scholarly journals Iodimetric assay of olanzapine in pharmaceuticals using iodate and Nile blue as reagents

2009 ◽  
Vol 15 (2) ◽  
pp. 95-102 ◽  
Author(s):  
Kanakapura Basavaiah ◽  
O. Zenita ◽  
Kalsang Tharpa ◽  
Nagaraju Rajendraprasad ◽  
U.R. Anilkumar ◽  
...  
Keyword(s):  
Nile Blue ◽  
Cost Effective ◽  
Molar Absorptivity ◽  
Intermediate Precision ◽  
Experimental Conditions ◽  
Fixed Amount ◽  
Label Claim ◽  
Bulk Drug ◽  
Student’S T

A simple, selective and cost effective spectrophotometric method has been described for the determination of olanzapine (OLP) in bulk drug and in tablets. The method involves treating OLP with an excess of iodate in acid medium followed by the determination of liberated iodine by reacting with a fixed amount of Nile blue and measuring the absorbance at 400 nm. In this method, the amount of iodine reacted corresponds to the OLP concentration. The experimental conditions for the assay have been optimized and the absorbance is found to increase linearly with the concentration of OLP (r = 0.997). Beer's law is obeyed over the range 15-120 ?g mL-1. The calculated molar absorptivity and Sandell sensitivity values are 0.657?103 l mol-1 cm-1 and 0.475 ?g cm-2, respectively. The limits of detection (LOD) and quantification (LOQ) are 3.93 and 11.90 ?g ml-1. The performance of the method was validated according to the present ICH guidelines. The repeatability and intermediate precision, expressed by the RSD was better than 3%. The accuracy of the method expressed as relative error was satisfactory. The proposed method was applied to the analysis of tablet form of OLP and the results tallied well with the label claim. No interference was observed from concomitant substances normally added to tablets. The results were statistically compared with those of a literature method by applying the Student's t-test and F-test. The accuracy and validity of the method were further ascertained by performing recovery studies via spike method.

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 SENSITIVE SPECTROPHOTOMETRIC ASSAY OF MUSCARINIC RECEPTOR ANTAGONIST TOLTERODINE TARTRATE IN BULK DRUG AND PHARMACEUTICAL FORMULATIONS

2017 ◽  
Vol 10 (8) ◽  
pp. 346
Author(s):  
Ragaa El-sheikh ◽  
Wafaa S Hassan ◽  
Ayman A Gouda ◽  
Marwa M El-gabry
Keyword(s):  
Standard Addition ◽  
Pharmaceutical Formulations ◽  
Molar Absorptivity ◽  
Experimental Conditions ◽  
Fixed Amount ◽  
Spectrophotometric Methods ◽  
Accuracy And Precision ◽  
Tolterodine Tartrate ◽  
Bulk Drug ◽  
Student’S T

Objective: Simple, sensitive, and accurate spectrophotometric methods have been developed for the assay of tolterodine tartrate (TOL) in bulk drugand pharmaceutical formulations.Methods: The proposed methods are based on oxidation reaction of TOL with a known excess of cerium(IV) ammonium sulfate as an oxidizing agentin acid medium followed by determination of unreacted oxidant by adding a fixed amount of dye, e.g., amaranth (AM), rhodamine 6G (Rh6G), andindigo carmine (IC) followed by measuring the absorbance at 520, 530, and 610 nm, respectively. The effect of experimental conditions was studiedand optimized.Results: The Beer’s law was obeyed in the concentration ranges of 1.0-10, 1.0-12, and 0.5-9.0 μg/mL using AM, Rh6G, and IC dyes, respectively, witha correlation coefficient ≥0.9995. The calculated molar absorptivity values are 1.868×104, 1.008×104, and 1.623×104 L/mol/cm using AM, Rh6G, andIC dyes, respectively. The limits of detection and quantification were reported. Intraday and interday accuracy and precision of the methods have beenevaluated. No interference was observed from the additives.Conclusion: The proposed methods were successfully applied to the assay of TOL in tablets preparations, and the results were statistically comparedwith those of the reported method by applying Student’s t-test and F-test. The reliability of the methods was further ascertained by performingrecovery studies using the standard addition method.

scholarly journals Sensitive Bromatometric Methods for the Determination of Sumatriptan Succinate in Pharmaceutical Formulations

2011 ◽  
Vol 8 (1) ◽  
pp. 269-275 ◽  
Author(s):  
K. V. V. Satyanarayana ◽  
P. Nageswara Rao
Keyword(s):  
Indigo Carmine ◽  
Pharmaceutical Formulations ◽  
Molar Absorptivity ◽  
Experimental Conditions ◽  
Fixed Amount ◽  
Spectrophotometric Methods ◽  
Sumatriptan Succinate ◽  
Ich Guidelines ◽  
Label Claim

