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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
Sun Mar 01 2015
Journal Name
Baghdad Science Journal
Spectrophotometric determination of Phenylephrine hydrochloride and Salbutamol sulphate drugs in pharmaceutical preparations using diazotized Metoclopramide hydrochloride
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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 l

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Publication Date
Fri Nov 24 2023
Journal Name
Iraqi Journal Of Science
New Turbidimetric-Continuous Flow Injection Analysis Method for The Determination of Chlorpromazine HCl in Pharmaceutical Preparation Using Linear Array Ayah 5SX1-T-1D-CFI Analyser
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A new turbidimetric-flow injection method is described for the determination of chlorpromazine HCl in pure and pharmaceutical preparation. The method is characterized by simplicity, sensitivity and fast, it is based on formation of ion pair compound between chlorpromazine HCl and Potassium hexacyanoferrate(III) in an acid medium for the formation of greenish yellow precipitate. This precipitate was determined using homemade Linear Array Ayah 5SX1-T-1D continuous flow injection analyser. Optimum concentrations of chemical reactants, physical instrumental conditions have been investigated. The linear dynamic range of chlorpromazine HCl was 3-30 mmol.L-1 while correlation coefficient (r) was 0.9929 and percentage linearity (%r2) C.O.D was 9

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Publication Date
Sun Jun 05 2016
Journal Name
Baghdad Science Journal
Flame Atomic Emission and Colorimetric Methods for the Determination of Cephalexin Monohydrate in Pharmaceutical Preparations
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We propose two simple, rapid, and convenient spectrophotometric methods which are described for the determination of cephalexin in bulk and its pharmaceutical preparations. They are based on the measurement of the flame atomic emission of potassium ion (in the first method) and colorimetric determination of the green colored solution at 610 nm formed after the reaction of cephalexin with potassium permanganate as an oxidant agent (in the second method) in basic medium. The working conditions of the methods are investigated and optimized. Beer's law plot shows a good correlation in the concentration range of 5-40?g ml-1. The detection limits are 2.573,2.814 ?g ml-1 for the flame emission photometric method and 1.844,2.016 ?g ml-1 for colo

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Publication Date
Fri Dec 01 2023
Journal Name
Baghdad Science Journal
Simultaneous Determination of Binary Mixture of Estradiol and Progesterone Using Different Spectrophotometric Methods
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Four rapid, accurate and very simple derivative spectrophotometric techniques were developed for the quantitative determination of binary mixtures of estradiol (E2) and progesterone (PRG) formulated as a capsule. Method I is the first derivative zero-crossing technique, derivative amplitudes were detected at the zero-crossing wavelength of 239.27 and 292.51 nm for the quantification of estradiol and 249.19 nm for Progesterone. Method II is ratio subtraction, progesterone was determined at λmax 240 nm after subtraction of interference exerted by estradiol. Method III is modified amplitude subtraction, which was established using derivative spectroscopy and mathematical manipulations. Method IIII is the absorbance ratio technique, absorba

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Publication Date
Sun Sep 06 2009
Journal Name
Baghdad Science Journal
Nitroso-R-salt as a sensitive spectrophotometric reagent for the determination of paracetamol in pharmaceutical preparations
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Nitroso-R-salt is proposed as a sensitive spectrophotometric reagent for the determination of paracetamol in aqueous solution. The method is based on the reaction of paracetamol with iron(III) and subsequent reaction with nitroso-R-salt to yield a green colored complex with maximum absorption at 720 nm. Optimization of the experimental conditions was described. The calibration graph was linear in the concentration range of 0.1 – 2.0 ?g mL-1 paracetamol with a molar absorptivity of 6.9 × 104 L mol-1 cm-1. The method was successfully applied to the determination of paracetamol in pharmaceutical preparations without any interference from common excipients. The method has been statistically evaluated with British Pharmacopoeia method a

