scholarly journals Kinetic Spectrophotometric Determination of Ethamsylate in Dosage Forms

2007 ◽  
Vol 90 (3) ◽  
pp. 679-685 ◽  
Author(s):  
Nahed El-Enany ◽  
Fathalla Belal ◽  
Mohamed Rizk

Abstract A simple and sensitive kinetic method has been developed for the determination of ethamsylate (ESL) in its pharmaceutical preparations. The method is based upon oxidation of ESL with 3-methyl-2-benzothiazolinone hydrazone hydrochloride in presence of cerium(IV) ammonium sulfate at room temperature for 20 min. The absorbance of the reaction product is measured at 514 nm. The absorbance-concentration plot was rectilinear over the range of 430 g/mL (r = 0.9999). The lower detection limit was 0.267 g/mL (9.110 106 M) and the lower quantitation limit was 0.808 g/mL. The different experimental parameters affecting the development and stability of the reaction product were studied and optimized. The proposed method was applied to the determination of ESL in formulations, and the results obtained were in good agreement with those obtained using a reference method. The proposed method was also used for the in vitro detection of ESL in spiked human plasma at its therapeutic concentration level.

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.


2009 ◽  
Vol 74 (8-9) ◽  
pp. 977-984
Author(s):  
Sofija Rancic ◽  
Snezana Nikolic-Mandic

A new reaction was suggested and a new kinetic method was elaborated for determination of Bi(III) in solution, based on its catalytic effect on the oxidation of phenyl-fluorone (PF) by hydrogen peroxide in ammonia buffer. By application of spectrophotometric technique, a limit of quantification (LQ) of 128 ng cm-3 was reached, and the limit of detection (LD) of 37 ng cm-3 was obtained, where LQ was defined as the ratio signal: noise = 10:1 and LD was defined as signal 3:1 against the blank. The RSD value was found to be in the range 2.8-4.8 % for the investigated concentration range of Bi(III). The influence of some ions upon the reaction rate was tested. The method was confirmed by determining Bi(III) in a stomach ulcer drug ('Bicit HP', Hemofarm A.D.). The obtained results were compared to those obtained by AAS and good agreement of results was obtained.


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.


2002 ◽  
Vol 85 (6) ◽  
pp. 1316-1323 ◽  
Author(s):  
Mohamed I Walash ◽  
Fathalla Belal ◽  
Fawzia Ibrahim ◽  
Mohamed Hefnawy ◽  
Manal Eid

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.


2016 ◽  
Vol 29 (4) ◽  
pp. 184-189 ◽  
Author(s):  
Mohauman Mohammad Al-Rufaie

Abstract A simple, rapid, sensitive, inexpensive and easy to perform kinetic spectrophotometric procedure for the investigation of trace quantities of the drug, furosemide (FRO), as bulk and in the pharmaceutical preparations, has been improved upon. The enhanced method was depended on the fashioning of the Schiff ‘s base by the reaction of the aldehyde group present in the 5-sulfo salicylaldehyde reagent, and the primary amino group present in furosemide. The latter acts as a ligand for the formation of an intense colored complex with Co(II) in an acidic medium, with maximum absorption at 608 nm. In the work, kinetic spectrophotometrics were established through the fixed time method. Moreover, Beer’s law was applied on the range of concentration between 5-100 ppm, while the molar absorptivity and the Sandell sensitivity were 3.9295×104 l.mol−1cm−1, 0.008 μg.cm−2, respectively. The detection limit (LOD) was 2.133 µg/ml−1, and LOQ was 1.105 µg/ml−1. Ideal circumstances for all colour improvement were seen, and the suggested procedure has been effectively employed in investigating amounts of furosemide (FRO) in bulk forms and in pharmaceutical preparations (tablets, injection sample). Additives and general excipient materials did not affect the studied method. A statistical comparison between the results that were obtained from the reference method gave good agreement.


