.6932 x 104 and 3.748 x 104L mol-1cm-1. The Sandell sensitivity values are 0.0151 and 0.0068 μg cm-2 for method A and method B, respectively. The stoichiometry of the ion-pair complex formed between the dug and dye (1:1) was determined by Job’s continuous variations method and the stability constant of the complex was also calculated. The proposed methods were applied successfully for the determination of drug in commercial tablets.

scholarly journals Simple and rapid spectrophotometric assay of albendazole in pharmaceuticals using iodine and picric acid as CT complexing agents

2014 ◽  
Vol 50 (4) ◽  
pp. 839-850 ◽  
Author(s):  
Nagaraju Swamy ◽  
Kanakapura Basavaiah
Keyword(s):  
Picric Acid ◽  
Molar Absorptivity ◽  
Complexing Agents ◽  
Complexation Reaction ◽  
Experimental Conditions ◽  
Spectrophotometric Methods ◽  
Bulk Drug ◽  
Ct Complexes ◽  
Acceptor Method

Two simple, rapid and inexpensive spectrophotometric methods are described for the determination of albendazole (ALB) in bulk drug and in tablets. The methods are based on charge-transfer (CT) complexation reaction involving ALB as n-donor and iodine as σ-acceptor (method A) in dichloromethane or picric acid (PA) as π-acceptor (method B) in chloroform. The absorbance of CT complexes was measured at 380 nm for method A, and 415 nm for method B. The optimization of the experimental conditions is described. Under optimum conditions, Beer's law obeyed over the concentration ranges 8.0-240 and 2.4-42 μg mL-1 for method A and method B, respectively. The apparent molar absorptivity of CT complexes at the respective λmax are calculated to be 1.17×103 and 5.22×103 L mol-1cm-1 respectively, and the corresponding Sandell sensitivity values are 0.2273 and 0.0509 ng cm-2. The limits of detection (LOD) and quantification (LOQ) are calculated to be (0.69 and 2.08), and (0.10 and 0.30) μg mL-1 with method A, and method B, respectively. The intra-day and inter-day accuracy expressed as % RE and precision expressed as % RSD were less than 3%. The methods were applied to the determination of ALB in tablets.

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