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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
Wed May 24 2017
Journal Name
Ibn Al-haitham Journal For Pure And Applied Science
Direct and Indirect Spectrophotometric Determination of Paracetamol in Pharmaceutical Preparations By Oxidative Coupling With p-Amino-2-hydroxy Sodium Benzoate
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New simple and sensitive spectrophotometric methods for the determination of paracetamol in aqueous medium were developed. The first method is based on coupling of paracetamol with p-amino-2-hydroxy sodium benzoate (AHB) in the presence of sodium periodate, as oxidizing agent, to form a brownish-orange compound which shows a λmax at 470 nm. The molar absorptivity (εmax) of the colored product was found to be (3371) l. mole1. cm-1 and Sandel’s index 0.0449 μg. cm-2. The method follows Beer’s law in the concentration range of 12.5-500.0 μg of paracetamol in a final volume of 25 ml (0.5-20.0) μg. ml-1 with relative standard deviation percent (RSD%) ranged between 0.26-4.71% and accuracy, expressed by recovery percent, 95-106% for five

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Publication Date
Wed May 24 2017
Journal Name
Ibn Al-haitham Journal For Pure And Applied Sciences
Direct and Indirect Spectrophotometric Determination of Paracetamol in Pharmaceutical Preparations By Oxidative Coupling With p-Amino-2-hydroxy Sodium Benzoate
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 New simple and sensitive spectrophotometric methods for the determination of paracetamol in aqueous medium were developed. The first method is based on coupling of paracetamol with p-amino-2-hydroxy sodium benzoate (AHB) in the presence of sodium periodate, as oxidizing agent, to form a brownish-orange compound which shows a λmax at 470 nm. The molar absorptivity (εmax) of the colored product was found to be (3371) l.mole1.cm-1 and Sandel’s index 0.0449 μg.cm-2. The method follows Beer’s law in the concentration range of 12.5-500.0 μg of paracetamol in a final volume of 25 ml (0.5-20.0) μg.ml-1 with relative standard deviation percent (R.S.D%) ranged between 0.26-4.71% and accuracy, expressed by recover

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Publication Date
Sun Mar 07 2010
Journal Name
Baghdad Science Journal
Spectrophotometric determination of metoclopramide hydrochloride in pharmaceutical tablets, by diazotization-coupling method with 1-naphthol as the coupling agent
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Simple, rapid and sensitive spectrophotometric method was proposed for the analysis of metoclopramide hydrochloride (MPH) in pure form as well as in pharmaceutical tablets. The method is based on the diazotization reaction of MPH with sodium nitrite in hydrochloric acid medium to form diazonium salt, which is coupled with 1-naphthol in sodium hydroxide medium to form azo dye, showing absorption maxima at 550 nm. Beer’s law is obeyed in the concentration range of 0.4 – 18 µg mL-1 of MPH with detection limit 0.5448 µg mL-1. The molar absorptivity and Sandell’s sensitivity are 3.4969 × 104 L mol-1 cm-1 and 0.0101 µg cm-2, respectively. The method was successfully applied to the determination of MPH in pharmaceutical tablets with

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Publication Date
Sun Mar 02 2014
Journal Name
Baghdad Science Journal
With Solvent Extraction Method, and via new Organic Reagent 2-(Benzo thiazolyl azo)-4,5- Diphenyl Imidazole for Spectrophotometric Determination of Copper (II) in different Samples
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The new organic reagent 2-[Benzo thiazolyl azo]-4,5-diphenyl imidazole was prepared and used as complexing agent for separation and spectrophotometric determination of Cu2+ ion in some samples include plants, soil, water and human blood serum. Initially determined all factors effect on extraction method and the results show optimum pH was (pHex=9), optimum concentration was 40?g/5mLCu2+ and optimum shaking time was (15min.), as well stoichiometry study appears the complex structure was 1:1 Cu2+: BTADPI. Interferences effect of cations were studied. Synergism effect shows MIBK gave increasing in distribution ratio (D). Organic solvent effect appears there is no any linear relation between dielectric constant for organic solvent used and dis

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Publication Date
Wed Jun 30 2021
Journal Name
Iraqi Journal Of Market Research And Consumer Protection
SPECTROPHTOTOMETRIC DETERMINATION OF PURE SULFAMETHOXAZOLE IN PHARMACEUTICAL PREPARATIONS BY OXIDATIVE COUPLING REACTION: SPECTROPHTOTOMETRIC DETERMINATION OF PURE SULFAMETHOXAZOLE IN PHARMACEUTICAL PREPARATIONS BY OXIDATIVE COUPLING REACTION
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            A new, simple, rapid and sensitive spectrophotometric method for the determination of sulfamethoxazole in both pure form and pharmaceutical preparations has been reported.The adapted technique based on utilization 4-aminobenzene sulfonic acid as a new modern chromogenic through an oxidative coupling reaction with sulfamethoxazole and potassium iodate in basic media to form orange soluble dye product with absorption maxima at 490 nm. Subject to Beer's law in the range 2–32μg mL-1. The values of molarabsorption coefficient (ε) and correlation coefficient were found to be 9.118 × 103 and0.9999 respectively whereas the Sandels index was

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Publication Date
Sun Sep 01 2013
Journal Name
Baghdad Science Journal
Synthesis ,spectroscopic study of Antipyryl azo 2-Naphthol and use it as new reagent for determination of Co(II) and Cu(II)
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A simple ,accurate and sensitive spectrophotometric method has been developed the determination of Cobalt(II) and Cupper (II) .The method is based on the chelation of Co(II) and Cu(II) ions with 4-(4´-pyrazolon azo) -2-Naphthol(APAN) in aqueous medium . The complexes have a maximum absorption at (513) and (506) nm and ? max 0.531×10 4 and 0.12×10 5 L.mol -1.cm -1 for Co(II) and Cu(II) respectively .The reagent and two complexes have been prepared in ethanolic solution.The stoichiometry of both complexes were found to be 1:2 (metal :legend) .The effects of various cations and anions on Co(II) and Cu(II) determination have been investigated .The stability constants and standard deviations for Co(II) and Cu(II) 0.291 x107 ,0.909X108 L.mol

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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
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
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
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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