scholarly journals Spectrophotometric Determination of Reboxetine through Condensation and Diazo-Coupling Reactions

2011 ◽  
Vol 8 (1) ◽  
pp. 281-287 ◽  
Author(s):  
K. Srikanth ◽  
K. A. Emmanuel

In the present study, two simple, sensitive and reproducible visible spectrophotometric methods were developed for the determination of reboxetine in pure form and in pharmaceutical formulations. The methods involve acid hydrolysis of reboxetine methane sulphonate (Reboxetine as methane sulphonate) and the product obtained was used for the estimation. Out of the two methods developed in the laboratory, the first method involves the condensation reaction of hydrolysed reboxetine methane sulphonate with ethyl acetoacetate in sulphuric acid medium and the second method involves the diazocoupling reaction of hydrolysed reboxetine methane sulphonate with diazotizedp-sulphanilic acid in alkaline medium. They have absorption maxima at 400 nm and 430 nm respectively and obey Beer’s law in the concentration ranges of 0.5 - 0.3 μgmL-1and 1.0 - 7.5 μgmL-1respectively. Results of analysis were validated statistically and by recovery studies. The apparent molar absorptivity values (∈max) obtained are 7.549 x 104L mol-1cm-11 and 2.656x104Lmol-1cm-1respectively. Both these have correlation coefficient value of 0.9999. The proposed methods have good precision and accuracy.

2007 ◽  
Vol 4 (4) ◽  
pp. 496-501 ◽  
Author(s):  
M. Vamsi Krishna ◽  
D. Gowri Sankar

Simple, rapid and sensitive spectrophotometric procedures were developed for the analysis of Alfuzosin hydrochloride (AFZ) in pure form as well as in pharmaceutical formulations. The methods are based on the reaction of AFZ with nitrite in acid medium to form diazonium ion, which is coupled with ethoxyethylenemaleic ester (Method A) or ethylcyanoacetate (Method B) or acetyl acetone (method C) in basic medium to form azo dyes, showing absorption maxima at 440, 465 and 490 nm respectively. Beer’s law is obeyed in the concentration of 4-20 μg/mL of AFZ for methods A, B and 3-15 μg/mL of AFZ for method C. The molar absorptivity and sandell’s sensitivity of AFZ- ethoxyethylenemaleic ester, AFZ- ethylcyanoacetate and AFZ-acetyl acetone are1.90 × 104, 0.022; 1.93 × 104, 0.021 and 2.67 × 104L mole-1cm-1, 0.015 μg cm-2respectively. The optimum reaction conditions and other analytical parameters were evaluated. The methods were successfully applied to the determination of AFZ in pharmaceutical formulations.


2020 ◽  
Vol 13 (4) ◽  
pp. 394-401
Author(s):  
M.L.N. Acharyulu ◽  
P.V.S.R. Mohana Rao ◽  
I. Siva Ramakoti

Two visible spectrophotometric methods were developed Aand B for the determination of Darunavir in pure and pharmaceutical formulations. The methods are based on condensation reaction with PDAB (Method-A) and ONB (Method-B) in presence of acidic medium with the primaryamine group in DNV. The coloured products exhibit absorption λmax at 639 nm and 452nm for methods A and B respectively. Regression analysis of Beer-Lambert plots showed good correlation in the concentration ranges 10-60μg/ml, 50-300 μg/ml, correlation co-efficients are 0.9983, 0.9989;Sandell’s sensitivities are9.9833 x 10-3, 3.0456 x 10-2(1 mole cm-1); and molar absorptivity values are5.4857 x 104,1.7981x 104 (μg cm-2) for methods-Aand B respectively. The proposed methods are applied to commercial available formulations and the results are statistically compared with those obtained by the UV reference method and validated by recovery studies. The results are found satisfactory and reproducible. These methods are applied successfully for the estimation of the DNV in the presence of other ingredients that are usually present in formulations. These methods offer the advantages of rapidity, simplicity and sensitivity and low cost without the need for expensive instrumentation and reagents.


Author(s):  
MONIR Z. SAAD ◽  
ATEF AMER ◽  
KHALED ELGENDY ◽  
BASEM ELGENDY

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.


