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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
Wed Sep 01 2021
Journal Name
Baghdad Science Journal
Determination of Sulfacetamide Sodium in Pure and Their Pharmaceutical Formulations by Using Cloud Point Extraction Method
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      In this study, simple, low cost, precise and speed spectrophotometric methods development for evaluation of sulfacetamide sodium are described. The primary approach contains conversion of sulfacetamide sodium to diazonium salt followed by a reaction with p-cresol as a reagent in the alkaline media.  The colored product has an orange colour with absorbance at λmax 450 nm. At the concentration range of (5.0-100 µg.mL-1), the Beer̆ s Low is obeyed with correlation coefficient (R2= 0.9996), limit of detection as 0.2142 µg.mL-1, limit of quantification as 0.707 µg.mL-1 and molar absorptivity as 1488.249 L.mol-1.cm-1. The other approach, cloud point extraction w

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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)
Spectrophotometric Determination of Nitrofurantoin Drug in its Pharmaceutical Formulations Using MBTH as a Coupling Reagent
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A direct, sensitive and efficient spectrophotometric method for the determination of nitrofurantoin
drug (NIT) in pure as well as in dosage form (capsules) was described. The suggested method was
based on reduction NIT drug using Zn/HCl and then coupling with 3-methyl-2-benzothiazolinone
hydrazone hydrochloride (MBTH) in the presence of ammonium ceric sulfate. Spectrophotometric
measurement was established by recording the absorbance of the green colored product at 610 nm.
Using the optimized reaction conditions, beer’s law was obeyed in the range of 0.5-30 μg/mL, with
good correlation coefficient of 0.9998 and limits of detection and quantitation of 0.163 and 0.544
μg/mL, respectively. The accuracy and

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Publication Date
Sat Jan 27 2024
Journal Name
History Of Medicine
Developing and Validating a Spectrophotometric Method for Estimating Antifungal (Nystatin) in its Pure Form Pharmaceutical Formulation Using Tetrachloro-1,4 benzoquinone
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The UV−VIS absorption spectroscopy technique was used to study the formation of a new complex of charge transfer (CT) between bioactive organic molecules as (Nystatin) containing both a π-electrons from a conjugated system and lone-pair of electrons (amine) with Tetrachloro-1,4 benzoquinone (TCBQ) as a π-acceptor in which the transferred electron goes into its vacant anti-bonding molecular orbitals. The Tyrian purple-colored complex formed was quantitatively measured at 544 nm. This complex shows obeying Beer's law within the concentration range of (10-90) μg.ml-1The stoichiometry of the formed complex between the (Nys.) and (TCBQ) was found 1:2 as evaluated by continuous variation (Job's method) and mole ratio method The value of mola

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Publication Date
Sun Jun 21 2020
Journal Name
Baghdad Science Journal
Spectrophotometer Determination of Cefixime in pure form and pharmaceutical preparation by Using Cloud point Extraction
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Two simple methods spectrophotometric were suggested for the determination of Cefixime (CFX) in pure form and pharmaceutical preparation. The first method is based without cloud point (CPE) on diazotization of the Cefixime drug by sodium nitrite at 5Cº followed by coupling with ortho nitro phenol in basic medium to form orange colour. The product was stabilized and measured 400 nm. Beer’s law was obeyed in the concentration range of (10-160) μg∙mL-1 Sandell’s sensitivity was 0.0888μg∙cm-1, the detection limit was 0.07896μg∙mL-1, and the limit of Quantitation was 0.085389μg∙mL-1.The second method was cloud point extraction (CPE) with using  Trtion X-114 as surfactant. Beer

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Publication Date
Sun Jun 07 2015
Journal Name
Baghdad Science Journal
Flow Injection Spectrophotometric Determination of Thymol using 4-Aminoantipyrine and Copper(II) Nitrate
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Flow-injection (FI) spectrophotometric method has been developed for the analysis of thymol in pharmaceutical preparations. The method is based on organic coupling reaction between thymol and 4-amino antipyrine in the presence of alkaline medium to form an intense stable red color complex with copper nitrate that has a maximum absorption at 490 nm. Optimum conditions for determination of the drug was investigated .The calibration graph was linear over the range of 5-500 µg.ml-1 of thymol . The limit of detection (LOD) and limit of quantification (LOQ) were 1.81 ?g mL-1 and 3.60 ?g mL-1 respectively .The proposed method was applied satisfactorily to the determination of thymol in mouth wash preparations. The procedure is characterized by

