New Derivatization Methodology of 4-aminobenzoic Acid from its Dietary Supplements: Kinetic Spectrophotometric Methods for Determination

2019 ◽  
Vol 15 (7) ◽  
pp. 752-768
Author(s):  
Naser A. Naser ◽  
Kasim M. Alasedi ◽  
Zainab A. Khan
Keyword(s):  
Dietary Supplement ◽  
Initial Rate ◽  
Kinetic Method ◽  
Reference Method ◽  
Fixed Time ◽  
Proton Nuclear Magnetic Resonance ◽  
Aminobenzoic Acid ◽  
Spectrophotometric Methods ◽  
Significant Difference ◽  
Kinetic Spectrophotometric

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.

scholarly journals Kinetic Spectrophotometric Determination of Gemifloxacin Mesylate and Moxifloxacin Hydrochloride in Pharmaceutical Preparations Using 4-Chloro-7-nitrobenzo-2-oxa-1,3-diazole

2014 ◽  
Vol 2014 ◽  
pp. 1-12 ◽  
Author(s):  
Mohammed G. Abdel Wahed ◽  
Ragaa El Sheikh ◽  
Ayman A. Gouda ◽  
Sayed Abou Taleb
Keyword(s):  
Limit Of Detection ◽  
Kinetic Method ◽  
Pharmaceutical Preparations ◽  
Fixed Time ◽  
Spectrophotometric Methods ◽  
Relative Standard ◽  
Significant Difference ◽  
Kinetic Spectrophotometric ◽  
Comparison Of The Results

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.

scholarly journals Validated green spectrophotometric kinetic method for determination of Clindamycin Hydrochloride in capsules

BMC Chemistry ◽  
2021 ◽  
Vol 15 (1) ◽  
Author(s):  
Shaza Affas ◽  
Amir Alhaj Sakur
Keyword(s):  
Initial Rate ◽  
Limit Of Detection ◽  
Kinetic Method ◽  
Reference Method ◽  
Fixed Time ◽  
Iodide Ions ◽  
Kinetic Spectrophotometric ◽  
Optimized Conditions ◽  
Good Agreement

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.

scholarly journals Method Development and Validation for Estimation of Eperisone Hydrochloride as API and in Tablet Dosage Form by Two Spectroscopic Methods

2013 ◽  
Vol 2013 ◽  
pp. 1-8 ◽  
Author(s):  
Joytosh Banerjee ◽  
Renu Solanki ◽  
Badri Prakash Nagori
Keyword(s):  
Method Development ◽  
Initial Rate ◽  
Kinetic Method ◽  
Fixed Time ◽  
Calibration Graph ◽  
Spectrophotometric Methods ◽  
Significant Difference ◽  
Development And Validation ◽  
Tablet Dosage

Two simple and sensitive spectrophotometric methods have been developed for the determination of eperisone hydrochloride based on its ability to be detected in UV region (Normal UV) and its oxidation using potassium permanganate in alkaline medium (kinetic spectroscopic). The detection was done at 261.40 nm and 603.5 nm. The different experimental parameters affecting the method development were studied and optimized. The initial rate and fixed time method were utilized to construct calibration graph, and 5 minutes and 3 minutes, respectively, were found suitable for the determination of the concentration of drug. Linearity was found over the concentration range of 2–20 μg/mL, 15–30 μg/mL, and 15–35 μg/mL by UV, initial rate, and fixed time methods, respectively. The results were validated as per the ICH guidelines. RSD values were found to be less than 2%. The methods were applied for estimation of eperisone hydrochloride in RAPISONE (Abbott, Maharashtra). The assay results were found to be 100.4% ± 0.08, 99.93% ± 0.05, and 99.41% ± 0.04 by UV, initial rate, and fixed time method, respectively. Statistical comparison of the proposed methods showed a good agreement indicating no significant difference in accuracy and precision, thus confirming the suitability of UV and kinetic method for the estimation of eperisone hydrochloride in bulk as well as in tablet dosage forms.

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
Keyword(s):  
Reference Method ◽  
Fixed Time ◽  
Dosage Forms ◽  
Charge Transfer Complexes ◽  
Specific Rate ◽  
Spectrophotometric Methods ◽  
H Nmr ◽  
Nmr Techniques ◽  
Kinetic Spectrophotometric

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.

scholarly journals  Determination of CLINDAMYCIN HCl in Capsules by New, Validated, Simple and Green Kinetic Spectrometric Method

2021 ◽  
Author(s):  
Shaza Affas ◽  
Amir Alhaj Sakur
Keyword(s):  
Initial Rate ◽  
Limit Of Detection ◽  
Reference Method ◽  
Fixed Time ◽  
Spectrometric Method ◽  
Iodide Ions ◽  
Kinetic Spectrophotometric ◽  
Optimized Conditions ◽  
Good Agreement

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.

scholarly journals Kinetic Spectrophotometric Determination of Certain Cephalosporins in Pharmaceutical Formulations

2009 ◽  
Vol 2009 ◽  
pp. 1-12 ◽  
Author(s):  
Mahmoud A. Omar ◽  
Osama H. Abdelmageed ◽  
Tamer Z. Attia
Keyword(s):  
Initial Rate ◽  
Pharmaceutical Formulations ◽  
Fixed Time ◽  
Rate Of Change ◽  
Ceftriaxone Sodium ◽  
Accuracy And Precision ◽  
Significant Difference ◽  
Cephalosporin Antibiotics ◽  
Kinetic Spectrophotometric

