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

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.

Author(s):  
Mouhammed Khateeb ◽  
Basheer Elias ◽  
Fatema Al Rahal

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


2010 ◽  
Vol 7 (4) ◽  
pp. 1612-1620 ◽  
Author(s):  
M. Keyvanfard ◽  
N. Abedi

A new, simple, sensitive and selective kinetic spectrophotometric method was developed for the determination of ultra trace amounts of vanadium(V). The method is based on the catalytic effect of vanadium(V) on the oxidation of malachite green oxalate (MG) by bromate in acidic and micellar medium. The reaction was monitored spectrophotometrically by measuring the decrease in the absorbance of malachite green oxalate (MG) at 625 nm with a fixed-time method. The decrease in the absorbance of MG is proportional to the concentration of vanadium(V) in the range of 1-100 ng/mL with a fixed time of 0.5-2 min from the initiation of the reaction. The limit of detection is 0.71 ng/mL of vanadium(V). The relative standard deviation for the determination of 5, 30, 50 ng/mL of vanadium(V) was2.5% 2.6%, 2.4% and respectively. The method was applied to the determination of vanadium(V) in water samples.


2012 ◽  
Vol 204-208 ◽  
pp. 4067-4070 ◽  
Author(s):  
Zhi Rong Zhou ◽  
Li Zhen Zhang

A simple kinetic spectrophotometric method was developed for the determination of trace amounts of Ru (III). The method is based on the reduction of spadns by sodium hypophosphite (NaH2PO2) in micellar media. The reaction was monitored spectrophotometrically by measuring the decrease in the absorbance of spadns at 515 nm with a fixed-time method. The decrease in the absorbance of spadns is proportional to the concentration of Ru (III) in the range 0.40–10.0 μg/L with a fixed time of 2.5–7.0 min from the initiation of the reaction. The limit of detection is 0.12 μg/L Ru (III). The relative standard deviation for the determination of 0.10 and 0.20 μg/25mL Ru (III) was 2.3 % and 2.0 %, respectively. The method was applied to the determination of Ru (III) in some ores and metallurgy products.


2011 ◽  
Vol 17 (1) ◽  
pp. 81-89 ◽  
Author(s):  
Zenita Devi ◽  
K. Basavaiah ◽  
K.B. Vinay

Three simple and sensitive spectrophotometric methods are described for the determination of domperidone (DOM) in bulk drug and in dosage forms using bromate-bromide mixture as brominating agent in acid medium and three dyes, meta-cresol purple (MCP), amaranth (AMR) and erioglaucine (EGC). The methods involve the addition of a known excess of bromate-bromide mixture to an acidified solution of DOM followed by the determination of the residual bromine by reacting with a fixed amount of either MCP dye and measuring the absorbance at 530 nm (method A) or AMR dye and measuring the absorbance at 520 nm (method B) or EGC dye and measuring the absorbance at 630 nm (method C). Beer?s law is obeyed over the concentration ranges, 0.63 - 10.0, 0.25-4.0 and 0.13-2.0 ?g mL-1 for method A, method B and method C, respectively. The apparent molar absorptivities are calculated to be 3.751 ? 104, 6.604 ? 104 and 1.987 ? 105 L mol-1cm-1 for method A, method B and method C, respectively and the corresponding sandell sensitivity values are 0.011, 0.006 and 0.002 ?g cm-2. The limit of detection and the limit of quantification are also reported for all the three methods. No interference was observed from common additives found in pharmaceutical preparations. Statistical comparisons of the results with those of the reference method showed an excellent agreement, and indicated no significant difference in accuracy and precision. The accuracy and reliability of the methods were further ascertained by performing recovery tests via standard-addition technique.


2011 ◽  
Vol 25 (6) ◽  
pp. 303-315 ◽  
Author(s):  
Akram M. El-Didamony ◽  
Eman A. H. Erfan

Three visible spectrophotometric methods (A–C) were developed for the analysis of someβ-blocker drugs, namely atenolol (ATE) and timolol (TIM) based on their reactivity with bromine, generated in situ by the action of hydrochloric acid on bromate–bromide mixture. The determination of residual bromine is based on its ability to bleach the indigo carmine dye and measuring the absorbance at 610 nm (method A). Methods B and C involve treating the unreacted bromine with a measured excess of iron (II), the remaining iron (II) is complexed with 1,10-phenanthroline (method B) or with 2,2'-bipyridyl (method C) and measuring the increase in absorbance at 510 and 522 nm, respectively. In all the methods, the amount of bromine reacted corresponding to the drug content. Regression analysis of Beer's plot showed good correlation in the concentration ranges of 0.4–16.4, 0.8–10.4 and 0.4–12.8 µg/ml using methods A–C, respectively, for ATE and 14–38, 12–32 and 14–38 µg/ml using methods A–C, respectively, for TIM. The optimum reaction conditions and other analytical parameters are evaluated. No interference was observed from the additives and the applicability of the methods was tested by analyzing the pharmaceutical preparations containing the investigated drugs. Statistical comparison of the results with those of official methods shows excellent agreement and indicates no significant difference in precision.