Two simple and sensitive spectrophotometric methods are described for the determination of sumatriptan succinate (STS) in pure and tablets using bromate-bromide as the bromination reagent in acid medium and two dyes as subsidiary reagents. The two methods are based on the bromination of STS by a known excess ofin situgenerated bromine followed by determination of unreacted bromine by reacting with a fixed amount of methyl orange (Method A) or indigo carmine (Method B) and measuring the absorbance at 508 or 610 nm. In both methods, the amount of bromine reacted corresponds to the amount of STS. The experimental conditions for the assay have been optimized. In two methods, the absorbance was found to increase linearly with the concentration of STS at the respective wavelengths. Beer’s law was obeyed over the ranges 0.2-1.6 and 2.0-12.0 μg mL-1for method A and method B respectively and the respective molar absorptivity values were 1.898×105and 2.71×104L mol-1cm-1. The statistical analysis of the methods was validated according to the present ICH guidelines. The proposed methods were applied to the analysis of tablet form of STS and the results tallied well with the label claim.

scholarly journals Spectrophotometric Determination of Zidovudine in Pharmaceuticals Based on Charge-Transfer Complexation Involving N-Bromosuccinimide, Metol and Sulphanilic Acid as Reagents

2007 ◽  
Vol 4 (2) ◽  
pp. 173-179 ◽  
Author(s):  
K. Basavaiah ◽  
U. R. Anil Kumar
Keyword(s):  
Limit Of Detection ◽  
Pharmaceutical Preparations ◽  
Reference Method ◽  
Standard Addition ◽  
Molar Absorptivity ◽  
Sulphanilic Acid ◽  
Bulk Drug ◽  
Student’S T ◽  
Charge Transfer Complexation

A simple spectrophotometric method is proposed for the determination of zidovudine(ZDV) in bulk drug and in pharmaceutical preparations. The method is based on the oxidation of ZDV by a known excess of oxidant N-bromosuccinimide (NBS), in buffer medium of pH 1.5, followed by the estimation of unreacted amount of oxidant with metol and sulphanilic acid. The reacted oxidant corresponds to the amount ZDV. The purple-red reaction product absorbs maximally at 530 nm and Beer’s law is obeyed over a range 5 to 75 μg mL-1. The apparent molar absorptivity is calculated to be 5.1×103L mol-1cm-1, and the corresponding Sandell sensitivity value is 0.052 μg cm-2. The limit of detection and quantification are found to be 0.90 and 2.72, respectively. Intra-day and inter-day precision and accuracy of the developed methods were evaluated as per the current ICH guidelines. The method was successfully applied to the assay of ZDV in tablet/capsule preparations 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 tablet/capsule excipients. The accuracy of the method was further ascertained by performing recovery studies via standard-addition method.

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 NEW REAGENTS FOR THE SPECTROPHOTOMETRIC DETERMINATION OF RANITIDINE HYDROCHLORIDE

2018 ◽  
Vol 35 (3) ◽  
pp. 109
Author(s):  
Badiadka Narayana ◽  
K. Veena ◽  
K. Ashwani ◽  
Divya N. Shetty
Keyword(s):  
Ammonium Sulphate ◽  
Crystal Violet ◽  
Spectrophotometric Method ◽  
Molar Absorptivity ◽  
Dosage Forms ◽  
Reagent Blank ◽  
Fixed Amount ◽  
Ranitidine Hydrochloride ◽  
Bulk Drug

A new spectrophotometric method is proposed for the assay of ranitidine hydrochloride (RNH) in bulk drug and in its dosage forms using ceric ammonium sulphate (CAS) and two dyes, malachite (MAG) green and crystal violet (CV) as reagents. The method involves the addition of a known excess of ceric ammonium sulphate to ranitidine hydrochloride in acid medium, followed by the determination of unreacted CAS by reacting with a fixed amount of malachite green or crystal violet and measuring the absorbance at 615 or 582 nm respectively against the reagent blank. The Beer’s law is obeyed in the concentration range of 0.4-8.0 μg/ml of ranitidine hydrochloride (RNH) for RNH-MAG system and 0.2-1.6μg/ml of ranitidine hydrochloride for RNH-CV system. The molar Absorptivity, Sandell’s sensitivity for each system were calculated. The method has been successfully applied to the determination of ranitidine hydrochloride in pure and dosage forms.

scholarly journals Simple Spectrophotometric Determination of Torsemide in Bulk Drug and in Formulations

2008 ◽  
Vol 5 (3) ◽  
pp. 473-478 ◽  
Author(s):  
Marothu Vamsi Krishna ◽  
Dannana Gowri Sankar
Keyword(s):  
Limit Of Detection ◽  
Regression Line ◽  
Cost Effective ◽  
Pharmaceutical Formulations ◽  
High Accuracy ◽  
Molar Absorptivity ◽  
Good Precision ◽  
Experimental Parameters ◽  
Bulk Drug

