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 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 Of bromination reaction for the spectrophotometric assay of domperidone in pharmaceuticals

2011 ◽  
Vol 17 (1) ◽  
pp. 81-89 ◽  
Author(s):  
Zenita Devi ◽  
K. Basavaiah ◽  
K.B. Vinay
Keyword(s):  
Limit Of Detection ◽  
Pharmaceutical Preparations ◽  
Reference Method ◽  
Standard Addition ◽  
Limit Of Quantification ◽  
Fixed Amount ◽  
Spectrophotometric Methods ◽  
Significant Difference ◽  
Bulk Drug

Three simple and sensitive spectrophotometric methods are described for the determination of domperidone (DOM) in bulk drug and in dosage forms using bromate-bromide mixture as brominating agent in acid medium and three dyes, meta-cresol purple (MCP), amaranth (AMR) and erioglaucine (EGC). The methods involve the addition of a known excess of bromate-bromide mixture to an acidified solution of DOM followed by the determination of the residual bromine by reacting with a fixed amount of either MCP dye and measuring the absorbance at 530 nm (method A) or AMR dye and measuring the absorbance at 520 nm (method B) or EGC dye and measuring the absorbance at 630 nm (method C). Beer?s law is obeyed over the concentration ranges, 0.63 - 10.0, 0.25-4.0 and 0.13-2.0 ?g mL-1 for method A, method B and method C, respectively. The apparent molar absorptivities are calculated to be 3.751 ? 104, 6.604 ? 104 and 1.987 ? 105 L mol-1cm-1 for method A, method B and method C, respectively and the corresponding sandell sensitivity values are 0.011, 0.006 and 0.002 ?g cm-2. The limit of detection and the limit of quantification are also reported for all the three methods. No interference was observed from common additives found in pharmaceutical preparations. Statistical comparisons of the results with those of the reference method showed an excellent agreement, and indicated no significant difference in accuracy and precision. The accuracy and reliability of the methods were further ascertained by performing recovery tests via standard-addition technique.

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 Simple and extraction-free spectrophotometric methods for risperidone in pure form and in dosage forms

2013 ◽  
Vol 19 (1) ◽  
pp. 121-128 ◽  
Author(s):  
Hemavathi Deepakumari ◽  
Shiramahally Mallegowda ◽  
Kanakapura Vinay ◽  
Hosakere Revanasiddappa
Keyword(s):  
Limit Of Detection ◽  
Ion Pairs ◽  
Pharmaceutical Preparations ◽  
Reference Method ◽  
Standard Addition ◽  
Bromophenol Blue ◽  
Phenol Red ◽  
Spectrophotometric Methods ◽  
Accuracy And Precision

Two simple, sensitive and extraction-free spectrophotometric methods are described for the estimation of risperidone (RSP) in both pure and in pharmaceutical preparations. The proposed methods are based on the formation of ion-pair complex between RSP and the dyes, bromophenol blue (BPB) in method A and Phenol red (PR) in method B at room temperature to form yellow colored products which show maximum absorbance at 410 and at 400 nm in methods A and B, respectively. Beer's law was obeyed in the concentration range of 0.5-10 and 0.5-25 ?g mL-1 in methods A and B with apparent molar absorptivities of 3.43 ? 104 and 0.85 ? 104 L moL-1 cm-1, respectively. The limit of detection for method A is found to be 0.0056 and for method B is 0.132 ?g mL-1. The composition of the ion-pairs was established by Job?s method and it was found to be 1:1 for both the methods A and B. The proposed methods have been applied successfully to the determination of RSP in pharmaceutical preparations. The results were statistically compared with those of a reference method by applying the Student?s t-test and F-test. The methods developed were validated for accuracy and precision by performing recovery experiments via standard addition technique.

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 Spectrophotometric Indirect Determination of Captopril through Redox Reaction with n-bromosuccinimide and RB dye in Pharmaceutical Products

2020 ◽  
Vol 8 (2) ◽  
pp. 8-14
Author(s):  
Dashne M. Kokhasmail ◽  
Tara F. Tahir ◽  
Kurdistan F. Azeez
Keyword(s):  
Limit Of Detection ◽  
Pharmaceutical Preparations ◽  
Reference Method ◽  
Pharmaceutical Products ◽  
Indirect Determination ◽  
Relative Standard ◽  
Experimental Parameters ◽  
Replicated Measurements ◽  
Student’S T

A simple, accurate, and sensitive method for the spectrophotometric determination of captopril in bulk and dosage forms is reported. The method is based on the bromination of captopril with excess solution of n-bromosuccinimide (NBS) in HCl acid medium. The excess NBS is pursued by the assessment of the residual NBS based on its ability to bleach the rhodamine B dye and measuring the absorbance at 555 nm. The amount of NBS reacted coincides to the drug content. The different experimental parameters influencing the development and stability of the color are precisely studied and optimized. Beer’s law is valid within a concentration range of 0.3–1.0 μg/mL with a correlation coefficient R2 = 0.991. The limit of detection 0.169 μg/mL is attained and relative standard deviation values for five replicated measurements of 0.3, 0.7, and 1.0 μg/mL captopril were between 0.53% and 2.03%. No interference is detected from prevalent additives found in pharmaceutical preparations. The proposed method is profitably put on to the determination of captopril in the tablet formulations with mean recoveries 98.91–101.27% and the results were statistically confronted with those of a reference method by applying Student’s t-and F-test.