2018 ◽  
Vol 39 (4) ◽  
pp. 49
Author(s):  
Halil İbrahim Ulusoy ◽  
Ramazan Gürkan

A novel sensitive and relatively selective kinetic method is presented for the determination of V(V), based on its catalytic effect on the oxidation reaction of Ponceau Xylydine by potassium bromate in presence of 5-sulfosalicylic acid (SSA) as activator. The reaction was monitored spectrophotometrically by measuring the decrease in absorbance of Ponceau Xylydine at 640 nm between 0.5 to 7 min (the fixed time method) in H3PO4 medium at 25oC. The effect of various parameters such as concentrations of H3PO4, SSA, bromate and Ponceau Xylydine, temperature and ionic strength on the rate of net reaction were studied. The method is free from most interferences, especially from large amounts of V(IV). The decrease in absorbance is proportional to the concentration of V(V) over the entire concentration range tested (1–15 ng mL−1) with a detection limit of 0.46 ng mL–1 (according to statistical 3Sblank/k criterion) and a coefficient of variation (CV) of 1.8% (for ten replicate measurement at 95% confidence level).The proposed method suffers few interferences such as Cr(VI) and Hg(II) ions. The method was successfully applied to the determination of V(V) in tap water, drinking water, bottled mineralwater samples and a certified standard reference material such as SRM-1640 with satisfactory results. The vanadium contents of water samples were also determined by FAAS for a comparison.The recovery of spiked vanadium(V) was found to be quantitative and the reproducibility was satisfactory. It was observed that the results of the SRM 1640 were in good agreement with the certified value.


2008 ◽  
Vol 91 (2) ◽  
pp. 349-359 ◽  
Author(s):  
Mohamed I Walash ◽  
Fathalla Belal ◽  
Nahed El-Enany ◽  
Amina Abdelal

Abstract A rapid, simple, and highly sensitive second-derivative synchronous fluorometric method has been developed for the simultaneous analysis of binary mixtures of cinnarizine (CN) and nicergoline (NIC). The method is based upon measurement of the native fluorescence of these drugs at constant wavelength difference () = 80 nm in aqueous methanol (50, v/v). The different experimental parameters affecting the native fluorescence of the studied drugs were carefully studied and optimized. The fluorescence-concentration plots were rectilinear over the range of 0.0251.5 and 0.255.5 g/mL for CN and NIC, respectively, with lower detection limits of 0.58 and 0.82 ng/mL and quantitation limits of 1.93 and 2.73 ng/mL for CN and NIC, respectively. The proposed method was successfully applied for the determination of the studied compounds in synthetic mixtures and in commercial tablets. The results obtained were in good agreement with those obtained with reference methods. The high sensitivity attained by the proposed method allowed the determination of CN in real and spiked human plasma. The mean recovery in the case of spiked human plasma [number of trials (n) = 3] was 102.82 2.17, while that in real human plasma (n = 3) was 105.25 2.05.


2000 ◽  
Vol 68 (3) ◽  
pp. 281-296 ◽  
Author(s):  
Ekram M. Hassan ◽  
Mohammed E.M. Hagga ◽  
Haya I. Al Johar

An accurate kinetic method for the determination of cisapride is described. The method is based on the reaction of cisapride with potassium dichromate in 2.5 M sulphuric acid at room temperature for a fixed-time of 10 min, afterwards the absorbance of the reaction product is measured at 527 nm. The concentration of cisapride is computed using the corresponding calibration equation for the fixed-time method. The method is applied successfully to commercial tablets and oral suspension dosage forms. The results obtained are compared statistically with the British Pharmacopoeia method. The determination of cisapride by other kinetic methods is feasible with calibration equation obtained but the fixed-time method proves to be more applicable.


2014 ◽  
Vol 68 (4) ◽  
pp. 429-434
Author(s):  
Sofija Rancic ◽  
Snezana Nikolic-Mandic ◽  
Aleksandar Bojic

A new, simple, rapid, sensitive and selective spectrophotometric kinetic method for Ag(I) traces determination at room temperature was elaborated in this paper. It is based on catalytic effect of silver ions upon the oxidation of methylene blue B (MBB) by K2S2O8 (PPS) in citric buffer (BUF) solution. The method was confirmed by determination of Ag(I) in PbO. The obtained results were compared to those obtained by ICP-OES method and good agreement of results was found.


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