scholarly journals Oxidative Coupling Reaction for Micro Trace Analysis of Mebendazol Residual with p-bromoaniline in Presence of n- bromosuccinimide

2020 ◽  
Vol 17 (3) ◽  
pp. 0780
Author(s):  
Takleef Sallal ◽  
Sumayha Abbas
Keyword(s):  
Limit Of Detection ◽  
Coupling Reaction ◽  
Accurate Method ◽  
Molar Absorptivity ◽  
Mean Value ◽  
Oxidative Coupling Reaction ◽  
Relative Standard ◽  
Limit Of Quantitation ◽  
Colored Product ◽  
Hydrolysis Of

Rapid, reproducible and accurate method has been developed for the assay for of mebendazol (MBZ) residual assay. The method is based on alkaline hydrolysis of MBZ with sodium hydroxide then oxidation with N-bromosuccinimide (NBS) followed by coupling with 4-Bromoaniline (4-BA) to yield a highly colored product absorbed at maximum 434 nm. Regression analysis of linearity range was found (0.6-2.8) µg.ml-1.  The optimum conditions that affect the oxidation were studied. The developed method was found to be precise with mean value of relative standard deviation (1.153- 1.303) and accurate with relative error (-0.5940-1.7821) .The calculated molar absorptivity and sandal sensitivity values of (29825 L.mol-1.cm-1), 0.0099 µg.cm-2 respectively.  The limit of detection and limit of quantitation were of 0.04696, 0.156548 µg.ml-1 respectively .The suggested method showed good recovery with a mean value of 100.77% for analysis of dosage forms.

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 Spectrophotometric Determination of Bisacodyl in Pure and Pharmaceutical Preparation via Oxidative Coupling Organic Reaction

2017 ◽  
Vol 14 (1) ◽  
pp. 181-188
Author(s):  
Baghdad Science Journal
Keyword(s):  
Oxidative Coupling ◽  
Pharmaceutical Preparation ◽  
Pharmaceutical Preparations ◽  
Coupling Reaction ◽  
Molar Absorptivity ◽  
Water Soluble ◽  
Alkaline Media ◽  
Oxidative Coupling Reaction ◽  
Relative Standard ◽  
Limit Of Quantitation

A simple, accurate and sensitive spectrophotometric way is used to determine Bisacodyl in pure and pharmaceutical preparations. The proposed method depends on using 2,4-Dinitrophenylhydrazine as chromogenic reagent . The method was based on the oxidative coupling reaction of Bisacodyl with 2,4-Dinitrophenylhydrazine with Sodium periodate in the presence of sodium hydroxide as alkaline media to form red water soluble dye product , that has a maximum absorption at ?max 522nm . Beer ,s law is obeyed in the concentration of (2.00–20.00) ?g.ml -1 .The molar absorptivity is (6505) L.mol-1.cm-1,a sandall sensitivity of(0.0555) ?g.cm-2), correlation coefficient of (0.9970) , Limitof detection (LOD) (0.0312 ?g.ml-1), limit of Quantitation (LOQ) (0. 3125 ?g.ml-1) and the relative standard deviation of RSD% (1.6). The method gave a successful determination for Bisacodyl in pharmaceutical preparations and the value of recovery % was better than (100.16%)

scholarly journals FLOW INJECTION SPECTROPHOTOMETRIC DETERMINATION OF NARINGENIN IN SUPPLEMENTS USING SOLID-PHASE REACTOR CONTAINING IMMOBILIZED MANGANESE DIOXIDE

2018 ◽  
Vol 11 (8) ◽  
pp. 473
Author(s):  
Israa M Jawad Al Mashhadani ◽  
Sadeem Subhi Abed
Keyword(s):  
Manganese Dioxide ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Coupling Reaction ◽  
Accurate Method ◽  
Oxidative Coupling Reaction ◽  
Daily Diet ◽  
Solid Phase Reactor ◽  
Colored Product

Objective: Naringenin (NAR) is a part of the human daily diet, and it plays an important role in human health for its biological functions. This study describes a new, sensitive, simple, and accurate method for determining NAR in supplements.Methods: The method is based on oxidative coupling reaction between NAR and N, N-dimethyl-p-phenylenediamine in an alkaline medium using manganese dioxide immobilized in cellulose acetate as online oxidant agent to form a colored product which can be monitored at λ max598 nm. Results: Several operating parameters such as reactor column length, particles size, chemicals, and physicals reaction conditions were studied. The proposed method was sensitive and good repeatable, the linear range of NAR concentration was from 1 to 70 μg/ml with a limit of detection of 0.292 μg/ml, and recovery range of analysis was 99.55–100.48%. Conclusion: The proposed method was successfully applied for determining NAR in supplements.

scholarly journals Spectrophotometric Determination of Azithromycin using Oxidative Coupling Reaction