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.


2008 ◽  
Vol 5 (1) ◽  
pp. 10-15 ◽  
Author(s):  
H. D. Revanasiddappa ◽  
M. A. Veena

Two simple and sensitive spectrophotometric methods (A and B) have been described for the determination of ascorbic acid. Method A is based on the oxidation of ascorbic acid (AA) by known excess of Se(IV) in hydrochloric acid medium and subsequent determination of unreacted Se(IV) by reacting it with iodide in the same acid medium to liberate iodine, which react with starch to form a stable blue coloured iodine-starch complex, which shows maximum absorbance at 590 nm. Method B is based on the oxidation of ascorbic acid (AA) by known excess of Cr(VI) in sulphuric acid medium and the determination of unreacted Cr(VI) with diphenyl carbazide (DPC) under the same acidic medium to produce a stable red-violet coloured species, which shows a maximum absorbance at 550 nm. The reacted oxidants (in methods A and B) correspond to the AA content. The apparent molar absorptivity values are found to be 1.627×104and 1.641×104L mol-1cm-1for methods A and B, respectively. The proposed methods are simple, sensitive and suitable for the routine analysis of AA in pharmaceutical formulations and in real samples.


2016 ◽  
Vol 2016 ◽  
pp. 1-9 ◽  
Author(s):  
Kanakapura Basavaiah ◽  
Nagib A. S. Qarah ◽  
Sameer A. M. Abdulrahman

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.


2012 ◽  
Vol 2012 ◽  
pp. 1-6
Author(s):  
Divya N. Shetty ◽  
B. Narayana

Two simple spectrophotometric methods are described for the determination of carvedilol (CAR). Method A is the condensation reaction of CAR with p-dimethylaminobenzaldehyde (PDAB), and the reaction mixture exhibits maximum absorbance at 601 nm. Method B is based on the charge transfer complex formation of CAR with p-chloranil; the color developed is measured at 662 nm. The calibration graphs are found to be linear over 50.00–250.00 and 20.00–100.0 μg mL−1 with molar absorptivity values of 0.92×103 and 0.257×104 L mol−1cm−1 for CAR-PDAB and CAR-p-chloranil, respectively. Statistical comparisons of the results are performed with regard to accuracy and precision using Student’s t-test and F-test at 95% confidence level. The methods are successfully employed for the determination of CAR in pharmaceutical preparations, and the results agree favorably with the reference and proposed methods.


2001 ◽  
Vol 69 (2) ◽  
pp. 151-160
Author(s):  
A. Amin ◽  
H. Saleh

A simple spectrophotometric methods has been developed for the determination of nortriptyline hydrochloride in pure and in pharmaceutical formulations based on the formation of ion-pair complexes with sudun II (SII), sudan (IV) (SIV) and sudan black B (SBB). The selectivity of the method was improved through extraction with chloroform. The optimum conditions for complete extracted colour development were assessed. The absorbance measurements were made at 534, 596 and 649 nm for SII, SIV and SBB complexes, respectively. The calibration graph was linear in the ranges 0.5- 280. 0.5- 37.5 and 0.5 – 31.0 μg ml−1 of the drug usiny the same reagents, respectively. The precision of the procedure was checked by calculating the relative standard deviation of ten replicate determinations on 15 μg ml−1 of nortriptyline HCI and was found to be 1.7, 1.3 and 1.55% using SII, SIV, and SBB complexes, respectively. The molar absorptivity and Sandell sensitivity for each ion-pair were calculated. The proposed methods were successfully applied to the deterniination of pure nortriptyline HCI and in pharmaceutical formulations, and the results demonstrated that the method is equally accurate, precise and reproducible as the official method.


Author(s):  
El Sheikh R ◽  
Hassan W. S. ◽  
Gouda A. A. ◽  
Al OwairdhiA. ◽  
Al Hassani K K H

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.


2008 ◽  
Vol 5 (3) ◽  
pp. 473-478 ◽  
Author(s):  
Marothu Vamsi Krishna ◽  
Dannana Gowri Sankar

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.


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