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 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.

Micellar-Enhanced Spectrofluorimetric Method for Quantification of Diclofenac Potassium in Pure Form, in Pharmaceutical Preparations and Human Plasma

2021 ◽  
Vol 58 (6) ◽  
pp. 427-434
Author(s):  
Muhammad Naeem Khan ◽  
Irum ◽  
Saba Gul ◽  
Muslima ◽  
Muhammad Mursaleen
Keyword(s):  
Human Plasma ◽  
Limit Of Detection ◽  
Sodium Dodecyl ◽  
Pharmaceutical Preparations ◽  
Pharmaceutical Products ◽  
Pure Form ◽  
Fluorescence Signal ◽  
Spectrofluorimetric Method ◽  
Relative Standard

Abstract A rapid, simple and economical spectrofluorimetric method for the determination of diclofenac potassium in pure form, in pharmaceutical preparations and in human plasma has been developed. The method is based on the enhancement of the fluorescence signal of diclofenac potassium by the addition of sodium dodecyl sulphate in McIvaine buffer with a pH of 5. Different experimental conditions such as buffer type, pH, type and concentration of surfactants were investigated. The fluorescence intensity of the solution was recorded at 361 nm after excitation at 243 nm. The method shows linearity in the concentration range of 0.2 μg mL–1–10 μg mL–1 with a good correlation coefficient of 0.997. The relative standard deviation value was 3.62 (n = 7). The limit of detection and limit of quantification were calculated to be 2.84 × 10–3 μg mL–1 and 9.47 × 10–3 μg mL-1, respectively. The effect of excipients and co-administrated drugs was investigated and no interference was observed. The method was successfully applied for the determination of diclofenac potassium in pure form, in pharmaceutical products and in human plasma. The percentage recoveries obtained ranged from 100.25% to 102.16% for pure form and 97.50% to 102.00% for pharmaceutical products and from 98.50% to 101.67% for human plasma.

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 Spectrophotometric determination of Phenylephrine hydrochloride and Salbutamol sulphate drugs in pharmaceutical preparations using diazotized Metoclopramide hydrochloride

2015 ◽  
Vol 12 (1) ◽  
pp. 167-177 ◽  
Author(s):  
Baghdad Science Journal
Keyword(s):  
Limit Of Detection ◽  
Pharmaceutical Preparations ◽  
Correlation Coefficients ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Forms ◽  
Salbutamol Sulphate ◽  
Phenylephrine Hydrochloride ◽  
Relative Standard ◽  
Metoclopramide Hydrochloride

A spectrophotometric method has been proposed for the determination of two drugs containing phenol group [phenylephrine hydrochloride (PHP) and salbutamol sulphate (SLB)] in pharmaceutical dosage forms. The method is based on the diazotization reaction of metoclopramide hydrochloride (MCP) and coupling of the diazotized reagent with drugs in alkaline medium to give intense orange colored product (?max at 470 nm for each of PHP and SLB). Variable parameters such as temperature, reaction time and concentration of the reactants have been analyzed and optimized. Under the proposed optimum condition, Beer’s law was obeyed in the concentration range of 1-32 and 1-14 ?g mL-1 for PHP and SLB, respectively. The limit of detection (LOD) and limit of quantification (LOQ) for each of PHP and SLB were 0.60, 0.52 ?g mL-1 and 2.02, 1.72 ?g mL-1, respectively. No interference was observed from common excipients present in pharmaceutical preparations. The good correlation coefficients and low relative standard deviation assert the applicability of this method. The suggested method was further applied for the determinations of drugs in commercial pharmaceutical preparations, which was compared statistically with reference methods by means of t- test and F- test and were found not to differ significantly at 95% confidence level. The procedure was characterized by its simplicity with accuracy and precision.

scholarly journals Kinetic Spectrophotometric Determination of Gemifloxacin Mesylate and Moxifloxacin Hydrochloride in Pharmaceutical Preparations Using 4-Chloro-7-nitrobenzo-2-oxa-1,3-diazole

2014 ◽  
Vol 2014 ◽  
pp. 1-12 ◽  
Author(s):  
Mohammed G. Abdel Wahed ◽  
Ragaa El Sheikh ◽  
Ayman A. Gouda ◽  
Sayed Abou Taleb
Keyword(s):  
Limit Of Detection ◽  
Kinetic Method ◽  
Pharmaceutical Preparations ◽  
Fixed Time ◽  
Spectrophotometric Methods ◽  
Relative Standard ◽  
Significant Difference ◽  
Kinetic Spectrophotometric ◽  
Comparison Of The Results