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 Rapid and Sensitive Spectrophotometric Method for the Determination of the Trace Amount of Thallium (III) in Water and Urine Samples by New Oxidative Coupling Reaction

2019 ◽  
Vol 53 (4) ◽  
Author(s):  
Padmarajaiah Nagaraja ◽  
Naef Ghllab Saeed Al-Tayar ◽  
Anantharaman Shivakumar ◽  
Ashwinee Kumar Shresta ◽  
Avinash K. Gowda
Keyword(s):  
Spectrophotometric Method ◽  
Limit Of Detection ◽  
Rapid Determination ◽  
Coupling Reaction ◽  
Molar Absorptivity ◽  
Urine Samples ◽  
Oxidative Coupling Reaction ◽  
Relative Standard ◽  
Student’S T

A very simple, sensitive and fairly selective direct spectrophotometric method is presented for the rapid determination of thallium(III) at trace level. The method is based on the oxidation of 2-hydrazono-3-methyl-2,3-dihydrobenzo[d]thiazole hydrochloride (MBTH) by thallium(III) in phosphoric acid medium to form a diazoniumcation, which couples immediately with 10,11-dihydro-5Hdibenzo[b,f]azepine (IDB) at room temperature giving a blue colored species having a maximum absorption at 660 nm. The reaction conditions and other important analytical parameters were optimized.The calibration curve was found to be linear over the range of 0.1-4 μg/mL with molar absorptivity of 4.5 × 104 L mol- cm-1 and Sandell’s sensitivity of 0.00454 μg cm-2. The relative standard deviation and limit of detection have been found to be 0.58% and 0.0147 μg/mL respectively. Almost all common anions and cations are found notto interfering in matrix level of the analytical process. The method has been successfully applied for the determination of thallium(III) in synthetic standard mixtures, water and human urine samples. The performance of proposed method was evaluated in terms of student’s t-test and variance ratio F-test, to find out the significance of proposed method over the reported methods.    

scholarly journals Microtitrimetric determination of a drug content of pharmaceuticals containing olanzapine in non-aqueous medium

2009 ◽  
Vol 15 (2) ◽  
pp. 77-81 ◽  
Author(s):  
Kanakapura Basavaiah ◽  
Nagaraju Rajendraprasad ◽  
Basavaiah Vinay
Keyword(s):  
Standard Deviation ◽  
Aqueous Medium ◽  
Reference Method ◽  
Standard Addition ◽  
Cost Effective ◽  
Pharmaceutical Products ◽  
Relative Standard ◽  
Bulk Drug ◽  
Point Detection

Two simple, rapid, reliable and cost-effective methods based on titrimetry in non-aqueous medium are described for the determination of olanzapine in pharmaceuticals. In these methods, the drug dissolved in the glacial acetic acid was titrated with the acetous perchloric acid with visual and potentiometric end point detection, crystal violet being used as the indicator for visual titration. The methods are applicable over 1-15 mg range of olanzapine. The procedures were applied to determine olanzapine in pharmaceutical products and the results were found to be in a good agreement with those obtained by the reference method. Associated pharmaceutical materials did not interfere. The precision results, expressed by inter-day and intra-day relative standard deviation values, were satisfactory, higher than 2%. The accuracy was satisfactory as well. The methods proved to be suitable for the analysis of olanzapine in bulk drug and in tablets. The accuracy and reliability of the methods were further ascertained by recovery studies via a standard addition technique with percent recoveries in the range 97.51-103.7% with a standard deviation of less than 2%.

scholarly journals Rapid titrimetric and spectrophotometric determination of ofloxacin in pharmaceuticals using N-bromosuccinimide

2011 ◽  
Vol 47 (2) ◽  
pp. 251-260 ◽  
Author(s):  
Kanakapura Basavaiah Vinay ◽  
Hosakere Doddarevanna Revanasiddappa ◽  
Okram Zenita Devi ◽  
Pavagada Jagannathamurthy Ramesh ◽  
Kanakapura Basavaiah
Keyword(s):  
Indigo Carmine ◽  
Reference Method ◽  
Standard Addition ◽  
Addition Method ◽  
Fixed Amount ◽  
Spectrophotometric Methods ◽  
Analytical Reagent ◽  
Bulk Drug ◽  
Reaction Stoichiometry

One titrimetric and two spectrophotometric methods have been described for the determination of ofloxacin (OFX) in bulk drug and in tablets, employing N-Bromosuccinimide as an analytical reagent. The proposed methods involve the addition of a known excess of NBS to OFX in acid medium, followed by determination of unreacted NBS. In titrimetry, the unreacted NBS is determined iodometrically, and in spectrophotometry, unreacted NBS is determined by reacting with a fixed amount of either indigo carmine (Method A) or metanil yellow (Method B). In all the methods, the amount of NBS reacted corresponds to the amount of OFX. Titrimetry allows the determination of 1-8 mg of OFX and the calculations are based on a 1:5 (OFX:NBS) reaction stoichiometry. In spectrophotometry, Beer's law is obeyed in the concentration ranges 0.5-5.0 µg/mL for method A and 0.3-3.0 µg/mL for method B. The molar absorptivities are calculated to be 5.53x10(4) and 9.24x10(4) L/mol/cm for method A and method B, respectively. The methods developed were applied to the assay of OFX in tablets, and results compared statistically with those of a reference method. The accuracy and reliability of the methods were further ascertained by performing recovery tests via the standard-addition method.

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