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 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.

scholarly journals Utility of N-Bromosuccinimide for the Titrimetric and Spectrophotometric Determination of Famotidine in Pharmaceutical Formulations

2011 ◽  
Vol 2011 ◽  
pp. 1-11 ◽  
Author(s):  
O. Zenita ◽  
K. Basavaiah
Keyword(s):  
Indigo Carmine ◽  
Pharmaceutical Formulations ◽  
Neutral Red ◽  
Titration Method ◽  
Fixed Amount ◽  
Indicator Method ◽  
Spectrophotometric Methods ◽  
Back Titration ◽  
Hcl Medium

Two titrimetric and two spectrophotometric methods are described for the assay of famotidine (FMT) in tablets using N-bromosuccinimide (NBS). The first titrimetric method is direct in which FMT is titrated directly with NBS in HCl medium using methyl orange as indicator (method A). The remaining three methods are indirect in which the unreacted NBS is determined after the complete reaction between FMT and NBS by iodometric back titration (method B) or by reacting with a fixed amount of either indigo carmine (method C) or neutral red (method D). The method A and method B are applicable over the range of 2–9 mg and 1–7 mg, respectively. In spectrophotometric methods, Beer's law is obeyed over the concentration ranges of 0.75–6.0 μg mL-1(method C) and 0.3–3.0 μg mL-1(method D). The applicability of the developed methods was demonstrated by the determination of FMT in pure drug as well as in tablets.

scholarly journals Bromatomatric assay of gatifloxacin in pharmaceuticals

2008 ◽  
Vol 14 (3) ◽  
pp. 185-190
Author(s):  
Kanakapura Basavaiah ◽  
Urdigere Kumar ◽  
Kalsang Tharpa
Keyword(s):  
Methyl Orange ◽  
Indigo Carmine ◽  
Pharmaceutical Preparations ◽  
Cost Effective ◽  
Thymol Blue ◽  
Fixed Amount ◽  
Spectrophotometric Methods ◽  
Hydrochloric Acid Medium ◽  
Ich Guidelines

Three new, simple, and cost-effective visible spectrophotometric methods are proposed for determination of gatifloxacin (GTF) using bromate-bromide mixture, and three dyes, methyl orange, indigocarmine and thymol blue, as reagents. The methods engross the addition of a known excess of bromate-bromide mixture to GTF in hydrochloric acid medium followed by determination of residual bromine by reacting with a fixed amount of either methyl orange and measuring the absorbance at 520 nm (method A) or indigo carmine and measuring the absorbance at 610 nm (method B) or thymol blue and measuring the absorbance at 550 nm (method C). In all the methods, the amount of bromine reacted corresponds to the amount of GTF, and the absorbance is found to increase linearly with the concentration of GTF. Under the optimum conditions, GTF could be assayed in the concentration range 0.25-1.5, 0.5-6.0, and 0.5-10 mg/mL by method A, method B and method C, respectively. The apparent molar absorptivities are calculated to be 1.6x105, 4.0x104 and 3.2x104 L mol-1 cm-1 for the method A, method B and method C, respectively, and the corresponding Sandell sensitivity values are 0.0025, 0.010 and 0.012 ?g/cm2. The intra-day and inter-day precision, and the accuracy of the methods were evaluated as per the current ICH guidelines. The methods were successfully applied to the determination of GTF in pharmaceutical preparations without the interference from any of the pharmaceutical adjuvant.

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 Simple Spectrophotometric Methods for the Determination of Zidovudine in Pharmaceuticals Using Chloramine-T, Methylene Blue and Rhodamine-B as Reagents

2006 ◽  
Vol 3 (3) ◽  
pp. 173-181
Author(s):  
K. Basavaiah ◽  
U. R. Anil Kumar
Keyword(s):  
Methylene Blue ◽  
Rhodamine B ◽  
Pharmaceutical Formulations ◽  
Fixed Amount ◽  
Spectrophotometric Methods ◽  
Hydrochloric Acid Medium ◽  
Ich Guidelines ◽  
Chloramine T ◽  
Bulk Drug

Two new spectrophotometric methods are proposed for the determination of zidovudine(ZDV) in pharmaceuticals. The methods use chloramine-T (CAT) and two dyes, methylene blue and rhodamine-B, as reagents and are based on adding of a known excess of CAT to ZDV in hydrochloric acid medium followed by determination of residual oxidant by reacting with a fixed amount of either methylene blue and measuring the absorbance at 665 nm (Method A) or rhodamine B and measuring the absorbance at 555 nm (Method B). In both methods, the amount of CAT reacted corresponds to the amount of ZDV. The absorbance measured is found to increase linearly with concentration of ZDV. Under the optimum conditions, ZDV could be assayed in the concentration range 1.25-15.0 and 0.25-3.0 μg ML-1by method A and method B, respectively. The apparent molar absorptivities are calculated to be 7.7x103and 5.6x104L mol-1cm-1for method A and method B, respectively, and the corresponding Sandell sensitivity values are 0.035 and 0.005 μg cm-2. The limits of detection and quantification are reported for both methods. Intra-day and inter-day precision and accuracy of the developed methods were evaluated as per the current ICH guidelines. The proposed methods can be readily utilized for bulk drug and in pharmaceutical formulations.

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 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.

Colorimetric Determination of Amoxicillin in Pure and some Pharmaceutical Formulations Via Reaction with Potassium Permanganate as Oxidant Reagent

2019 ◽  
Vol 10 (02) ◽  
Author(s):  
Abbas Shebeeb Al-kadumi ◽  
Sahar Rihan Fadhel ◽  
Mohammed Abdullah Ahmed ◽  
Luma Amer Musa
Keyword(s):  
Potassium Permanganate ◽  
Pharmaceutical Preparations ◽  
Pharmaceutical Formulations ◽  
Atomic Emission ◽  
Basic Medium ◽  
Photometric Method ◽  
Colorimetric Determination ◽  
Spectrophotometric Methods ◽  
Label Claim

We proposed two simple, rapid, and convenient spectrophotometric methods are described for the determination of Amoxicillin in bulk and its pharmaceutical preparations. They are based on the measurement of the flame atomic emission of potassium ion (in first method) and colorimetric determination of the green colored solution for manganite ion at 610 nm formed after reaction of Amoxicillin with potassium permanganate as oxidant agent (in the second method) in basic medium. The working conditions of the methods were investigated and optimized. Beer's law plot showed a good correlation in the concentration range of 5-45 μg/ml. The detection limits and relative standared deviations were (2.573, 2.814 μg/ml) (2.137, 2.498) for the flame emission photometric method and (1.844, 2.016 μg/ml) (1.645,1.932) for colorimetric methods for capsules and suspensions respectively. The methods were successfully applied to the determination of Amoxicillin in capsules and suspensions, and the obtained results were in good agreement with the label claim. No interference was observed from the commonly encountered additives and expectancies.

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.

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