scholarly journals New Sensitive Kinetic Spectrophotometric Methods for Determination of Omeprazole in Dosage Forms

2009 ◽  
Vol 2009 ◽  
pp. 1-11 ◽  
Author(s):  
Ashraf M. Mahmoud

New rapid, sensitive, and accurate kinetic spectrophotometric methods were developed, for the first time, to determine omeprazole (OMZ) in its dosage forms. The methods were based on the formation of charge-transfer complexes with both iodine and 2,3-dichloro-5,6-dicyano-1,4-benzoquinone (DDQ). The variables that affected the reactions were carefully studied and optimized. The formed complexes and the site of interaction were examined by UV/VIS, IR, and1H-NMR techniques, and computational molecular modeling. Under optimum conditions, the stoichiometry of the reactions between OMZ and the acceptors was found to be 1 : 1. The order of the reactions and the specific rate constants were determined. The thermodynamics of the complexes were computed and the mechanism of the reactions was postulated. The initial rate and fixed time methods were utilized for the determination of OMZ concentrations. The linear ranges for the proposed methods were 0.10–3.00 and 0.50–25.00   with the lowest LOD of 0.03 and 0.14   for iodine and DDQ, respectively. Analytical performance of the methods was statistically validated; RSD was <1.25% for the precision and <1.95% for the accuracy. The proposed methods were successfully applied to the analysis of OMZ in its dosage forms; the recovery was 98.91–100.32%  0.94–1.84, and was found to be comparable with that of reference method.

2014 ◽  
Vol 2014 ◽  
pp. 1-12 ◽  
Author(s):  
Mohammed G. Abdel Wahed ◽  
Ragaa El Sheikh ◽  
Ayman A. Gouda ◽  
Sayed Abou Taleb

Simple, sensitive, and accurate kinetic spectrophotometric method was proposed for the determination of gemifloxacin mesylate (GMF) and moxifloxacin hydrochloride (MOX) in pure forms and pharmaceutical preparations (tablets). The method is based on coupling the studied drugs with 4-chloro-7-nitrobenzo-2-oxa-1,3-diazole (NBD-Cl) in the presence of alkaline borate buffer. Spectrophotometric measurement was achieved by recording the absorbance at 466 and 464 nm for GMF and MOX, respectively, after a fixed time of 20 and 15 min on a water bath adjusted at 70 ± 5°C for both drugs. The different experimental parameters affecting the development and stability of the color were carefully studied and optimized. The absorbance-concentration plots were linear over the ranges 0.5–8.0 and 2.0–12 μg mL−1for GMF and MOX, respectively. The limit of detection of the kinetic method was about 0.12 (2.47 × 10−7 M) and 0.36 (8.22 × 10−7 M) μg mL−1for GMF and MOX, respectively. The proposed methods have been applied and validated successfully with percentage relative standard deviation (RSD% ≤ 0.52) as precision and percentage relative error (RE% ≤ 1.33) as accuracy. The robustness of the proposed method was examined with recovery values that were 97.5–100.5 ± 1.3–1.9%. Statistical comparison of the results with the reference spectrophotometric methods shows excellent agreement and indicates no significant difference in accuracy or precision.


2021 ◽  
Author(s):  
Shaza Affas ◽  
Amir Alhaj Sakur

Abstract Background: simple, sensitive, free of organic solvents, kinetic spectrophotometric method has been developed for the determination of Clindamycin Hydrochloride, both in pure form and Capsules. Method used is based on reaction of Clindamycin with potassium iodide and potassium iodate in aqueous medium at (25 ±2 °c) to produce yellow colored tri iodide ions (I3-). the reaction is followed spectrophotometrically by measuring the absorbance at 350 nm wavelength during 40 minutes. Results: the effects of analytical parameters on reported kinetic methods were investigated. Under the optimized conditions, the initial rate and fixed time (at 10 min) methods were used for constructing the calibration graphs. The graphs were linear in concentration ranges 1-20 μg.ml-1 with limit of detection of 0.12 and 0.22 μg ml-1for the initial rate and fixed time methods, respectively. The results were satisfactory and the analytical performance for both methods was validated. Conclusion: The proposed methods have been applied to determine the components in capsules with an average recovery of 98.25% to 102.00% and the results are in good agreement with those found by the reference method.


