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Development and Validation of Spectrophotometric Methods for the Quantitative Determination of Doxycycline Hyclate in Pure Form and Pharmaceutical Formulations Using Flow‐Injection and Batch procedures: A Comparative Study
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Abstract<p>Doxycycline hyclate is an antibiotic drug with a broad‐spectrum activity against a variety of gram‐positive and gram‐negative bacteria and is frequently used as a pharmacological agent and as an effector molecule in an inducible gene expression system. A sensitive, reliable and fast spectrophotometric method for the determination of doxycycline hyclate in pure and pharmaceutical formulations has been developed using flow injection analysis (FIA) and batch procedures. The proposed method is based on the reaction between the chromogenic reagent (V<sup>4+</sup>) and doxycycline hyclate in a neutral medium, resulting in the formation of a yellow compound that shows maximum absorbance at 396 nm. In a batch procedure, the proposed method was validated over the concentration range of 1.0–80 μg mL<sup>−1</sup> with a sampling frequency of 30/h, and commercial pharmaceutical samples were successfully determined. The proposed method was successfully adapted with an FIA system where the peak heights are proportionally connected to doxycycline hyclate over the concentration range of 25–400 μg mL<sup>−1</sup> with a sampling frequency of 50/h. The limits of detection (LOD) and quantification (LOQ) were 0.9 and 10.44 μg mL<sup>−1</sup> and 3.01 and 34.81 μg mL<sup>−1</sup> for batch and FIA respectively. The samples were submitted to an HPLC analysis, and the outcomes demonstrated excellent agreement with the suggested procedures. The adopted FIA procedure allows fast monitoring of doxycycline hyclate in pharmaceutical formulations and it can be used for quality control purposes during the production processes of doxycycline hyclate.</p>
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Publication Date
Fri Oct 20 2023
Journal Name
Ibn Al-haitham Journal For Pure And Applied Sciences
Normal and Reverse Flow Injection Analysis Methods for Estimation of Mesalazine in Pharmaceutical Dosage Forms
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Determining the actual amounts of active ingredients in various pharmaceutical commercial forms is still receiving a lot of attention. Two flow injection analysis (FIA) methods were suggested for determination of mesalazine (MES) in pharmaceutical forms. Normal and reverse FIA systems (nFIA and rFIA) combined with UV-Vis spectrophotometric technique were used for the analysis. The methods involved using two mods of FIA systems for measuring a colored product result from coupling of MES with 2,2'-dihydroxybiphenyl after oxidized with sodium periodate in alkaline medium. The absorbance of the red colored dye was measured at maximum wavelength of 500 nm. The calibration graphs for MES were linear in the ranges 2.5-200 and 0.5-60 µg/mL with

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Publication Date
Sun Jun 11 2017
Journal Name
Ibn Al-haitham Journal For Pure And Applied Sciences
Using of Third and Fourth Order Derivative Spectra to Simultaneous Determination of Olanzapine and Ephedrine in Its Pure and Pharmaceutical Formulations
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 Two new simultaneous spectrophotometric methods for determination of Olanzapine and Ephedrine depend on third (D3) and fourth (D4) derivative of zero spectrum of two drugs were developed. The peak – to- base line, peak to peak and area under peak were found proportional with concentration of the drugs up to (4-24 µg/ml-1) at known experimental wavelengths. The results showed that the method was precise and accurate through  RSD% (0.5026-4.0273),( 0.2399 6.9888) and  R.E %(-2.3889-0.8333) ,) -2.9444-0.2273) while the LOD (0.0057-  0.8510 μg.ml-1), ( 0.0953-0.9844 μg.ml-1) and LOQ (0.0173- 2.5788μg.ml-1),( 0.5774-2.9829 μg.ml-1) were found for the two drugs respectively. The methods were applied i

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Publication Date
Sat Apr 01 2023
Journal Name
Baghdad Science Journal
Development and Validation of a Simple and Sensitive Reverse-Phase High Performance Liquid Chromatographic Method for the Determination of Ibuprofen in Pharmaceutical Suspensions
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The aim of this work was to develop and validate a rapid and low cost method for estimation of ibuprofen in pharmaceutical suspensions using Reverse-Phase High Performance Liquid Chromatography. The proposed method was conducted and validated according to International Conference on Harmonization (ICH) requirements. The chromatographic parameters were as follows: column of octyldecylsilyl C18 with dimensions (150 × 4.6) mm, mobile phase composed of acetonitrile with phosphoric acid with a ratio of 50 to 50 each using isocratic mode, flow rate of 1.5 mL/min and injection volume of 5 μL. The detection was carried out using UV detector at 220 nm. The method was validated and showed short retention time for ibuprofen peak at 7.651 min, wit

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Publication Date
Mon Mar 08 2021
Journal Name
Baghdad Science Journal
Flow injection- Spectrophotometric determination of some catecholamine drugs
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A new spectrophotometric flow injection method has been establish for the determintaions of some catecholaminedrugs

