scholarly journals Novel Reagents for the Spectrophotometric Determination of Isoniazid

2012 ◽  
Vol 2012 ◽  
pp. 1-5 ◽  
Author(s):  
Divya N. Shetty ◽  
Badiadka Narayana ◽  
Seranthimata Samshuddin
Keyword(s):  
Spectrophotometric Determination ◽  
Pharmaceutical Products ◽  
Molar Absorptivity ◽  
Basic Medium ◽  
Antitubercular Drug ◽  
Substitution Reactions ◽  
Experimental Conditions ◽  
Simple Method ◽  
Bulk Drug

Isoniazid is an antitubercular drug, widely used for tuberculosis. Owing to its importance in therapeutics, the present study aims to develop simple method for the spectrophotometric determination of isoniazid (INH). Two novel reagents, epichlorohydrine (ECH) and 4-hydroxyphenaylchloride (HPC) are used for the spectrophotometric determination of INH. Based on the nucleophilic substitution reactions of INH with EPI & HPC in basic medium, rapid, simple, inexpensive, precise, and accurate visible spectrophotometric method is proposed for the determination of INH in bulk drug and in formulations. Method involves the reaction of INH with EPI and HPC in basic medium to form yellow-colored chromogen, measuring the absorbances at 405 and 402 nm for INH-EPI & INH-HPC, respectively. The optimum experimental conditions have been studied. The absorbance was found to increase linearly with the concentration of the drug and formed the basis for quantification. The calibration graphs were linear from 2.00–22.00 μg mL−1 and 20.00–120.00 μg mL−1 for INH-EPI & INH-HPC, respectively. The apparent molar absorptivity and Sandell's sensitivity are calculated to be 0.51×104 & 0.10×104 L mol−1 cm−1 and 0.027 & 0.134 μg cm−2 for INH-EPI & INH-HPC, respectively. The procedure is used to determine INH in pharmaceutical products. The associated pharmaceutical materials do not interfere in the measurements.

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.

Use of Acidic Hydrolysis and Diazo Coupling Reaction for Spectrophotometric Determination of Furosemide in Urine and Pharmaceutical Formulation.

2018 ◽  
pp. 225
Author(s):  
Hawraa Ali ◽  
Sumayha Muhammed
Keyword(s):  
Spectrophotometric Determination ◽  
Limit Of Detection ◽  
Coupling Reaction ◽  
Molar Absorptivity ◽  
Pharmaceutical Formulation ◽  
Basic Medium ◽  
Ratio Method ◽  
Diazo Coupling ◽  
Limit Of Quantitation

     Simple and rapid spectrophotometric determination of furosemide (FUR) has been investigated .The method is based on acid hydrolysis of FUR to free primary aromatic amine and diazotization followed by coupling with 3, 5 di methyl phenol (3, 5-DMPH) at basic medium. The absorbance was measured at 434 nm, the method was optimized for best condition, and beers’ law is obeyed over the range of 0.4-50 µg.mL-1 with molar absorptivity and sandal’s sensitivity 1.3899 x104 L moL-1 .cm-1 and 0.0238x104 µg.cm-2 respectively. Analysis of solution containing nineteen different concentrations of FUR gave a correlation coefficient of (0.9999) and limit of detection, limit of quantitation were 0.127, 0.464µg.mL-1 respectively. The reaction stoichiometry was evaluated by Job’s and mole ratio method was found to be 1:1(diazotized FUR: 3, 5-DMPH) .The method was applied in synthetic urine and pharmaceutical formulation. The recovery of FUR in spiked urine was satisfactory resulting in the values of (99±3.32) %, the results of the suggested method was compared with available official literature method.

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 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.

scholarly journals New Diazo Coupling Reactions for Visible Spectrophotometric Determination of Alfuzosin in Pharmaceutical Preparations

2007 ◽  
Vol 4 (4) ◽  
pp. 496-501 ◽  
Author(s):  
M. Vamsi Krishna ◽  
D. Gowri Sankar
Keyword(s):  
Pharmaceutical Preparations ◽  
Pharmaceutical Formulations ◽  
Molar Absorptivity ◽  
Basic Medium ◽  
Coupling Reactions ◽  
Acetyl Acetone ◽  
Diazo Coupling ◽  
Optimum Reaction ◽  
Diazonium Ion

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.

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.

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