2020 ◽  
Vol 10 (03) ◽  
pp. 389-394
Author(s):  
Maadh T. Abdulrahman ◽  
Ihab M. Rashid ◽  
Nashwan H. Ali
Keyword(s):  
Oxidative Coupling ◽  
Limit Of Detection ◽  
Pharmaceutical Preparations ◽  
Coupling Reaction ◽  
Sensitivity Index ◽  
Oxidative Coupling Reaction ◽  
Relative Standard ◽  
Sensitivity And Selectivity ◽  
Colored Product ◽  
The Stability

For determining the azithromycin (AZT) in medicinal and pure formulas, a simple spectrophotometric technique was developed. An approach suggested is dependent on an AZT’s oxidative coupling reaction by sodium period (SPI) and 4-amino antipyrine (AAP) producing a pink colored compound with optimum absorption of 480 nm. Different experimental parameters are extensively researched and mastered, which affects the stability of a colored product formed, then developed. The law of the Beer is obeyed over its concentration range 3 to 44 ppm, whereas the limit of detection and quantification is 0.1908 and 0.5726 ppm, respectively, for a connection factor (r) = 0.9998. Also calculated are the molar absorption of 8.23 × 103 L/mol.cm, and the sensitivity index for Sandell is 7 × 10-5 mg/cm2. A method’s accuracy and precision are tested by also determining a relative standard deviation (RSD) less than 0.645 percent, and 100.189 percent average recovery. Practically possible external interferences about a calculation for AZT are checked in drug tablets. The results demonstrated that the procedure for determining AZT was successful in its application in pharmaceutical preparations. Comparing the literature survey that shows good sensitivity and selectivity, the reliability of the proposed method is chalked in.

scholarly journals Spectrophotometric Determination of the Trace Amount of Thallium in Water and Urine Samples by Novel Oxidative Coupling Reaction

2009 ◽  
Vol 6 (4) ◽  
pp. 1153-1163 ◽  
Author(s):  
P. Nagaraja ◽  
N. Ghllab Saeed Al-Tayar ◽  
A. Shivakumar ◽  
A. K. Shresta ◽  
A. K. Gowda
Keyword(s):  
Coupling Reaction ◽  
Molar Absorptivity ◽  
Urine Samples ◽  
Standard Reference Materials ◽  
Oxidative Coupling Reaction ◽  
Relative Standard ◽  
Imipramine Hydrochloride ◽  
Optimum Reaction ◽  
Synthetic Standard

A novel, simple, rapid, sensitive and selective method has been proposed for the trace determination of thallium by spectrophotometric detection. This method is based on the oxidation of MBTH (3-methyl-2-benzothiazolinone hydrazone hydrochloride) by thallium(III) to form diazonium cation, which couples with IPH (Imipramine hydrochloride) in phosphoric acid medium at room temperature giving a blue colored species having a maximum absorption at 635 nm. The reagents and manifold variables influences on the sensitivity were investigated and the optimum reaction conditions have been established. The calibration curve was found to be linear over the range 0.1-5 μg mL-1with the molar absorptivity and Sandell’s sensitivity of 2.9x104L mol-1cm-1, 0.0071 μg cm-2respectively. The tolerance limit of the method towards various ions usually associated with thallium has been detected. The relative standard deviation for five replicate determination of 2μg mL-1thallium was 0.47%. The method has been successfully applied for the determination of thallium(ІΙΙ) and thallium(I) in synthetic, standard reference materials, water and urine samples with satisfactory results. The performance of the proposed method was evaluated in terms of student’st-test and variance ratioF-test, to find out the significance of proposed method over the reported methods.

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 New Spectrophotometric Method for the Assay of Sulfadiazine Drug Based on Diazotization Coupling Reaction

2016 ◽  
Vol 24 (2) ◽  
pp. 88-101
Author(s):  
Mohauman Mohammad Al-Rufaie
Keyword(s):  
Solvent Extraction ◽  
Spectrophotometric Method ◽  
Limit Of Detection ◽  
Coupling Reaction ◽  
Molar Absorptivity ◽  
Colored Complex ◽  
Spectrophotometric Procedure ◽  
Limit Of Quantitation ◽  
Diluted Solution ◽  
Beer’S Law

Abstract A sensitive, simple and rapid spectrophotometric procedure for the assay of trace quantities of sulfadiazine (SDZ) drug as bulk and in diluted solution is characterized. The procedure depends on the diazotization reaction which is produced by coupling SDZ with (4-amino-2-hydroxy acetophenon) (AHA) to produce an intense colored complex spectrophotometrically determined at 410 nm. Beer’s law was applied in the range of concentration 0.5 - 15 ppm; the molar absorptivity and Sandell’s sensitivity were 2.8484 × 104 L mol-1 cm-1 and 0.008 μg cm-2 respectively. The method limit of detection (LOD) was 0.443 μg mL-1 and LOQ (the method limit of quantitation) was 0.249 μg mL-1. The procedure is not based on solvent extraction and the additives and excipients do not significantly influence the developed procedure.

scholarly journals Development of Green Method for Trace Determination of Bendiocarb in Real Samples Using Emerson