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Publication Date
Sat Dec 30 2023
Journal Name
Iraqi Journal Of Science
Flow Injection- Spectrophotometric Determination of Salbutamol Sulphate and Pyridoxine Hydrochloride Using 2,4-Dinitrophenylhydrazine
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A batch and flow injection (FI) methods with spectrophotometric detection is proposed for determining of two of phenolic drugs: salbutamol sulphate(SLB)and pyridoxine hydrochloride(PYD) in pure and in pharmaceutical formulations. The methods utilized an oxidative-coupling reaction based upon oxidation of 2,4-dinitrophenylhydrazine (DNPH) with sodium periodate, where an electrophilic intermediate (diazonium salt of the reagent) is produced, which couples with either SLB or PYD in the presence of sodium hydroxide yielding a highly colored condensation product. The absorbance is measured after 15min at 525and515 nm for SLB and PYD respectively. Calibration graphs for both batch and FIA methods were linear over the concentration ranges of 1-

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Publication Date
Mon Sep 25 2017
Journal Name
Ibn Al-haitham Journal For Pure And Applied Sciences
Spectrophotometric Determination of Cefotaxime via Diazotization Reaction in Pure and Pharmaceutical Samples
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      An accurate and sensitive spectrophotometric method has been developed for the determination of cefotaxime (CEF) in pure and pharmaceutical samples. The suggested method depended on the coupling reaction between diazotized cefotaxime and 3,5-dimethyl phenol (3,5-DMPH) in basic medium to form light orange, water soluble dye, that is stable and has a maximum absorbance at 497nm. The calibration graph was liner over the concentration range (1-70) µg.mL-1 with LOD of 0.750 µg.mL-1 and LOQ of. 2.740 µg. mL-1, sandal sensitivity of 0.0526 µg. cm-2 . molar absorptivity 11328 Lmol-1 cm-1 . The stoichiometry composition was found by Jobs a

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Publication Date
Sat Apr 01 2023
Journal Name
Baghdad Science Journal
Spectrophotometric Analysis of Vancomycin Hydrochloride in Pure and Pharmaceutical Injections via Batch and Cloud Point Extraction Techniques
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Development of a precise and delicate reaction has been acquired for the determination of vancomycin hydrochloride using batch and cloud point extraction (CPE) methods. The first method is based on the formation of azo dye as a result of diazotized dapsone coupled with vancomycin HCl (VAN) in a basic medium. The sensitivity of this reaction was enhanced by utilizing a nonionic surfactant (Triton X-114) and the cloud point extraction technique (second method). The azo dye formed was extracted into the surfactant-rich phase, dissolved in ethanol and detected at λmax 440 nm spectrophotometrically. The reaction was investigated using both batch and CPE methods (with and without extraction), and a simple comparison between the two

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Publication Date
Sun Dec 01 2013
Journal Name
Baghdad Science Journal
Flow injection analysis for the photometric determination of promethazine-HCl in pure and pharmaceutical preparation via oxidation by persulphate using Ayah 3SX3-3D solar micro photometer
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The first flow injection spectrophotometric method is characterized by its speed and sensitivity which have been developed for the determination of promethazine-HCl in pure and pharmaceutical preparation. It is based on the in situ detection of colored cationic radicals formed via oxidation of the drug with sodium persulphate to pinkish-red species and the same species was determined by using homemade Ayah 3SX3-3D solar flow injection photometer. Optimum conditions were obtained by using the high intensive green light emitted diode as a source. Linear dynamic range for the absorbance versus promethazine-HCl concentration was 0-7 mmol.L-1, with the correlation coefficient (r) was 0.9904 while the percentage linearity (r2%) was 98.09%. the L.

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Publication Date
Thu Jul 01 2021
Journal Name
Journal Of Pharmaceutical And Biomedical Analysis
An optoelectronic flow-through detectors for active ingredients determination in the pharmaceutical formulations
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An optoelectronic flow-through detector for active ingredients determination in pharmaceutical formulations is explained. Two consecutive compact photodetector’s devices operating according to light-emitting diodes-solar cells concept where the LEDs acting as a light source and solar cells for measuring the attenuated light of the incident light at 180˚ have been developed. The turbidimetric detector, fabricated of ten light-emitting diodes and five solar cells only, integrated with a glass flow cell has been easily adapted in flow injection analysis manifold system. For active ingredients determination, the developed detector was successfully utilized for the development and validation of an analytical method for warfarin determination

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