scholarly journals Spectrophotometric Investigations of the Assay of Physiologically Active Catecholamines in Pharmaceutical Formulations

2002 ◽  
Vol 85 (6) ◽  
pp. 1288-1292 ◽  
Author(s):  
Basavaraj S Nagaralli ◽  
Jaldappa Seetharamappa ◽  
Mahaveer B Melwanki ◽  
Kunabevu C Ramesh ◽  
Jathi Keshavayya

Abstract Two simple, sensitive, and accurate spectrophotometric methods are proposed for the determination of levodopa (LD), methyldopa (MD), dopamine hydrochloride (DP), and pyrocatechol (PC) in pure and pharmaceutical preparations. The methods are based on measurement of the absorbances of tris( o-phenanthroline)iron(II) (method A) and tris(bipyridyl)iron(II) (method B) obtained by the oxidation of the catecholamines by iron(III) in the presence of 1,10-phenanthroline and 2,2′-bipyridyl at 510 and 522 nm, respectively. The absorbances were found to increase linearly with increases in the concentrations of the catecholamines, results which were corroborated by the calculated correlation coefficients (0.9990–0.9996). Beer's law was valid over the concentration ranges of 0.04–0.6, 0.06–0.75, 0.06–0.65, and 0.05–0.70 μg/mL in method A and 0.02–1.0, 0.04–1.3, 0.05–1.0, and 0.06–1.1 μg/mL in method B for PC, MD, LD, and DP, respectively. The common excipients and additives did not interfere in their determinations. The proposed methods were successfully applied to the assay of LD, MD, and DP in various dosage forms. The results were validated by statistical analysis.

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.


2017 ◽  
Vol 56 (2) ◽  
Author(s):  
Jasmin Shah ◽  
M. Rasul Jan ◽  
Inayatullah . ◽  
Sultan Shah

Two simple, sensitive and accurate spectrofluorimetric and spectrophotometric methods have been developed for the determination of sparfloxacin in bulk and pharmaceutical preparations. The proposed methods were based on oxidation of sparfloxacin with Ce (IV) in acidic medium. The spectrophotometric method involved the measurement of unconsumed Ce (IV) concentration at 315 nm. The spectrofluorimetric method based on the measurement of reduced fluorescent Ce (III) at 352 nm after excitation at 250 nm. Different variables affecting the reaction such as concentration and volume of cerium (IV), type and concentration of acidic medium, heating temperature and time were carefully studied and optimized. Under the optimum conditions, linear relationship in the range of 0.02-0.2 μg mL<sup>-1</sup> and 0.02-0.1 μg mL<sup>-1</sup> were obtained using spectrophotometric and spectrofluorimetric methods, respectively. No interferences were observed from the common formulations excipients present in the dosage form of the drug. The proposed methods were successfully applied to the analysis of the investigated drug in pure and pharmaceutical formulations with good accuracy and precision. The recovery percentage ranged from 93-102 ± 1.73-2.66%. The precision of the methods were good; RSD ≤ 2.55%.


Author(s):  
Abbas Shebeeb Al-kadumi ◽  
Sahar Rihan Fadhel ◽  
Mohammed Abdullah Ahmed ◽  
Luma Amer Musa

We proposed two simple, rapid, and convenient spectrophotometric methods are described for the determination of Amoxicillin in bulk and its pharmaceutical preparations. They are based on the measurement of the flame atomic emission of potassium ion (in first method) and colorimetric determination of the green colored solution for manganite ion at 610 nm formed after reaction of Amoxicillin with potassium permanganate as oxidant agent (in the second method) in basic medium. The working conditions of the methods were investigated and optimized. Beer's law plot showed a good correlation in the concentration range of 5-45 μg/ml. The detection limits and relative standared deviations were (2.573, 2.814 μg/ml) (2.137, 2.498) for the flame emission photometric method and (1.844, 2.016 μg/ml) (1.645,1.932) for colorimetric methods for capsules and suspensions respectively. The methods were successfully applied to the determination of Amoxicillin in capsules and suspensions, and the obtained results were in good agreement with the label claim. No interference was observed from the commonly encountered additives and expectancies.


2007 ◽  
Vol 90 (1) ◽  
pp. 128-141 ◽  
Author(s):  
Abd El-Maaboud I Mohamed ◽  
Osama H Abdelmageed ◽  
Ibrahim H Refaat

