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 Validated spectophotometric methods for the assay of cinitapride hydrogen tartrate in pharmaceuticals

2013 ◽  
Vol 19 (2) ◽  
pp. 303-311
Author(s):  
K.V.V. Satyanarayana ◽  
Rao Nageswara
Keyword(s):  
Hydrochloric Acid ◽  
Alkaline Medium ◽  
Sodium Nitrite ◽  
Azo Dyes ◽  
Molar Absorptivity ◽  
Optimum Conditions ◽  
Pharmaceutical Tablets ◽  
Spectrophotometric Methods ◽  
Ich Guidelines

Three simple, selective and rapid spectrophotometric methods have been established for the determination of cinitapride hydrogen tartrate (CHT) in pharmaceutical tablets. The proposed methods are based on the diazotization of CHT with sodium nitrite and hydrochloric acid, followed by coupling with resorcinol, 1-benzoylacetone and 8-hydroxyquinoline in alkaline medium for methods A, B and C respectively. The formed azo dyes are measured at 442, 465 and 552 nm for methods A, B and C respectively. The parameters that affect the reaction were carefully optimized. Under optimum conditions, Beer?s law is obeyed over the ranges 2.0-32.0, 1.0-24.0 and 1.0-20.0 ?g. mL-1 for methods A, B, and C, respectively. The calculated molar absorptivity values are 1.2853 x104, 1.9624 x104 and 3.92 x104 L.mol-1.cm-1 for methods A, B and C, respectively. The results of the proposed procedures were validated statistically according to ICH guidelines. The proposed methods were successfully applied to the determination of CHT in Cintapro tablets without interference from common excipients encountered.

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 SPECTROPHOTOMETRIC METHODS FOR DETERMINATION OF SOFOSBUVIR AND DACLATASVIR IN PURE AND DOSAGE FORMS

2021 ◽  
pp. 112-119
Author(s):  
MONIR Z. SAAD ◽  
ATEF AMER ◽  
KHALED ELGENDY ◽  
BASEM ELGENDY
Keyword(s):  
Indigo Carmine ◽  
Reference Method ◽  
Standard Addition ◽  
Pharmaceutical Formulations ◽  
Molar Absorptivity ◽  
Experimental Conditions ◽  
Fixed Amount ◽  
Alizarin Red ◽  
Spectrophotometric Methods

Objective: Two simple, sensitive and accurate spectrophotometric methods have been developed for the determination of sofosbuvir (SOF) and daclatasvir (DAC) in pure forms and pharmaceutical formulations. Methods: The proposed methods are based on the oxidation of SOF and DAC by a known excess of cerium(IV) ammonium nitrate in sulphuric acid medium followed by determination of unreacted cerium(IV) by adding a fixed amount of indigo carmine (IC) and alizarin red S (ARS) dyes followed by measuring the absorbance at 610 and 360 nm, respectively. The experimental conditions affecting the reaction were studied and optimized. Results: The beer’s law was obeyed in the concentration ranges of 0.2-3.0, 0.2-4.0 for SOF and 0.5-4.5 and 0.5-5.0 μg/ml for DAC using IC and ARS methods, respectively with a correlation coefficient ≥ 0.9991. The calculated molar absorptivity values are 2.354 × 104, 1.933 × 104 for SOF and 1.786 × 104 and 2.015 × 104 L/mol. cm for DAC using IC and ARS methods, respectively u. The limits of detection and quantification are also reported. Intra-day and inter-day precision and accuracy of the methods have been evaluated. Conclusion: The methods were successfully applied to the assay of SOF and DAC in tablets and the results were statistically compared with those of the reference method by applying Student’s t-test and F-test. No interference was observed from the common tablet excipients. The accuracy and reliability of the methods were further ascertained by performing recovery studies using the standard addition method.

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.