2011 ◽  
Vol 17 (3) ◽  
pp. 259-267 ◽  
Author(s):  
Nagaraju Rajendraprasad ◽  
Kanakapura Basavaiahf ◽  
Basavaiah Vinay

Quetiapine fumarate (QTF) is an antipsychotic drug belonging to the benzisoxazole derivatives indicated for the treatment of schizophrenia. A sensitive and selective method based on dichloromethane-extractable ion-pair of QTF with calmagite (CGT), which exhibited an absorption maximum at 490 nm, is described. At this wavelength, Beer?s law is obeyed over the concentration range of 3.0 - 30.0 ?g ml-1. The apparent molar absorptivity, limit of detection (LOD) and quantitation (LOQ) values are 1.32 ? 104 l mol-1 cm-1, 0.27 and 0.81 ?g ml-1 respectively. The reaction is extremely rapid at room temperature and the absorbance values remain unchanged upto 19 h. The precision results, expressed as intra-day and inter-day relative standard deviation values, are satisfactory (RSD ? 2.2%). The accuracy is satisfactory as well (RE ? 2.44%). The method was successfully applied to the determination of QTF in pharmaceuticals and spiked human urine with satisfactory results. No interference was observed from common pharmaceutical adjuvants in tablets. Statistical comparison of the results with official method showed an excellent agreement and indicated no significant difference in precision.


2012 ◽  
Vol 610-613 ◽  
pp. 446-451
Author(s):  
Zhi Rong Zhou ◽  
Li Zhen Zhang

Based on the oxidation of neutral red by KIO4 in 3.2×10-4 mol/L sulfuric acid solution, a simple kinetic spectrophotometric method was developed for the determination of trace amounts of Se(IV).The reaction was monitored spectrophotometrically by measuring the decrease in the absorbance of neutral red at 530 nm with a fixed-time method. The decrease in the absorbance of neutral red is proportional to the concentration of Se(IV) in the range 0.0–8.0 µg/L with a fixed time of 4–6 min from the initiation of the reaction. The limit of detection is 0.36 µg/L Se(IV). The influence of the factors such as acidity, concentration of reactants, reaction time, temperature and co-existing ions on the reaction is discussed. The optimum conditions of reaction are established and some kinetic parameters are determined. The apparent activation energy of catalytic reaction is 81.60 kJ/mol. The relative standard deviation for the determination of 0.1 and 0.2 µg/mL Se(IV) was 2.1 and 1.9 %, respectively. The method has been successfully applied to the determination of Se (IV) in tea and human hair samples with the relative standard deviation of 0.33 %–1.5 % and the recovery of 97.5 %–103.5 %.


2012 ◽  
Vol 538-541 ◽  
pp. 2358-2363 ◽  
Author(s):  
Zhi Rong Zhou ◽  
Li Zhen Zhang

Based on the oxidation of acid chrome blue K (ACBK) by hydrogen peroxide in 0.002 mol/L sulfuric acid solution, while 1,10-phenanthroline (phen) acts as an activator, a simple kinetic spectrophotometric method was developed for the determination of trace amounts of Se(IV).The reaction was monitored spectrophotometrically by measuring the decrease in the absorbance of ACBK at 524 nm with a fixed-time method. The decrease in the absorbance of ACBK is proportional to the concentration of Se (IV) in the range 0.06–1.0 µg/L with a fixed time of 4–10 min from the initiation of the reaction. The limit of detection is 0.018 µg/L Se (IV). The influence of the factors such as acidity, concentration of reactants, reaction time, temperature and co-existing ions on the reaction is discussed. The optimum conditions of reaction are established and some kinetic parameters are determined. The apparent activation energy of catalytic reaction is 62.30 kJ/mol. The relative standard deviation for 11 replicate determination of 0.01 and 0.02 µg/25mL selenium (III) was calculated to be 2.3 % and 2.0 %, respectively. Combined with sulphydryl dextrane gel (SDG) separation and enriching, the method has been successfully applied to the determination of Se (IV) in foodstuff samples with the relative standard deviation of 1.1 %–3.7 % and the recovery of 99.0 %–104.0 %, the results are in good agreement with those provided by HG-AAS method.


2013 ◽  
Vol 2013 ◽  
pp. 1-5 ◽  
Author(s):  
Masoud Reza Shishehbore ◽  
Ali Sheibani ◽  
Masoumeh Eslami

A simple, selective, and inexpensive kinetic method was developed for the determination of hydrazine based on its inhibitory effect on the thionine-bromate system in sulfuric acid media. The reaction was monitored spectrophotometrically at 601 nm by a fixed time method. The effect of different parameters such as concentration of reactants, ionic strength, temperature, and time on the rate of reaction was investigated, and the optimum conditions were obtained. Under optimum conditions, the calibration curve was linear in the concentration range from 0.8–23.0 μg mL−1of hydrazine, and the detection limit of the method was 0.22 μg mL−1. The relative standard deviation for five replicate determinations of 1.0 μg mL−1of hydrazine was 0.74%. The potential of interfering effect of foreign species on the hydrazine determination was studied. The proposed method was successfully applied for the determination of hydrazine in different water samples.


Author(s):  
Mouhammed Khateeb ◽  
Bashir Elias ◽  
Shahama Adi

A new, simple and sensitive kinetic spectrophotometric method has been proposed for the determination of captopril (CPT) in pharmaceutical formulations. The method is based on oxidation of 3-methyl-2-benzothiazolinone hydrazone hydrochloride monohydrate (MBTH) by ferric chloride followed by its coupling with the drug to form green-yellow colored product with absorbance maximum at 395nm. The concentration of CPT was calculated using the calibration equation for the rate data and fixed time methods. The linearity range was found to be 0.5–22.5 μg mL-1for each method. The correlation coefficients were 0.9994 and 0.9971 for rate data and fixed time methods respectively. The proposed methods were applied successfully for the determination of CPT in pharmaceutical formulations. Statistical comparison of the results shows that there is no significant difference between the proposed and official methods.


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