2016 ◽  
Vol 13 (2) ◽  
pp. 426-439
Author(s):  
Baghdad Science Journal
Keyword(s):  
Cloud Point ◽  
Limit Of Detection ◽  
Molar Absorptivity ◽  
Optimum Conditions ◽  
Green Method ◽  
Colored Product ◽  
Aqueous Layer ◽  
Triton X ◽  
Hydrolysis Of

In this study, cloud point extraction combined with molecular spectrometry as an eco-friendly method is used for extraction, enrichment and determination of bendiocarb (BC) insecticide in different complex matrices. The method involved an alkaline hydrolysis of BC followed Emerson reaction in which the resultant phenol is reacted with 4-aminoantipyrene(4-AAP) in the presence of an alkaline oxidant of potassium ferric cyanide to form red colored product which then extracted into micelles of Triton X-114 as a mediated extractant at room temperature. The extracted product in cloud point layer is separated from the aqueous layer by centrifugation for 20 min and dissolved in a minimum amount of a mixture ethanol: water (1:1) followed the determination of BC by using spectrophotometry at a wavelength maximum of 470 nm. The most important parameters affecting the extraction and determination of BC are conducted via a classical optimization. Under the optimum conditions established , Beer’s law is obeyed in the range of 0.1-4 µg mL-1 while the optimum concentration ranges estimated by Ringbom’s plot was of 0.4-2.12 µg mL-1. The enrichment factor was of 59.87 fold leading to achieve the limit of detection of 0.076 ?g mL-1. The proposed method gives superior sensitivity in terms of the molar absorptivity of 1.99x105 L mol-1 cm-1 and extraction efficiency of 98.0%. The established method is applied in the analysis of the spiked vegetables, orange, soil and water samples with appropriate concentration with BC standard.

scholarly journals Spectrophotometric Determination of sulphadiazine by oxidative coupling reaction with ortho-amino phenol as reagent

2019 ◽  
Vol 24 (4) ◽  
pp. 40
Author(s):  
Aisha A. Abd ◽  
Ali I. Khaleel ◽  
, Faiez M. Hamed
Keyword(s):  
Oxidative Coupling ◽  
Coupling Reaction ◽  
Molar Absorptivity ◽  
Dosage Forms ◽  
Pharmaceutical Dosage Forms ◽  
Oxidative Coupling Reaction ◽  
Relative Standard ◽  
Amino Phenol ◽  
532 Nm

A simple, rapid and sensitive spectrophotometric method for determination of sulphadiazine (SDZ) in aqueous solution is described. The method iis based on the oxidation of SDZ by potasium Periodate, and coupling with ortho-amino phenol to give a violet colour of  maximum absorbaance at 532 nm. Beer's law is obeyed over the concentration range of 5-40 µg /ml of SDZ with a (R2=0.9980) and molar absorptivity 5581.6 L.mol-1.cm-1  and a relative error in the range of - 0.06 - 2.3  % and a relative standard deviation of not more than 0.31 %. The composition of the resulting product is also investigated and it is found to be1:1. The method is successfully applied for the determinatiion of SDZ in pure and pharmaceutical dosage forms, with recovery of noot less than 101.1%.   http://dx.doi.org/10.25130/tjps.24.2019.070

Rapid and Sensitive Liquid Chromatographic Method for Determination of Anastrozole in Different Polymer–Lipid Hybrid Nanoparticles

2021 ◽  
pp. 247263032098230
Author(s):  
Dilshad Ahmad ◽  
Faisal A. Al Meshaiti ◽  
Yazeed K. Al Anazi ◽  
Osama Al Owassil ◽  
Alaa Eldeen B. Yassin
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Reversed Phase ◽  
Hplc Method ◽  
Hybrid Nanoparticles ◽  
Array Detector ◽  
Relative Standard ◽  
Validation Parameters ◽  
Limit Of Quantitation ◽  
Inhibitor Drug

Anastrozole, an aromatase inhibitor drug, is used for the treatment of breast cancer in pre- and postmenopausal women. Anastrozole’s incorporation into nanoparticulate carriers would enhance its therapeutic performance. To perceive the exact loaded amount of drug in nanocarriers, a valid analytical method is required. The reversed-phase high-performance liquid chromatography (RP-HPLC) method was developed and validated by using the C18 column, 150 × 4.6 mm, 5 µm particle size, in isocratic mobile phase composed of 50:50 V/V (volume/volume) acetonitrile–phosphate buffer (pH 3) flowing at a rate of 1.0 mL/min, and a diode array detector (DAD) set at λmax = 215 nm. The validation parameters such as linearity, accuracy, specificity, precision, and robustness have proven the accuracy of the method, with the relative standard deviation percentage (% RSD) values < 2. The limit of detection of the method was found equal to 0.0150 µg/mL, and the limit of quantitation was 0.0607 µg/mL. The percent recovery of sample was in the range of 98.04–99.25%. The method has the advantage of being rapid with a drug retention time of 2.767 min, specific in terms of resolution of peaks void of interference with any of the excipients, and high reproducibility. This makes it highly applicable for quality control purposes.

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