Abstract Simple chemometrics-assisted spectrophotometric methods are described for determination of 2 antibacterial binary mixtures. The mixtures are composed of norfloxacin in combination with tinidazole and erythromycin (as ethylsuccinate ester or stearate salt) in combination with trimethoprim. The normal UV absorption spectra of each pair of drugs in the studied mixtures, in the range of 200-400 nm, showed a considerable degree of spectral overlapping: 77.5% for the norfloxacintinidazole mixture and 84.3% for the erythromycintrimethoprim mixture. Resolution of the norfloxacintinidazole mixture and trimethoprim in the presence of erythromycin was accomplished successfully by using zero-crossing first derivative (1D), classical least-squares (CLS) regression analysis, and principal component regression (PCR) analysis methods. In addition, an alternative simple and accurate colorimetric method was developed for the determination of erythromycin in the presence of trimethoprim using 2,4-dinitrophenylhydrazine. All variables affecting the development of the colored chromogen were studied and optimized, and the product was measured at 526-529 and 538-542 nm for erythromycin stearate and erythromycin ethylsuccinate, respectively. For zero-crossing, first derivative technique Beer’s law was obeyed in the general concentration range of 250 μg/mL for norfloxacin, tinidazole, and trimethoprim with good correlation coefficients (0.9994-0.9996). Overall limits of detection (LOD) and quantification (LOQ) ranged from 0.59 to 2.81 and 1.96 to 9.33 μg/mL, respectively. The obtained results from CLS and PCR were compared with those obtained from a 1D spectrophotometric method. With the exception of erythromycin, overall recoveries in the average range of 97.33-103.0% were obtained with a considerable degree of accuracy when the suggested methods were applied to analysis of synthetic binary mixtures, some commercial dosage forms such as tablets and oral suspension without interference from the commonly encountered excipients and additives. For the colorimetric method, Beer's law was obeyed in the general concentration range of 7.21-28.84 μg/mL erythromycin with good correlation coefficients (0.9980-0.9996). Overall LOD and LOQ ranged from 0.73 to 1.65 and 2.43-5.49 μg/mL, respectively. Erythromycin derivatives were determined in the commercial dosage form, without interference from trimethoprim-encountered excipients and additives. The obtained results, with both chemometric and colorimetric methods, have been compared with those obtained from reported methods, and proper F- and t-values were observed, indicating no significant difference between the results of the suggested methods and reported method(s). The good percentage recoveries and proper statistical data obtained proved the efficiency of the proposed procedures for the determination of the studied drugs in their binary mixtures as well as in the commercial dosage forms with quite satisfactory precision.


2005 ◽  
Vol 88 (1) ◽  
pp. 38-45 ◽  
Author(s):  
Ibrahim A Darwish

Abstract Three simple and sensitive spectrophotometric methods were developed and validated for determination of the hydrochloride salts of fluoxetine, sertraline, and paroxetine in their pharmaceutical dosage forms. These methods were based on the reaction of the N-alkylvinylamine formed from the interaction of the free secondary amino group in the investigated drugs and acetaldehyde with each of 3 haloquinones, i.e., chloranil, bromanil, and 2,3-dichloronaphthoquinone, to give colored vinylamino-substituted quinones. The colored products obtained with chloranil, bromanil, and 2,3-dichloronaphthoquinone exhibit absorption maxima at 665, 655, and 580 nm, respectively. The factors affecting the reactions were studied and optimized. Under the optimum reaction conditions, linear relationships with good correlation coefficients (0.9986–0.9999) were found between the absorbances and the concentrations of the investigated drugs in the range of 4–120 μg/mL. The limits of detection for the assays ranged from 1.19 to 2.98 μg/mL. The precision values of the methods were satisfactory; the relative standard deviations were 0.56–1.24%. The proposed methods were successfully applied to the determination of the 3 drugs in pure and pharmaceutical dosage forms with good accuracy; the recoveries ranged from 99.1 to 101.3% with standard deviations of 1.15–1.92%. The results compared favorably with those of reported methods.


2010 ◽  
Vol 60 (2) ◽  
pp. 217-227 ◽  
Author(s):  
Padmarajaiah Nagaraja ◽  
Ashwinee Shrestha ◽  
Anantharaman Shivakumar ◽  
Avinash Gowda

Use ofN, N-diethyl-p-phenylenediamine sulphate for the spectrophotometric determination of some phenolic and amine drugsSpectrophotometric methods are proposed for the determination of drugs containing a phenol group [salbutamol sulphate (SLB), ritodrine hydrochloride (RTD), isoxsuprine hydrochloride (IXP)] and drugs containing an aromatic amine group [dapsone hydrochloride (DAP), sulfamethoxazole (SFM), and sulfadiazine (SFD)] in pharmaceutical dosage forms. The methods are based on coupling ofN, N-diethyl-p-phenylenediamine sulphate with the drugs in the presence of KIO4to give a green colored product (λmaxat 670 nm) and a red colored product (λmaxat 550 nm), respectively. Linear relationships with good correlation coefficients (0.9986-0.9996) were found between absorbance and the corresponding concentration of drugs in the range 1-7, 2-22, 1-17, 1.5-12, 2-25, and 2-21 μg mL-1for SLB, RTD, IXP, DAP, SFM and SFD, respectively. Variable parameters such as temperature, reaction time and concentration of the reactants have been analyzed and optimized. The RSD of intra-day and inter-day studies was in the range of 0.2-1.0 and 0.4-1.0%, respectively. No interference was observed from common pharmaceutical adjuvants. The reliability and performance of the proposed methods was validated statistically; the percentage recovery ranged from 99.5 ± 0.1 to 99.9 ± 0.3%. Limits of detection were 0.14, 0.21, 0.51, 0.44, 0.33 and 0.37 μg mL-1for SLB, RTD, IXP, DAP, SFM, and SFD, respectively.