2012 ◽  
Vol 9 (3) ◽  
pp. 1645-1654 ◽  
Author(s):  
K. Raghubabu ◽  
L. Shanti Swarup ◽  
B. Kalyanaramu ◽  
M. N. Rao ◽  
C. Ramdas

Two simple, sensitive and cost effective visible spectrophotometric methods (M1 and M2) have been developed for the determination of venlafaxine hydrochloride from bulk and tablet dosage forms. The method M1 is based on the formation of green colored coordination complex by the drug with cobalt thiocyanate which is quantitatively extractable into nitro benzene with an absorption maximum of 626.4 nm. The method M2 involves internal salt formation of aconitic anhydride, dehydration product of citric acid [CIA] with acetic anhydride [Ac2O] to form colored chromogen with an absorption maximum of 561.2 nm. The calibration graph is linear over the concentration range of 10-50 µg/mL and 8-24 µg/mL for method M1 and M2 respectively. The proposed methods are applied to commercial available tablets and the results are statistically compared with those obtained by the reference method and validated by recovery studies. The results are found satisfactory and reproducible. These methods are applied successfully for the estimation of the venlafaxine hydrochloride in the presence of other ingredients that are usually present in dosage forms.


2002 ◽  
Vol 85 (4) ◽  
pp. 817-823 ◽  
Author(s):  
Sheikha M Al-Ghannam ◽  
Fathalla Belal

Abstract A simple kinetic procedure is described for the determination of atenolol in its dosage forms. The procedure is based on coupling the drug with 4-chloro-7-nitrobenzo-2-oxa-1,3-diazole in pH 8 borate buffer at the boiling temperature for a fixed time of 30 min, and then measuring the absorbance of the reaction product at 460 nm. The absorbance–concentration plot is rectilinear over the range 5–50 μg/mL with a minimum detection limit of 1.3 μg (4.9 × 10−6M). The determination of atenolol by the fixed-concentration and rate-constant methods is also feasible with the calibration equations obtained, but the fixed-time method proved to be more applicable. The procedure was applied successfully to commercial tablets, and statistical analysis showed that the results compared favorably with those obtained by the official methods. The interference likely to be introduced from some coformulated drugs and the effect of sensitizers and surfactants on the performance of the proposed method were also studied. A proposed reaction pathway is presented.


BMC Chemistry ◽  
2021 ◽  
Vol 15 (1) ◽  
Author(s):  
Shaza Affas ◽  
Amir Alhaj Sakur

Abstract Background simple, sensitive, free of organic solvents, kinetic spectrophotometric method has been developed for the determination of Clindamycin Hydrochloride, both in pure form and Capsules. Method is based on reaction of Clindamycin with potassium iodide and potassium iodate in an aqueous medium at (25 ± 2 °C) to produce yellow-coloured tri iodide ions (I3−). The reaction is followed spectrophotometrically by measuring the absorbance at wavelength 350 nm during 40 min. Results the effects of analytical parameters on reported kinetic methods were investigated. Under the optimized conditions, the initial rate and fixed time (at 10 min) methods were used for constructing the calibration graphs. The graphs were linear in concentration ranges 1–20 μg ml−1 with limit of detection of 0.12 and 0.22 μg ml−1for the initial rate and fixed time methods, respectively. The results were satisfactory and the analytical performance for both methods was validated. Conclusion The proposed methods have been applied to determine the components in capsules with an average recovery of 98.25–102.00% and the results are in good agreement with those found by the reference method.


2010 ◽  
Vol 93 (2) ◽  
pp. 510-515 ◽  
Author(s):  
Serap Saglik Aslan ◽  
Betul Demir

Abstract Two kinetic spectrophotometric methods were developed for determination of ciprofloxacin (CIP) in a pharmaceutical preparation. The methods are based on oxidation of CIP with potassium permanganate in alkaline media and measurement of the enhancement in the absorbance of manganate ion at 603 nm by spectrophotometry. The calibration graphs were constructed using the initial rate and fixed time methods. The linearity range for concentrations of CIP was found to be 4.020.0 g/mL. The RSD values for intraday and interday precision were 0.050.50 and 0.070.63, respectively. The procedures were applied successfully for determination of CIP in commercial tablets. The results compared well with those from a reference HPLC method. The proposed methods can be recommended for routine analysis of CIP in QC laboratories.


2013 ◽  
Vol 2013 ◽  
pp. 1-8 ◽  
Author(s):  
Serife Evrim Kepekci Tekkeli ◽  
Armağan Önal ◽  
Fatemeh Bahadori

This study presents three simple, rapid, and accurate spectrophotometric methods for the determination of Rasagiline (RSG) in pharmaceutical preparations. The determination procedures depend on the reaction of RSG with chloranilic acid for method A, tetrachloro-1,4-benzoquinone for method B, and 7,7,8,8-tetracyanoquinodimethane for method C. The colored products were quantitated spectrophotometrically at 524, 535, and 843 nm for methods A, B, and C, respectively. Different variables affecting the reaction were optimized. Linearity ranges of the methods with good correlation coefficients (0.9988–0.9996) were observed as 25–300 µg mL−1, 25–350 µg mL−1, and 50–500 µg mL−1for methods A, B, and C, respectively. The formation of products takes place through different mechanisms. The sites of interaction were confirmed by elemental analysis using IR and1H-NMR spectroscopy. The validation of the methods was carried out in terms of specificity, linearity, accuracy, precision, robustness, limit of detection, and limit of quantitation. No interference was observed from concomitants usually present in dosage forms. The methods were applied successfully to the determination of RSG in pharmaceutical preparations.