Validated Spectrophotometric Determination of Rizatriptan Benzoate in Pharmaceutical Formulations using Alizarin Derivatives

2019 ◽  
Vol 10 (01) ◽  
Author(s):  
El Sheikh R ◽  
Hassan W. S. ◽  
Gouda A. A. ◽  
Al OwairdhiA. ◽  
Al Hassani K K H
Keyword(s):  
Standard Addition ◽  
Pharmaceutical Formulations ◽  
Molar Absorptivity ◽  
Optimum Conditions ◽  
Reaction Conditions ◽  
Alizarin Red ◽  
Rizatriptan Benzoate ◽  
Spectrophotometric Methods ◽  
Relative Standard

Two simple, sensitive, accurate, precise and economical spectrophotometric methods have been developed and validated for the determination of rizatriptan benzoate (RZT) in pure form and pharmaceutical formulations. These methods were based on the formation of charge transfer complex between RZT as n-electron donor and alizarin red S (ARS) or quinalizarin (Quinz) as π-acceptor in methanol to form highly colored chromogens which showed an absorption maximum at 532 and 574 nm using ARS and Quinz, respectively. The optimization of the reaction conditions such as the type of solvent, reagent concentration and reaction time were investigated. Under the optimum conditions, Beer’s law is obeyed in the concentration ranges 1.0-16 and 2.0-20 g mL-1 using ARS and Quinz, respectively with good correlation coefficient (r2 ≥ 0.9996) and with a relative standard deviation (RSD% ≤ 1.16). The molar absorptivity, Sandell sensitivity, detection and quantification limits were also calculated. The methods were successfully applied to the determination of RZT in its pharmaceutical formulations and the validity assesses by applying the standard addition technique. Results obtained by the proposed methods for the pure RZT and commercial tablets agreed well with those obtained by the reported method.

New, simple and validated UV-spectrophotometric methods for the estimation of sodium usnate in preparations

2010 ◽  
Vol 29 (2) ◽  
pp. 157 ◽  
Author(s):  
Ivana Savić ◽  
Goran Nikolić ◽  
Ivan Savić ◽  
Saša Zlatković ◽  
Dragiša Djokić
Keyword(s):  
Phosphate Buffer ◽  
Pharmaceutical Preparations ◽  
High Sensitivity ◽  
Cost Effective ◽  
Sensitivity Coefficient ◽  
Molar Absorptivity ◽  
Spectrophotometric Methods ◽  
Ich Guidelines ◽  
Beer’S Law

New, simple, cost effective, accurate and reproducible UV-spectrophotometric methods were developed and validated for the estimation of sodium usnate in pharmaceutical preparations. Sodium usnate was estimated at 290 nm in water and phosphate buffer (pH 3):methanol (11:20 V/V). Beer’s law was obeyed in the concentration range of 0.1–5 μg·cm−3 (r = 0.997) in water and 1–12 μg·cm−3 (r = 0.999) in the phosphate buffer:methanol. The apparent molar absorptivity and Sandell’s sensitivity coefficient were found to be 3.16×104 dm3·mol−1·cm−1 and 11.58 ng·cm–2/0.001 A in water and 3.72×104 dm3·mol−1·cm−1 and 9.83 ng·cm–2/0.001 A in phosphate buffer:methanol, respectively, indicating the high sensitivity of the proposed methods. These methods were tested and validated for various parameters according to ICH guidelines. The detection and quantitation limits were found to be 0.0721 and 0.2163 μg·cm–3 in water and 0.163, 0.489 μg·cm−3 in phosphate buffer:methanol, respectively. The proposed methods were successfully applied for the determination of sodium usnate in pharmaceutical preparations. The results demonstrated that the procedure is accurate, precise and reproducible (R.S.D. < 2 %).

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 Spectrophotometric study on the charge transfer complex between sumatriptan succinate and some π-acceptors and alizarin derivatives

2013 ◽  
Vol 19 (4) ◽  
pp. 529-540 ◽  
Author(s):  
Sheikh El ◽  
Ayman Gouda ◽  
Rham El-Azzazy
Keyword(s):  
Charge Transfer ◽  
Standard Addition ◽  
Spectrophotometric Study ◽  
Molar Absorptivity ◽  
Charge Transfer Complexes ◽  
Alizarin Red ◽  
Spectrophotometric Methods ◽  
Sumatriptan Succinate ◽  
Relative Standard

