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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
Sat Jan 01 2022
Journal Name
Chemical Methodologies
Determination of the Quantity of Losartan Active Ingredient in the Medication Formulations via Turbidimetric-Flow Injection Technique
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Publication Date
Tue Mar 14 2017
Journal Name
Ibn Al-haitham Journal For Pure And Applied Sciences
Spectrophotometric Method for the Determination of Tetracycline and Doxycycline by Oxidizing Coupling Reaction with 4-aminoantipyrine
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 A simple,  sensitive, accurate and low cost effective spectrophotometric method has been developed for the determination of Tetracycline and Doxycycline in pure and pharmaceutical formulations. The method is based on the reaction of methyldopa with 4-aminoantipyren (4-AAP) in presence of potassium ferriecyanide (PFC) in an alkaline medium. Two optimization methods were applied to determine the optimum conditions of oxidizing coupling reaction variables; univariate and design of experiment (DOE) method. The conditions effecting the  reaction; pH, buffer Volume,   reagent concentration, oxidant concentration, type of buffer, order of addition, time of reaction and stability were optimized . Under univariate and design

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Publication Date
Sun Jun 07 2015
Journal Name
Baghdad Science Journal
Spectrophotometric Determination of Paracetamol in bulk and Pharmaceutical Preparations
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A simple, and rapid spectrophotometric method for the estimation of paracetamol has been developed. The methods is based on diazotisation of 2,4-dichloroaniline followed by a coupling reaction with paracetamol in sodium hydroxide medium. All variables affecting the reaction conditions were carefully studied. Beer's law is obeyed in the concentration range of 4-350 ?gml?1 at 490 nm .The method is successfully employed for the determination of paracetamol in pharmaceutical preparations. No interferes observed in the proposed method. Analytical parameters such as accuracy and precision have been established for the method and evaluated statistically to assess the application of the method.

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Publication Date
Fri Dec 08 2023
Journal Name
Iraqi Journal Of Science
Determination of Atenolol in pharmaceutical formulations by continuous flow injection analysis via turbidimetric (T180o) and scattered light effect at two opposite position (2N90o ) using Ayah 4SW-3D-T180 -2N90 -Solar - CFI
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A simple, rapid and sensitive method for the analysis of Atenolol in pure and pharmaceutical preparation as an alternative analytical procedure were developed by continuous flow injection analysis via turbidimetric (T180o) and scattered light effect at two opposite position (2N90o). The method is based upon the formation of white precipitate for the ion pair compound by phosphomolybidic acid with Atenolol in aqueous medium. The precipitate is measured via the attenuation of incident light and scattering of the incident light in two opposite direction namely +90o and -90o angle were measured. Chemical and physical parameters were investigated. The linearity of Atenolol is ranged from (0.1-11) mmol.L-1, with correlation coefficient r=0.993

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Publication Date
Fri Sep 25 2020
Journal Name
International Journal Of Drug Delivery Technology
Simultaneous Determination of Trace Mefenamic Acid in Pharmaceutical Samples via Flow Injection Fluorometry
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Mefenamic acid belongs to non-steroidal anti-inflammatory drugs that are used widely for the treatment of analgesia. Our aim from this study is to establish a new assay for the quantitative determination of mefenamic acid (MFA) in the pharmaceutical sample by two sensitive and rapid flow injection-fluorometric methods. A homemade fluorometer was used in fluorescence measurements, which using solid-state laser diode 405 and 532 nm as a source, combined with a continuous flow injection technique. The first method depends on the effect of MFA on calcein blue (CLB) fluorescence at 405 nm. Another method is a study of rhodamine-6G (Rh-6G) fluorescence after adding MFA, and recording at 532 nm. Optimum parameters as fluorescent dye concen

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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
Mon Mar 01 2021
Journal Name
Journal Of Applied Spectroscopy
SPECTROPHOTOMETRIC METHOD FOR THE DETERMINATION OF METOCLOPRAMIDE IN PHARMACEUTICAL FORMS
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A UV-Vis spectrophotometry method was developed for the determination of metoclopramide hydrochloride in pure and several pharmaceutical preparations, such as Permosan tablets, Meclodin syrups, and Plasil ampoules. The method is based on the diazotization reaction of metoclopramide hydrochloride with sodium nitrate and hydrochloric acid to yield the diazonium salt, which is then reacted with 3,5-dimethyl phenol in the presence of sodium hydroxide to form a yellow azo dye. Calibration curves were linear in the range from 0.3 to 6.5 µg/mL, with a correlation coefficient of 0.9993. The limits of detection and quantification were determined and found to be 0.18 and 0.61 µg/mL, respectively. Accuracy and precision were also determined b

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Publication Date
Sun Sep 01 2013
Journal Name
Baghdad Science Journal
A sensitive spectrophotometric determination of tadalafil in pharmaceutical preparations and industrial wastewater samples
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A simple, accurate, precise, rapid, economical and a high sensitive spectrophotometric method has been developed for the determination of tadalafil in pharmaceutical preparations and industrial wastewater samples, which shows a maximum absorbance at 204 nm in 1:1 ethanol-water. Beer's law was obeyed in the range of 1-7?g/ mL ,with molar absorptivity and Sandell ? s sensitivity of 0.783x105l/mol.cm and 4.97 ng/cm2respectively, relative standard deviation of the method was less than 1.7%, and accuracy (average recovery %) was 100 ± 0. 13. The limits of detection and quantitation are 0.18 and 0.54 µg .ml-1, respectively. The method was successfully applied to the determination of tadalafil in some pharmaceutical formulations

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Publication Date
Mon Jun 10 2019
Journal Name
Chemistry &chemical Technology
Quantitative Determination of Ephedrine Hydrochloride in Pharmaceutical Injections by Highly Sensitive Turbidimetric and Reversed-Phase Combined with UFLC Methods
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In this paper, turbidimetric and reversed-phase ultra-fast liquid chromatography (UFLC) methods were described for the quantitative determination of ephedrine hydrochloride in pharmaceutical injections form. The first method is based on measuring the turbidimetric values for the formed yellowish white precipitate in suspension status in order to determine the ephedrine hydrochloride concentration. The suspended substance is formed as a result of the reaction of ephedrine hydrochloride with phosphomolybdic acid which was used as a reagent. The physical and chemical characteristics of the complex were investigated. The calibration graphs of ephedrine were established by turbidity method. While the second method (UFLC) was conducted using the

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Publication Date
Thu Jun 01 2023
Journal Name
Baghdad Science Journal
Simultaneous Determination of Piroxicam and Codeine Phosphate Hemihydrate in a Pharmaceutical Dosage Form Using Validated HPLC Method
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An easy, eclectic, precise high-Performance Liquid Chromatographic (HPLC) procedure was evolved and validated to estimate of Piroxicam and Codeine phosphate. Chromatographic demarcation was accomplished on a C18 column [Use BDS Hypersil C18, 5μ, 150 x 4.6 mm] using a mobile phase of methanol: phosphate buffer (60:40, v/v, pH=2.3), the flow rate was 1.1 mL/min, UV detection was at 214 nm. System Suitability tests (SSTs) are typically performed to assess the suitability and effectiveness of the entire chromatography system. The retention time for Piroxicam was found to be 3.95 minutes and 1.46 minutes for Codeine phosphate. The evolved method has been validated through precision, limit of quantitation, specificity,

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