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Publication Date
Thu Dec 29 2016
Journal Name
Ibn Al-haitham Journal For Pure And Applied Sciences
Spectrophotometric Determination of Ketotifen Fumarate in Pure and Pharmaceutical Preperations by Bromophenol Blue Reagent
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         A spectrophotometric reliable, rapid and sensitive method has been developed and validated for  the determination Ketotifen fumarate  . A method was described for the determination of Ketotifen Fumarate  in pure form or pharmaceutical formulations, a colored ion-pair complex formation reaction among ketotifen fumarate and acid-dye bromophenol blue at pH 3.0 was used for the colorimetric determination of the drug. The complex formed was extracted into chloroform and the maximum absorbance of the solution was measured at 413 nm against blank. The calibration curve calculated obey Beer's law over the concentration range of 0.4-16 μg/ml and the regression equation was A=0.069

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Publication Date
Sun Mar 05 2017
Journal Name
Baghdad Science Journal
Spectrophotometric Determination of Bisacodyl in Pure and Pharmaceutical Preparation via Oxidative Coupling Organic Reaction
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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) (

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Publication Date
Sun Dec 03 2017
Journal Name
Journal Of Babylon University
Spectrophotometric Determination of Sulfamethoxazole in Pure and Pharmaceutical Preparations Based on Condensation Reaction Method
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A new, Simple, sensitive and accurate spectrophotometric methods have been developed for the determination of sulfamethoxazole (SMZ) drug in pure and dosage forms. This method based on the reaction of sulfamethoxazole (SMZ) with 1,2-napthoquinone-4-sulphonic acid (NQS) to form Nalkylamono naphthoquinone by replacement of the sulphonate group of the naphthoquinone sulphonic acid by an amino group. The colored chromogen shows absorption maximum at 460 nm. The optimum conditions of condensation reaction forms were investigated by (1) univariable method, by optimizing the effect of experimental variables (different bases, reagent concentration, borax concentration and reaction time), (2) central composite design (CCD) including the effect of

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Publication Date
Mon Apr 20 2020
Journal Name
Ibn Al-haitham Journal For Pure And Applied Sciences
Spectrophotometric Method for the Estimation of Ceftriaxone in Pure Form and Pharmaceuticals
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Ceftriaxone sodium were one of the widely antibacterial drugs used. Azo dye derivatization of diazonium salt that formed via the reaction between ceftriaxone with hydrochloric acid and sodium nitrite was developed for the on-research drug analysis then coupling with each one 2,5-dimethylphenol (2,5-DMP) and 4-tertbutylphenol (4-TBP) respectively in the alkaline media. The developed diazonium coupling methods include an optimization study. The results show a limit of detection and limit of quantification 0.482, 0.284 µg/mL, and 1.607, 0.945 µg/mL using 2,5-DMP and 4-TBP reagents respectively. Moreover, the recovery % obtained was 100.89%, and 103.37% at linear concentration range 3.0 – 50, and 10 – 30 µg/mL, with mo

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Publication Date
Sun Apr 16 2017
Journal Name
Ibn Al-haitham Journal For Pure And Applied Sciences
Univariate and Multivariate Optimization of Spectrophotometric Determination of Europium (III) in Pure Form and Synthetic Sample
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    Two different approaches, univariate and multivariate (simplex method), have been used to obtain the optimum conditions for the quantitative Spectrophotometric determination of Eu3+ using Solochrome violet RS (3-Hydroxy-4-(2-hydroxy phenyl azo) naphthalene -1sulfonic acid) (SVRS) as a chromogenic reagent. The investigation shows that Eu3+ ion forms a wine-red complex with SVRS in alkaline buffer solution having a maximum absorbance at 464 nm against reagent blank.       Calibration graphs obtained under univariate and simplex were found to be linear in the range of (0.30-8.0) µg/ml with detection limit 0.061µg/ml and molar absorptivity of 9877.66 L/mol.cm and (0.40-10.0)µg/ml with

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Publication Date
Mon Apr 01 2019
Journal Name
International Journal Of Pharmaceutical Research
Sensitive spectrophoto metric determination of doxycycline in pure and dosage forms using p-bromanil
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A simple, precise, and sensitive spectrophotometric method has been established for the analysis of doxycycline. The method includes direct charge transfer complexation of doxycycline withp-Bromanil in acetonitrileto form a colored complex. The intensely colored product formed was quantified based on the absorption band at 377 nm under optimum condition. Beer’s law is obeyed in the concentration range of 1–50 μg.mL-1 with molar absorptivity of 1.5725x104 L.mol-1.cm-1, Sandell's sensitivity index (0.0283) μg.cm-2, detection limit of 0.1064 μg.mL-1, quantification limit 0.3224 μg.mL-1 and association constant of the formed complex (0.75x103). The developed method could find application in routine quality control of doxycycline and has

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