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Publication Date
Wed May 31 2017
Journal Name
Ibn Al-haitham Journal For Pure And Applied Sciences
Spectrophotometric Determination of Amiodarone Hydrochloride in Pharmaceutical Preparations
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Amiodarone hydrochloride (AH) has been determined spectrophotometrically Using methyl orange (MO).  In our previous researches MO was used for determination of Mexiletine Hydrochloride [1]. The method based on complexation between MO and AH.  After shaking and diluting the complex solution with D.W, the pH was adjusted with NaOH and HCl to pH 3. The colored complex formed between AH and the reagent were transferred into separating funnels and extracted using 5.5ml CH2Cl2 and were shaken for (5 minutes).  The extracted organic layer was used for preparation of the calibration curves for spectrophotometric measurements of AH at 434nm.  The blanks were carried out in exactly the same way throughout the whole procedure.&n

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Publication Date
Wed Apr 12 2017
Journal Name
Ibn Al-haitham Journal For Pure And Applied Sciences
Spectrophotometric Determination of Mefenamic Acid in Pharmaceutical Preparations
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  A simple, accurate and precise spectrophotometric method has been proposed for the determination of Mefenamic acid(MA) in dosage forms. Proposed  method based on the reaction of cited drug with 1,2-Naphthoquinone-4-Sulfonic sodium (NQS). The optimum experimental condition have been studied. Beer's Law is obeyed in the concentration range 0.5-10.0 µg/mL at 450nm with detection limit of 0.189µg/mL.  Effect of pH, reaction time, and volume of NQS on the determination of Mefenamic acid, have been examined. The proposed method has been successfully applied for the determination of  Mefenamic acid in pharmaceutical preparations.
 

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Publication Date
Sun Mar 06 2011
Journal Name
Baghdad Science Journal
Spectrophotometric Determination of Epinephrine in Pharmaceutical Preparations Using Praseodymium as Mediating Metals
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A simple, accurate and sensitive spectrophotometric method for the determinaion of epinephrine is described . The method is based on the coordination of Pr (III) with epinephrine at pH 6. Absorbance of the resulting orange yellow complex is measured at 482 nm . A graph of absorbance versus concentrations shows that beer 's low is obeyed over the concentration range (1-50)mg.ml-1 of epinephrine with molar absorpitivity of ( 2.180x103 L.mol-1.cm-1 ), a sandell sensitivity of (0.084 mg.cm-2 ), a relative error of (-2.83%) , a corrolation coffecient (r= 0.9989) and recovery % ( 97.03 ± 0.75 ) depending on the concentration.This method is applied to analyse EP in several commercially available pharmaceutical preparations

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Publication Date
Mon Mar 13 2017
Journal Name
Ibn Al-haitham Journal For Pure And Applied Sciences
Indirect Spectrophotometric Determination of Oxymetazoline Hydrochloride in Pharmaceutical Formulation Using Fluorophotometric Method
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This research involves an indirect Fluorophotometric method for the determination of microgram amount of oxymetazoline hydrochloride in the concentration range 0.1-5.0 g/ml. The method is based on the oxidation of the drug by cerium sulphate solution which is acidic medium where Ce IV is reduced to Ce III which can be excited at 259 nm to give an emitted light at 377 nm which  is directly proportional to the concentration of Ce III which is equivalent to Ce IV that is needed to oxidize the studied drug. The average recovery of the method is 100.19% and relative standard deviation (RSD) < 0.37% . The method have been successfully applied to the determination of the studied drug in its pure and pharmaceutical preparations and it wa

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Publication Date
Fri Nov 24 2023
Journal Name
Iraqi Journal Of Science
New Approach for the On-Line Spectrophotometric Determination of Folic Acid in Pure and Pharmaceutical Preparation via Oxidation by Cerium(IV) Sulphate Using Ayah 3Sx3-3D-Solar Cell CFI Spectrophotometer Analyzer
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A newly photometric analytical method characterized by its speed and sensitivity was developed for the determination of folic acid in pure and pharmaceutical samples via its oxidation to reddish-orange coloured complex through oxidation by cerium (IV) sulphate in aqua medium using homemade Ayah 3Sx3-3D-solar cell CFI photometer. The colored species were determined using supper bright green light emitting diode (LED) as a source. A 100μl was taken as a best sample volume for the determination of folic acid. The linearity of calibration curve for the instrument response versus folic acid concentration was 0.005-20 mmol.L-1 while the L.O.D. was 0.5  mol.L-1 from the stepwise dilution for the minimum concentration of lowest concentration

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