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Azo Coupling Reaction for indirect Spectrophotometric Determination of Furosemide using Resorcinol as a Reagent
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Abstract<p>A simple and accurate method to determinate furosemide (FUR) based on converting the secondary amine to primary amine with acidic hydrolysis then azotization by nitrous acid and coupled with resorcinol as a coupling agent in aqueous medium at pH 13. The optical characteristic like beers law limit found to be (0.25-2.5) μg.ml<sup>−1</sup>, detection and quantification limits (0.0196) (0.0654) μg.ml<sup>−1</sup>respectivly and Sandel sensitivity was 0.006738 μg.cm<sup>−2</sup>. The least-square method was used to evaluate the regression equation and the correlation coefficient. The resulted azo dye has a maximum absorbance at 430 nm with light orange color. The developed method was successfully applied to determinate FUR in its formulation with 84-105 % as a recovery with a relative standard deviation not more 2% and less than 5% relative error. To validate the proposed method, the standard addition method was applied to evaluate FUR in different formulation sources.</p>
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Publication Date
Sun Apr 29 2018
Journal Name
Iraqi Journal Of Science
FIA– Spectrophotometric methods for the determination of Naringenin in supplements and urine samples using diazotization coupling reactions
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Direct FIA methods for estimation of Naringenin (NG) in different samples were proposed. These methods are based on diazotization coupling reactions of two reagents: method (A) p-chloroaniline (PCA) and method (B) procaine hydrochloride (PRH) with NG in basic medium. Yellow dyes with maximum absorption at 416 and 415 nm were formed respectively. Calibration curves were constructed over different NG concentrations, linearity was from 1- 70 and 1- 40 µgmL-1 with detection limits of 0.55 and 0.24 µgmL-1 for (A) and (B) respectively. All analytical variables involved in the FIA procedure were evaluated and optimized. The established methods were successfully applied for the determination of NG in its supplements and u

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Publication Date
Sat Mar 11 2017
Journal Name
Ibn Al-haitham Journal For Pure And Applied Sciences
Spectrophotometric Determination of Sulfamethoxazole with P-N,N-dimethyl amino benzaldehyde as Condensation Reaction
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Sulfamethoxazole (SMX) was added to P-N,N-dimethyl amino benzaldehyde (PDAB) by condensation reaction in acidic medium to form, a yellow colored dye compound which exhibits maximum absorption (λmax) at 450.5 nm. The concentration of (SMX) was determined spectrophotometrically. The optimum reaction conditions and other analytical parameters were evaluated. In addition to classical univariate optimization, design of experiment method has been applied in optimization of the variables affecting the color producing reaction.    Beer’s law obeyed in the concentration range of 0.1-10 μg.mL-1 with molar absorptivity of 5.7950×104  L.mol-1.cm-1. The limit of detection and Sandell's sensitivity value were 0.078 μ

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Publication Date
Mon Mar 27 2017
Journal Name
Iraqi Journal Of Pharmaceutical Sciences ( P-issn 1683 - 3597 E-issn 2521 - 3512)
Spectrophotometric Determination of Clonazepam in Pure and Dosage forms using Charge Transfer Reaction
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A rapid, sensitive and without extraction spectrophotometric method for determination of clonazepam (CLO) in pure and pharmaceutical dosage forms has been described. The proposed method was simply depended on charge transfer reaction between reduced CLO (n-donor) and metol (N-methyl-p-aminophenol sulfate) as a chromogenic reagent (π- acceptor). The reduced drug, with zinc and concentrated hydrochloric acid, produced a purple colored soluble charge-transfer complex with metol in the presence of sodium metaperiodate in neutral medium, which has been measured at λmax 532 nm. All the variables which affected the developed and the stability of the colored product such as concentration of reagent and oxidant, temperature and time of rea

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Publication Date
Sat Oct 28 2023
Journal Name
Baghdad Science Journal
Indirect Flow Injection Spectrophotometric and Chromatographic Methods for the Determination of Mebendazole in Pharmaceutical Formulations
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Chromatographic and spectrophotometric methods for the estimation of mebendazole in
pharmaceutical products were developed. The flow injection method was based on the oxidation of
mebendazole by a known excess of sodium hypochlorite at pH=9.5. The excess sodium hypochlorite is then
reacted with chloranilic acid (CAA) to bleach out its color. The absorbance of the excess CAA was recorded
at 530 nm. The method is fast, simple, selective, and sensitive. The chromatographic method was carried out
on a Varian C18 column. The mobile phase was a mixture of acetonitrile (ACN), methanol (MeOH), water
and triethylamine (TEA), (56% ACN, 20% MeOH, 23.5% H2O, 0.5% TEA, v/v), adjusted to pH = 3.0 with
1.0 M hy