Simple, sensitive, and accurate kinetic spectrophotometric method was proposed for the determination of gemifloxacin mesylate (GMF) and moxifloxacin hydrochloride (MOX) in pure forms and pharmaceutical preparations (tablets). The method is based on coupling the studied drugs with 4-chloro-7-nitrobenzo-2-oxa-1,3-diazole (NBD-Cl) in the presence of alkaline borate buffer. Spectrophotometric measurement was achieved by recording the absorbance at 466 and 464 nm for GMF and MOX, respectively, after a fixed time of 20 and 15 min on a water bath adjusted at 70 ± 5°C for both drugs. The different experimental parameters affecting the development and stability of the color were carefully studied and optimized. The absorbance-concentration plots were linear over the ranges 0.5–8.0 and 2.0–12 μg mL−1for GMF and MOX, respectively. The limit of detection of the kinetic method was about 0.12 (2.47 × 10−7 M) and 0.36 (8.22 × 10−7 M) μg mL−1for GMF and MOX, respectively. The proposed methods have been applied and validated successfully with percentage relative standard deviation (RSD% ≤ 0.52) as precision and percentage relative error (RE% ≤ 1.33) as accuracy. The robustness of the proposed method was examined with recovery values that were 97.5–100.5 ± 1.3–1.9%. Statistical comparison of the results with the reference spectrophotometric methods shows excellent agreement and indicates no significant difference in accuracy or precision.

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 Spectrophotometric and RP-HPLC Methods for Determining Cefotaxime Sodium in Pharmaceutical Preparations

2020 ◽  
Vol 32 (6) ◽  
pp. 1314-1320
Author(s):  
Lamya A. Sarsam ◽  
Salim A. Mohammed ◽  
Sahar A. Fathe
Keyword(s):  
Limit Of Detection ◽  
Phosphate Buffer Solution ◽  
Pharmaceutical Preparations ◽  
Molar Absorptivity ◽  
Hplc Method ◽  
Buffer Solution ◽  
Limit Of Quantification ◽  
Rp Hplc ◽  
Relative Standard

A rapid, simple and sensitive spectrophotometric and RP-HPLC methods have been developed for the quantitative determination of cefotaxime-Na in both pure and dosage forms. The spectrophotometric method was based on diazotization of cefotaxime-Na and then coupling with 8-hydroxyquinoline in an alkaline medium. The resulting azo dye exhibited maximum absorption at 551 nm with a molar absorptivity of 0.597 × 104 L mol-1 cm-1. Beer′s law was obeyed over the range 10-700 μg/25 mL (i.e. 0.4-28.0 ppm) with an excellent determination coefficient (R2 = 0.9993). The limit of detection (LOD) and limit of quantification (LOQ) were found to be 0.0194 and 0.3765 μg mL-1, respectively. The recoveries were obtained in the range 97.3-102.5% and the relative standard deviation (RSD) was better than ± 1.56. The HPLC method has been developed for the determination of cefotaxime-Na. The analysis were carried out on a C18 column and a mobile phase composed of acetonitrile and phosphate buffer solution (0.024M KH2PO4 and 0.01M H3PO4) at pH 3.5 in the ratio of 60:40 (v:v), with a flow rate of 1.0 mL min-1 and UV detection at 258 nm. The proposed method showed good linearity (in a range of concentration 1.0-200 μg mL-1. The recovery percent and a relative standard deviations were found in the range 96 to 104.8% and ± 0.017 to ± 0.031%, respectively. Both methods were applied successfully to the assay of cefotaxime-Na in commercial injection preparations.

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 Diclofenac Sodium Determination in Pharmaceutical Preparations After Complexation With Calcium and Magnesium and Molecular Modelling Study.

2021 ◽  
Author(s):  
Waheed Ali Soomro ◽  
Muhammad Yar Khuhawar ◽  
Taj Muhammad Jahaangir ◽  
Muhammad Farooque Lanjwani ◽  
Rafi-u-Zaman Brohi ◽  
...  
Keyword(s):  
Metal Ions ◽  
Aqueous Phase ◽  
Metal Ion ◽  
Limit Of Detection ◽  
Diclofenac Sodium ◽  
Pharmaceutical Preparations ◽  
Flame Atomic Absorption ◽  
Relative Standard ◽  
Complexation Reactions

Abstract The study was carried out for indirect determination of diclofenac sodium in preparations after complexation with Ca or Mg. The diclofenac was treated with the metals individually and the metal complexes formed as precipitates were extracted in chloroform or separated by centrifugation. A decrease in concentration of metal ions was observed in aqueous phase which was correlated with concentration of diclofenac sodium. The complexation reactions were optimized in terms of pH, nature of metal ion, extraction in chloroform or separation by centrifugation. The decrease in concentration of metal ions in aqueous phase was monitored using flame Atomic Absorption Spectrophotometry (AAS) or by complexometric titration with EDTA. The linear calibration range observed were from 40-200 µg /mland 40-200 ug/mL diclofenac sodium respectively by using both Ca and Mg. The limit of detection was 15 µg /mL diclofenac using Ca or Mg ions using both solvent extraction and precipitation methods with AAS. The method was repeatable with interday and intraday reproducibility with relative standard deviation within 5%. The method was applied for the determination of diclofenac from pharmaceutical preparations, Voltral, Voren, Qufen, Dicloplus, Dicloran with RSD% 1.3%-8.2%.

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