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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 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
Tue Apr 24 2018
Journal Name
Ibn Al-haitham Journal For Pure And Applied Sciences
Use of Acidic Hydrolysis and Diazo Coupling Reaction for Spectrophotometric Determination of Furosemide in Urine and Pharmaceutical Formulation.
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     Simple and rapid spectrophotometric determination of furosemide (FUR) has been investigated .The method is based on acid hydrolysis of FUR to free primary aromatic amine and diazotization followed by coupling with 3, 5 di methyl phenol (3, 5-DMPH) at basic medium. The absorbance was measured at 434 nm, the method was optimized for best condition, and beers’ law is obeyed over the range of 0.4-50 µg.mL-1 with molar absorptivity and sandal’s sensitivity 1.3899 x104 L moL-1 .cm-1 and 0.0238x104 µg.cm-2 respectively. Analysis of solution containing nineteen different concentrations of FUR gave a correlation coefficient of (0.9999) a

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Publication Date
Sun Feb 27 2011
Journal Name
University Of Baghdad
Determination of Cimetidine and Erythromycin ethylsuccinate Drugs Using Different Spectrophotometric Methods (Ph.D. Thesis)
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In this study, four different spectrophotometric methods were applied for determination of cimetidine and erythromycin ethylsuccinate drugs in pure form and in their pharmaceutical preparations. The suggested methods are simple, sensitive, accurate, not time consuming and inexpensive. The results showed the following: The first method: Based on the formation of ion pair complex of each drug with bromothymol blue (BTB) as a chromogenic reagent. The formed complexes were extracted with chloroform and their absorbance values were measured at 427.5 nm for cimetidine and 416.5nm for erythromycin ethylsuccinate; against their reagents blanks. Two different methods, univariate method and multivariate method, were used to obtain the optimum condit

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Publication Date
Sun Jun 01 2025
Journal Name
Baghdad Science Journal
Development of Spectrophotometric Method for Determination of Chlorpromazine-Hydrochloride in Pharmaceutical Preparations Via Use Ion-Exchange to Overcome the Interfering Ions
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Publication Date
Mon Jun 17 2019
Journal Name
Ibn Al-haitham Journal For Pure And Applied Sciences
Determination of Manganese (II) using Flow Injection Analysis with Chemiluminescence detection
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The determination of manganese (II) using flow injection analysis with chemiluminescence detection was investigated. Mn2+ in sample solutions injected into a carrier stream of sodium bismuthate (NaBiO3) were oxidised to form MnO4- ions which were capable of producing luminescence after reaction with luminol/KOH in a flow cell. The linear range of the system is from 20 to 80 mg/L with a detection limit 8 mg/L. The proposed system is suitable for determination of Mn2+ in steel alloys after dissolution, filtration and dilution at a rate of approximately 60 samples per hour with a relative standard deviation (RSD)1.2%. Statistical comparison between the proposed system and standard spectrophotometric method revealed that there is no signific

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Publication Date
Sun Apr 29 2012
Journal Name
Journal Of Karbala University
Optimization Quantitative Determination of Cimetidine in Pharmaceutical Preparations via Bromothymol Blue Using Central Composite Design
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Publication Date
Mon May 22 2017
Journal Name
Ibn Al-haitham Journal For Pure And Applied Sciences
Spectrophotometric Determination of Isoptin (Verapamil Hydrochloride) in Pharmaceutical Preparations
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Verapamil Hydrochloride (VH) has been determined spectrophotometrically by using Methyl Orange (MO).  In our previous researches MO was used for determination of Mexiletine Hydrochloride [1]. The method was based on complexation between (MO and VH).  After shaking and diluting the complex solution with D.W, the pH was adjusted with NaOH and HCl to pH 4. The colored complex formed between VH and the reagents were transferred into separating funnels and extracted using 4.5 ml CH2Cl2 and were shaken for (4 minutes).  The extracted organic layer was used for the preparation of the calibration curves for spectrophotometric measurements of VH at 437nm.  The blanks were carried out in exactly the same way throughout the whol

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Publication Date
Sun Dec 03 2017
Journal Name
Baghdad Science Journal
Synthesis New Liquid Selective Electrodes of Ciprofloxacin Hydrochloride for Determination Ciprofloxacin in Pure form and Pharmaceuticals Preparation.
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New membrane electrodes for determination of ciprofloxacin hydrochloride were prepared depending on ciprofloxacin hydrochloride - phosphotungstic acid (CFH-PT) as an active material and these electrodes were made with three plasticizers: Di-octylphenylphosphonate(DOPH), Di-butyl phosphate (DBP)Tri-n-butyl phosphate(TBP), in PVC matrix. One of the ciprofloxacin electrodes was gave Nernstian slope equal to 57.21 mV/ decade for DOPH membrane with concentration range from 1.5×10-5 to1.0×10-1 M, and detection limit equal to 1.5×10-6 M .Lifetime was 93 days. Non- Nernstian responses equal to 39.40 and 30.70 mV/ decade for membranes DBP, TBP, respectively. These electrodes were gave concentration range from 1.0× 10-5 to 1.0×10-2 and from 4.0

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Publication Date
Mon Jun 01 2020
Journal Name
Journal Of Analytical Chemistry
Ion Pair-dispersive Liquid–Liquid Microextraction Combined with Spectrophotometry for Carbamazepine Determination in Pharmaceutical Formulations and Biological Samples
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A simple, economical and selective method employing ion pair dispersive liquid−liquid microextraction (DLLME) coupled with spectrophotometric determination of carbamazepine (CBZ) in pharmaceutical preparations and biological samples was developed. The method is based on reduction of Mo(VI) to Mo(V) using a combination of ammonium thiocyanate and ascorbic acid in acidic medium to form a red binary Mo(V) thiocyanate complex. After addition of CBZ to the complex, extraction of the formed CBZ−Mo(V)−(SCN)6 was performed using a mixture of methylene chloride and methanol. Then, the measurement of target complex was performed at the wavelength of 470 nm. The important extraction parameters affecting the efficiency of DLLME were studied and o

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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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