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Publication Date
Thu Jun 23 2022
Journal Name
Iraqi Journal Of Pharmaceutical Sciences ( P-issn 1683 - 3597 E-issn 2521 - 3512)
Flow Injection Spectrophotometric Technique for Determining of Genistein in Pure and Supplements Formulations Through Diazotization Coupling Reaction
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Genistein (GEN) is The major isoflavone found in soybeans, has a number of cardiovascular health benefits, Postmenopausal syndrome and osteoporosis. A direct flow injection analysis method for estimation of (GEN) in pure and supplements formulation . This system is based on diazotization coupling reactions between procaine penciline (PR) and genistein in basic medium, they formed yellow dyes have maximum absorption at 416 nm. Calibration curve were constructed over different GEN concentrations, linearity for GEN was 10-100 µg.mL-1 and detection limits of 1.51 ?g/mL. In the FIA technique, all analytical factors were analyzed and optimized. The established method was successfully used to determine GEN in the formulations of its supplement

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Publication Date
Wed Apr 12 2017
Journal Name
Ibn Al-haitham Journal For Pure And Applied Sciences
Spectrophotometric Determination of Sulfamethoxazole Following Simple Diazotization and Coupling with Diphenylamine
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    Simple, sensitive, accurate and inexpensive spectrophotometric methods have been developed for the determination of sulfamethoxazole (SMZ) in pure and dosage forms. This method is based on diazotization of primary amine group of sulfamethoxazole with sodium nitrite and hydrochloric acid followed by coupling with diphenylamine in acidic medium to obtain a stable blue colored dye and show a maximum absorption (max) at 530 nm. Different variables affecting the completion of reaction have been carefully optimized, following the classical univariate sequence and modified simplex method. Beer’s law is obeyed in the concentration range of (0.5-12.0 µg.mL-1) with molar absorptivity of 4.9617×104 L.mol-1.cm-1. The

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Publication Date
Mon Dec 25 2017
Journal Name
Iraqi Journal Of Pharmaceutical Sciences ( P-issn 1683 - 3597 E-issn 2521 - 3512)
Spectrophotometric Determination of Cefixime Following Simple Diazotization and Coupling with ?-Naphthol
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Cefixime (CFX) was treated with sodium nitrite and hydrochloric acid for diazotization reaction followed by coupling with ?-Naphthol in alkaline medium to form, a yellow colored azo dye compound which exhibits maximum absorption (?max) at 412 nm where the concentration of (CFX) was determined spectrophotometrically. The optimum reaction conditions and other analytical parameters were evaluated. Beer’s law was obeyed in the concentration range of (1-20) ?g.mL-1 with a molar absorptivity of 34870.5 L.mol-1.cm-1. The limit of detection was found to be 0.1090 ?g.mL-1 and the Sandell's sensitivity value was 0.0130 ?g.cm-2. The proposed method could be successfully applied to

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Publication Date
Sun Mar 26 2017
Journal Name
Iraqi Journal Of Pharmaceutical Sciences ( P-issn 1683 - 3597 E-issn 2521 - 3512)
The Spectrophotometric Determination of Olanzapine via Coupling with Diazotized p-Nitroaniline
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A new spectrophotometric method has been developed for the assay of olanzapine (OLN.) in pure and dosage forms. The method is based on the diazocoupling of (OLN.) with diazotized p-nitroaniline in alkaline medium to form a stable brown colored water-soluble azo dye with a maximum absorption at 405 nm.  The variables that affect the completion of reaction have been carefully optimized. Beer’s law is obeyed over the concentration range of (0.5-45.0 μg.mL-1) with a molar absorptivity of 1.5777×104 L.mol-1.cm-1.  The limit of detection was  0.3148  Î¼g.mL-1 and  Sandell’s  sensitivity value was 0.0198 μg.cm-2. The propose

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Publication Date
Sun Sep 01 2013
Journal Name
Baghdad Science Journal
Spectrophotometric Determination of Bismuth(III) with 4-(2-pyridylazo) Resorcinol-Application to Waters and Veterinary Preparation
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This paper describes the development of a simple spectrophotometric determination of bismuth III with 4-(2-pyridylazo) resorcinol (PAR) in aqueous solution in the presence of cetypyridinium chloride surfactant at pH 5 which exhibits maximum absorption at 532 nm. Beer's law is obeyed over the range 5-200 µg/25 mL. i.e. 0.2-8 ppm with a molar absorptivity of 3×104 l.mol-1.cm-1 and Sandell's sensitivity index of 0.0069 µg.cm-2. The method has been applied successfully in the determination of Bi (III) in waters and veterinary preparation.

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Publication Date
Sat Mar 11 2017
Journal Name
Ibn Al-haitham Journal For Pure And Applied Sciences
Simultaneous Determination of Sulfanilamide and Furosemide by Using Derivative Spectrophotometry
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A simple, precise and accurate spectrophotometric method has been developed for simultaneous estimation of sulfanilamide and furosemide in their mixture by using first and second order derivative method in the ultraviolet region. The method depends on first and second derivative spectrophotometry, with zero-crossing and peak to base line and peak area measurements. The first derivative amplitudes at 214, 238 and 266 nm were selected for the assay of sulfanilamide and 240, 260, 284, 314 and 352 nm for furosemide. Peak area at 201222, 222-251 and 251-281 nm selected for estimation of sulfanilamide and at 229-249, 249270, 270-294, 294-333 and 333-382 nm for furosemide. The second derivative amplitudes at 220, 252 and 274 nm for sulfanilamid

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