A simple, reliable, and sensitive kinetic spectrophotometric method was developed for determination of eight cephalosporin antibiotics, namely, Cefotaxime sodium, Cephapirin sodium, Cephradine dihydrate, Cephalexin monohydrate, Ceftazidime pentahydrate, Cefazoline sodium, Ceftriaxone sodium, and Cefuroxime sodium. The method depends on oxidation of each of studied drugs with alkaline potassium permanganate. The reaction is followed spectrophotometrically by measuring the rate of change of absorbance at 610 nm. The initial rate and fixed time (at 3 minutes) methods are utilized for construction of calibration graphs to determine the concentration of the studied drugs. The calibration graphs are linear in the concentration ranges 5–15 g  and 5–25 g  using the initial rate and fixed time methods, respectively. The results are validated statistically and checked through recovery studies. The method has been successfully applied for the determination of the studied cephalosporins in commercial dosage forms. Statistical comparisons of the results with the reference methods show the excellent agreement and indicate no significant difference in accuracy and precision.

scholarly journals Kinetic Spectrophotometric Determination of Ciprofloxacin in a Pharmaceutical Preparation

2010 ◽  
Vol 93 (2) ◽  
pp. 510-515 ◽  
Author(s):  
Serap Saglik Aslan ◽  
Betul Demir
Keyword(s):  
Potassium Permanganate ◽  
Initial Rate ◽  
Pharmaceutical Preparation ◽  
Fixed Time ◽  
Hplc Method ◽  
Alkaline Media ◽  
Spectrophotometric Methods ◽  
Kinetic Spectrophotometric ◽  
Interday Precision

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.

scholarly journals Kinetic Spectrophotometric Method for the Estimation of Ofloxacin in Pharmaceutical Formulations

2017 ◽  
Vol 56 (4) ◽  
Author(s):  
Lalit Kishore ◽  
Ashok Kumar ◽  
Anroop Nair ◽  
Navpreet Kaur
Keyword(s):  
Spectrophotometric Method ◽  
Reference Method ◽  
Pharmaceutical Formulations ◽  
Fixed Time ◽  
Rate Of Change ◽  
Accuracy And Precision ◽  
Ich Guidelines ◽  
Significant Difference ◽  
Rate Method ◽  
Kinetic Spectrophotometric

The objective of the current study was to develop a direct, sensitive spectrophotometric method based on the oxidation of Ofloxacin using potassium permanganate in alkaline medium. The rate of change of absorbance was measured at 603 nm. The initial rate method and fixed time method (at 4 min) are utilised to construct calibration graphs for calculating the concentration of the drug. The results were validated through inter day and intraday precision assays according to the ICH guidelines and also through recovery studies. Statistical comparison of the proposed methods with that of reference method shows excellent agreement and indicates no significant difference in their accuracy and precision.

scholarly journals New Kinetic Spectrophotometric Method for Determination of Folic Acid in Pharmaceutical Formulations

2015 ◽  
Vol 50 ◽  
pp. 169-178
Author(s):  
Mouhammed Khateeb ◽  
Basheer Elias ◽  
Fatema Al Rahal
Keyword(s):  
Folic Acid ◽  
Spectrophotometric Method ◽  
Pharmaceutical Formulations ◽  
Fixed Time ◽  
Rate Data ◽  
Sulfuric Acid Medium ◽  
Significant Difference ◽  
Kinetic Spectrophotometric ◽  
Comparison Of The Results

A simple and sensitive kinetic spectrophotometric method has been developed for the determination of folic acid (FA) in bulk and pharmaceutical Formulations. The method is based on the oxidation of FA by Fe (III) in sulfuric acid medium. Fe (III) subsequently reduces to Fe (II) which is coupled with potassium ferricyanide to form Prussian blue. The reaction is followed spectrophotometrically by measuring the increase in absorbance at λmax 725 nm. The rate data and fixed time methods were adopted for constructing the calibration curves. The linearity range was found to be 1–20 μg mL-1 for each method. The correlation coefficient was 0.9978 and 0.9993, and LOD was found to be 0.91 and 0.09 μg mL-1 for rate data and fixed time methods, respectively. The proposed method has been successfully applied to the determination of FA in formulations with no interference from the excipients. Statical comparison of the results shows that there is no significant difference between the proposed and pharmacopoeial methods

scholarly journals Kinetic Spectrophotometric Method for the Determination of Ranitidine and Nizatidine in Pharmaceuticals

2002 ◽  
Vol 85 (6) ◽  
pp. 1316-1323 ◽  
Author(s):  
Mohamed I Walash ◽  
Fathalla Belal ◽  
Fawzia Ibrahim ◽  
Mohamed Hefnawy ◽  
Manal Eid
Keyword(s):  
Spectrophotometric Method ◽  
Reaction Pathway ◽  
Kinetic Method ◽  
Fixed Time ◽  
Borate Buffer ◽  
The Other ◽  
Average Recovery ◽  
Kinetic Spectrophotometric ◽  
Good Agreement

Abstract An accurate and simple kinetic method is described for the determination of ranitidine and nizatidine in pure form and in pharmaceuticals. The method is based on the reaction of the compounds with 7-chloro-4-nitrobenz-2-oxa-1,3-diazole in pH 7.4 borate buffer at 60°C for a fixed time of 25 min for both compounds. The absorbance of the reaction product is measured at 495 nm for ranitidine and nizatidine. Calibration graphs were linear over the concentration range of 2–20 μg/mL, with limits of detection of 0.13 (3.7 × 10−7M) and 0.25 μg/mL (7.5 × 10−7M) for ranitidine and nizatidine, respectively. The proposed method was applied successfully to the determination of ranitidine in tablets and ampoules with average recoveries of 100.26 ± 0.69 and 100.29 ± 0.59%, respectively, and to the determination of nizatidine in capsules with an average recovery of 104.26 ± 0.44%. The results obtained are in good agreement with those obtained by the other methods used for comparison. A proposal of the reaction pathway is also presented.

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