2019 ◽  
Vol 15 (7) ◽  
pp. 752-768
Author(s):  
Naser A. Naser ◽  
Kasim M. Alasedi ◽  
Zainab A. Khan

Background: A new approach describing the validation and development of an easy, new spectrophotometric and kinetic method for identification of para-aminobenzoic acid in dietary supplement has been performed. In this study, para-aminobenzoic acid was derived in a pH-controlled environment, as a new organic compound 4(4-Benzophenylazo)pyrogallol, by incorporating diazotized para-aminobenzoic acid with pyrogallol. Objective: The determination of para-aminobenzoic acid was conducted by the fixed time and initial rate techniques. These approaches were based on the reaction of the compound containing paraaminobenzoic acid, 4(4-Benzophenylazo)pyrogallol, with Ag(I) to form colored product with a maximum absorbance at 468nm. Both of these techniques were adopted for constructing the calibration curves and examined for their suitability for the quantitation of para-aminobenzoic acid in dietary supplement. Methods: The determination process was established, using initial rate and fixed time kinetic spectrophotometric methods. Results: 4(4-Benzophenylazo)pyrogallol was characterized using proton-nuclear magnetic resonance, Fourier-transform infrared, differential scanning calorimetry and thermogravimetric thermal methods, gas chromatography–mass techniques, and solvatochromic behavior in solvents with different polarities was also examined. Conclusion: For the first time, para-aminobenzoic acid was well determined by incorporating it as an organic solid compound, 4(4-Benzophenylazo)pyrogallol, through coupling pyrogallol with diazotized para-aminobenzoic acid in regulated pH medium, ranging between 5.0 to 6.0. The existence of common excipients in the dietary supplement did not produce any significant interference. F- and ttest data analysis were used for statistical comparison of the suggested techniques with that of reference method, demonstrating excellent agreement with no significant difference in the associated precision and accuracy.


2003 ◽  
Vol 86 (3) ◽  
pp. 484-489 ◽  
Author(s):  
Abdulrahman A Al-Majed ◽  
Fathalla Belal ◽  
Kamal E E Ibrahim ◽  
Nasr Y Khalil

Abstract A simple kinetic spectrophotometric method was developed for the determination of josamycin in its dosage forms. The method is based on oxidation of the drug with alkaline potassium permanganate at room temperature for a fixed time of 20 min and measuring the produced green color at 611 nm. The absorbance–concentration plot is rectilinear over the range of 2–10 μg/mL (2.4 × 106–1.2 × 10−5M) with minimum detectability of 1.0 μg/mL (1.2 × 10−6M). The determination of josamycin by fixed concentration and the rate-constant methods is also feasible with the calibration equations obtained, but the fixed-time method proved to be more applicable. The procedure was applied successfully to commercial tablets, and statistical analysis showed that the results compared favorably with those obtained by reference methods. The effect of sensitizers and surfactants on the performance of the proposed method was also studied. A proposal of the reaction pathway was presented.


Molecules ◽  
2021 ◽  
Vol 26 (7) ◽  
pp. 2039
Author(s):  
Gamal A. E. Mostafa ◽  
Ahmed Bakheit ◽  
Najla AlMasoud ◽  
Haitham AlRabiah

The reactions of ketotifen fumarate (KT) with 2,3-dichloro-5,6-dicyano-p-benzoquinone (DDQ) and 7,7,8,8-tetracyanoquinodimethane (TCNQ) as π acceptors to form charge transfer (CT) complexes were evaluated in this study. Experimental and theoretical approaches, including density function theory (DFT), were used to obtain the comprehensive, reliable, and accurate structure elucidation of the developed CT complexes. The CT complexes (KT-DDQ and KT-TCNQ) were monitored at 485 and 843 nm, respectively, and the calibration curve ranged from 10 to 100 ppm for KT-DDQ and 2.5 to 40 ppm for KT-TCNQ. The spectrophotometric methods were validated for the determination of KT, and the stability of the CT complexes was assessed by studying the corresponding spectroscopic physical parameters. The molar ratio of KT:DDQ and KT:TCNQ was estimated at 1:1 using Job’s method, which was compatible with the results obtained using the Benesi–Hildebrand equation. Using these complexes, the quantitative determination of KT in its dosage form was successful.


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