2005 ◽  
Vol 2 (3) ◽  
pp. 199-202 ◽  
Author(s):  
L. D. Srinivas ◽  
P. Ravi Kumar ◽  
B. S. Sastry

Two simple and sensitive Visible spectrophotometric methods (A and B) for the determination of Fexofenadine (FEX) in bulk sample and pharmaceutical formulations are described. Methods A and B are based on the formation of ion-association complex involving carboxylic acid group of FEX and the basic dyes, Safranin-O (SFN-O, method A), methylene blue (MB, method B). The results obtained in the above two methods are reproducible and are statistically validated and found to be suitable for the assay of Fexofenadine in bulk and its pharmaceutical formulations.


2015 ◽  
Vol 1 (2) ◽  
pp. 11 ◽  
Author(s):  
Safwan Mohammad Fraihat

Two spectrophotometric methods were developed for the determination Tadalafil in pharmaceutical preparations. The methods are based on the oxidation reaction with known excess amount of Ce(IV) and estimation of the unreacted amount using Indigo carmine dye (Method A) and in Methylene blue dye  (Method B). the factors affecting the reaction conditions were studied and the absorbance of absorbance of the oxidation reaction products were monitored at 610 and 600 nm for methods A and B respectively. Beer's law is obeyed in the concentration ranges 11 to 50 and 10 to 55 ppm, the limits of detection and quantification are reported. The proposed method was applied to the determination of the drug in pharmaceutical formulations and the results demonstrated that the method is equally accurate, precise and reproducible as the official methods. The validity of method was established by recovery studies with satisfactory results.


2019 ◽  
Vol 27 (1) ◽  
pp. 47-64
Author(s):  
Ahmed I. Hassan

Abstract An environmentally safe, simple and robust spectrophotometric method has been developed for determination of H2-receptor antagonists namely: cimetidine (CIM), famotidine (FAM), nizatidine (NIZ), and ranitidine hydrochloride (RAN). The method was depend on the reaction of the studied drugs with N-bromosuccinimide (NBS), environmentally friendly reagent, and the excess NBS was measured by its reaction with phloroglucinol to give a yellow chromogenic product (λmax at 435 nm). The absorption intensity decrease (ΔA) was correlated with drug concentrations in the sample solutions. By using of the optimum conditions, linear calibration curves with good correlation coefficients (0.9958–0.9998) were found between the measured ΔA values and the corresponding drugs concentrations in the range of 12-80 μg mL−1. Limits of detection were in the range 1.31-2.21 μg mL−1. The proposed method was validated and successfully applied for the analysis of the above mentioned drugs in their bulk and pharmaceutical dosage forms with good recoveries (98.5 ± 0.98 to 102.5 ± 0.79%). No interferences were obtained from the common excipients. The proposed method was successfully applied for the analysis of H2RAs in their dosage forms and the results were comparable with that obtained by the official methods.


Author(s):  
Amir Alhaj Sakur ◽  
Bayan Balid

In this article, it has been reported new, simple, sensitive and direct spectrophotometric methods for the determination of Perindopril Erbumine (PPE) and Enalapril Maleate (ENL) in pure and in pharmaceutical forms. Spectrophotometric methods are based on the formation of yellow colored ion-pair complexes between PPE, ENL and sulphonphthalein acid dye, Bromocresol green (BCG) into chloroform were measured at the wavelength of 414 and 415nm for PPE and ENL, respectively. The optimal analytical conditions were determined. The obtained complexes (BCG: PPE) and (BCG: ENL) reached maximum absorbance directly after formation at room temperature for a stability period of 24 h. Beer’s law were obeyed in the concentration ranges of (2-20)µg/mL for PPE and (8- 44)µg/mL for ENL, the limit of detection of 0.125μg/mL and 0.230μg/mL were found for PPE and ENL, respectively. The molar absorptivity coefficients were 4.4045*104 L.moL-1.cm-1 for PPE and 1,9330*104 L.moL-1.cm-1 for ENL. The stoichiometry of the complexes formed between PPE, ENL and BCG were 1:1. No interference was observed from common excipients occurred in pharmaceutical formulations and the proposed methods have been successfully applied to determine the PPE and ENL in some pharmaceutical products and in ENL combination dosage forms with hydrochlorothiazide (HCTZ). The proposed methods were successfully validated to be utilized in the quantitative analysis of PPE and ENL in their pure and pharmaceutical products. A good agreement between the developed spectrophotometric methods with the results obtained from official reference methods for the determination of the two drugs in some real samples demonstrate that the proposed methods were suitable to quantify PPE and ENL in pharmaceutical formulations.


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