A facile, accurate, sensitive and validated spectrophotometric methods for the determination of sumatriptan succinate (SMT) in pure and in dosage forms are described. The methods are based on the formation of charge transfer products between SMT and chromogenic reagents 2,3-dichloro-5,6 dicyano-p-benzoquinone (DDQ), 7,7,8,8-tetracyanoquinodimethane(TCNQ), quinalizarin (Quiz) and alizarin red S (ARS) producing charge transfer complexes which showed an absorption maximum at 461, 841, 567 and 529 nm for DDQ, TCNQ, Quiz and ARS, respectively. The optimization of the reaction conditions such as the type of solvent, reagent concentration and reaction time were investigated. Beer?s law is obeyed in the concentration ranges 1.0-80 mg mL-1. The molar absorptivity, Sandell sensitivity, detection and quantification limits are also calculated. The correlation coefficient was ?0.9994 with a relative standard deviation (R.S.D.) of ? 1.08. The proposed methods were successfully applied for determination of sumatriptan in tablets with good accuracy and precision and without interferences from common additives by applying the standard addition technique. Developed methods have been validated statistically for their accuracy, precision, sensitivity, selectivity, robustness and ruggedness as per ICH guidelines and the results compared favourably with those obtained using the reported method.

scholarly journals Spectrophotometric Determination of Zolmitriptan in Bulk Drug and Pharmaceuticals Using Vanillin as a Reagent

2013 ◽  
Vol 2013 ◽  
pp. 1-7 ◽  
Author(s):  
Kudige N. Prashanth ◽  
Kanakapura Basavaiah ◽  
Madihalli S. Raghu
Keyword(s):  
Reference Method ◽  
Standard Addition ◽  
Molar Absorptivity ◽  
Ich Guidelines ◽  
Red Color ◽  
Reaction Proceeds ◽  
Recovery Study ◽  
Bulk Drug ◽  
Better Than

An accurate and precise spectrophotometric method is presented for the determination of zolmitriptan (ZMT) based on the formation of a red color product with vanillin in presence of concentrated H2SO4, with the chromogen being measured at 580 nm. The reaction proceeds quantitatively at room temperature in 10 min. The calibration curve is linear over the range 5.0–90.0 μg mL−1 and described by the regression equation with a regression coefficient of 0.9994 . The calculated molar absorptivity and Sandell sensitivity values are 3.3 × 103 L mol−1 cm−1 and 0.0872 μg cm−2, respectively. The limits of detection (LOD) and quantification (LOQ) calculated as per ICH guidelines are 1.26 and 3.81 μg mL−1, respectively. The within-day accuracy expressed as relative error was better than 1.78% with precision (RSD) ranging from 0.83 to 1.45%. The between-day accuracy ranged from 1.21 to 1.84% with a precision less than 1.66%. The method was successfully applied to the analysis of one brand of tablet containing zolmitriptan. The results obtained were in agreement with those obtained by published reference method. The accuracy was also checked by placebo blank and synthetic mixture analyses besides recovery study via standard addition procedure.

scholarly journals Application of bromate-bromide mixture as a green brominating agent for the spectrophotometric determination of atenolol in pharmaceuticals

2012 ◽  
Vol 18 (1) ◽  
pp. 43-52 ◽  
Author(s):  
Nagaraj Prashanth ◽  
Kanakapura Basavaiah ◽  
Sameer Abdulrahman ◽  
Nagaraju Rajendraprasad ◽  
Basavaiah Vinay
Keyword(s):  
Reference Method ◽  
Standard Addition ◽  
Pharmaceutical Formulations ◽  
Molar Absorptivity ◽  
Spectrophotometric Methods ◽  
Highly Sensitive ◽  
Bromination Reaction ◽  
Excess Iodide ◽  
Good Agreement

Two highly sensitive spectrophotometric methods are proposed for the quantification of atenolol (ATN) in pure drug as well as in pharmaceutical formulations. The methods are based on the bromination reaction of ATN with a known excess of bromate-bromide mixture in acid medium followed by the determination of unreacted bromine. The residual bromine is determined by its reaction with excess iodide and the liberated iodine (I3?) is either measured at 360 nm (method A) or reacted with starch followed by the measurement of the starch-iodine chromogen at 570 nm (method B). Under the optimum conditions, ATN could be assayed in the concentration ranges of 0.5-9.0 and 0.3-6.0?g mL-1 for method A and method B, respectively, with corresponding molar absorptivity values of 2.36?104 and 2.89?104 L/mol.cm. Sandell?s sensitivity values are found to be 0.0113 and 0.0092 ?g/cm2 for method A and method B, respectively. The proposed methods were successfully applied to the analysis of different commercial brands of pharmaceutical formulations and the results obtained by the proposed methods were in good agreement with those obtained using the reference method. The reliability of the methods was further ascertained by recovery studies using standard- addition method.

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