A simple and cost effective spectrophotometric method is described for the determination of torsemide in pure form and in pharmaceutical formulations. The method is based on the formation of blue colored chromogen when the drug reacts with Folin-Ciocalteu (F-C) reagent in alkaline medium. The colored species has an absorption maximum at 760 nm and obeys beer's law in the concentration range 30 – 150 ug mL−1. The absorbance was found to increase linearly with increasing concentration of TSM, which is corroborated by the calculated correlation coefficient value of 0.9999 (n=8). The apparent molar absorptivity and sandell sensitivity were 1.896×103L mol−1cm−1and 0.183 μg cm−2, respectively. The slope and intercept of the equation of the regression line are 5.4x10−3and 1.00×10−4respectively. The limit of detection was 0.94.The optimum experimental parameters for the reaction have been studied. The validity of the described procedure was assessed. Statistical analysis of the results has been carried out revealing high accuracy and good precision. The proposed method was successfully applied to the determination of TSM in pharmaceutical formulations.

Simple and Selective Titrimetric and Spectrophotometric Methods for the Determination of Loratadine Using Bromate-Bromide, Methyl Orange and Methylene Blue

2018 ◽  
Vol 9 (2) ◽  
Author(s):  
Venkatachalam K ◽  
Niranjani S ◽  
Raju T
Keyword(s):  
Methylene Blue ◽  
Methyl Orange ◽  
Reference Method ◽  
Standard Addition ◽  
Molar Absorptivity ◽  
Stoichiometric Ratio ◽  
Fixed Amount ◽  
Spectrophotometric Methods ◽  
Student’S T

One indirect titrimetric and two indirect visible spectrophotometric methods were described for the determination of loratadine in bulk drug and in its formulations. The methods used bromate-bromide, methyl orange and methylene blue as reagents. In titrimetry (method A), loratadine was treated with a known excess of bromate-bromide mixture in acidic medium and the residual bromine was back titrated iodometrically after the reaction between loratadine and in situ bromine was ensured to be complete. In spectrophotometric methods, the excess of bromine was estimated by treating with a fixed amount of either methyl orange (method B) and measuring the absorbance at 520 nm or methylene blue (method C) and measuring the absorbance at 680 nm. In all the methods, the amount of reacted bromine corresponded to the loratadine content. Titrimetric method was applicable over 1-8 mg range and the calculations were based on a 1:0.666 (loratadine:bromate) stoichiometric ratio. In spectrophotometry, the calibration graphs were found to be linear over 150- 350 and 1.75-3.5 μg mL-1 for method B and method C, respectively, with corresponding molar absorptivity values of 9.15 × 102 and 1.10 × 105 L mol-1 cm-1. Accuracy and precision of the assays were determined by computing the intra-day and inter-day variations at three different levels of loratadine. The methods were successfully applied to the assay of loratadine in tablet preparations and the results were compared with those of a reference method by applying Student’s t and F-tests. No interference was observed from common pharmaceutical excipients. The reliability of the methods was further ascertained by performing recovery tests by standard addition method

scholarly journals Titrimetric and spectrophotometric determination of doxycycline hyclate using bromate-bromide, methyl orange and indigo carmine

2010 ◽  
Vol 16 (2) ◽  
pp. 139-148 ◽  
Author(s):  
Jagannathamurthy Ramesh ◽  
Kanakapura Basavaiah ◽  
Ranganath Divya ◽  
Nagaraju Rajendraprasad ◽  
Basavaiah Vinay
Keyword(s):  
Methyl Orange ◽  
Indigo Carmine ◽  
Molar Absorptivity ◽  
Stoichiometric Ratio ◽  
Doxycycline Hyclate ◽  
Fixed Amount ◽  
Spectrophotometric Methods ◽  
Accuracy And Precision ◽  
Bulk Drug

One titrimetric and two indirect spectrophotometric methods are described for the determination of doxycycline hyclate (DCH) in bulk drug and in its formulations. The methods use bromate-bromide, methyl orange and indigo carmine as reagents. In titrimetry (method A), DCH is treated with a known excess of bromate-bromide mixture in acid medium and the residual bromine is back titrated iodometrically after the reaction between DCH and in situ bromine is ensured to be complete. In spectrophotometric methods, the excess of bromine is estimated by treating with a fixed amount of either methyl orange (method B) or indigo carmine (method C) and measuring the change in absorbance either at 520 or 610 nm. Titrimetric method is applicable over 1-8 mg range and the calculations are based on a 1:2 (DCH:bromate) stoichiometric ratio. In spectrophotometry, the calibration graphs were found to be linear over 0.25-1.25 and 1-5 ?g mL-1 for method B and method C, respectively, with corresponding molar absorptivity values of 2.62 ?105 and 6.97 ? 104 L mol-1 cm-1. Accuracy and precision of the assays were determined by computing the intra-day and inter-day variations at three different levels of DCH.

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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