scholarly journals Colorimetric and Titrimetric Methods for Determination of Some Cephalosporins in their Pure and Dosage Forms.

2000 ◽  
Vol 68 (3) ◽  
pp. 263-273 ◽  
Author(s):  
Hisham E. Abdellatef ◽  
Abdalla A. Shalaby ◽  
Heba M. Elsaid ◽  
Magda M. Ayad

Two colorimetric and titrimetric procedures are developed for determination of some cephalosporins, namely, cefotaxime sodium (CFT), cehroxime sodium (CFU) and ceftazidime pentahydrate (CFZ). The first method, a colorimetric method, was based on the reaction of these cited drugs with 4-chloro-7-nitrobenzofurazan (NBD-Cl), in the presence of 5x10-3 M borax, with the formation of stable colored chromogens with maximum absorbance in the range of 409 - 414 nm. All variables affecting the development of the colour have been investigated and the conditions were optimized. The method obeys Beer's law over concentration ranges of 19.09 - 95.49, 17.85 - 124.98 and 63.66 - 254.66 µg ml-1 of CFT, CFU and CFZ, respectively. Obedience to Beer's law permitted the successful application of the proposed method for the assay of cefuran, cefumax and fortum vials. The results obtained reveal good percentage recoveries, which are in good agreement with those obtained by the official methods. In the second method, the titrimetric method, the conditions for the oxidimetric titration of cephalosporins have been studied. The titration takes place because of catalytic quantities of KBr, which give rise to an intermediate that can be hydrolyzed to the sulfoxide. The operating conditions are described and a hypothesis is put forward concerning the mechanism of the reaction.

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.


Author(s):  
Amir Alhaj Sakur ◽  
Shaza Affas

Objective: To develop and validate simple, sensitive, precise and free of organic solvents method for the determination of sildenafil (SIL) and vardenafil (VAR) in bulk and pharmaceutical formulation.Methods: The method is based on the reaction of studied drugs with a mixture of potassium iodide and potassium iodate in an aqueous medium at (25±2 °C) to form yellow coloured triiodide ions (I3-) within 45 min. The reaction is followed spectrophotometrically by measuring the absorbance at 288, 351 nm and 285, 351 nm for sildenafil and vardenafil respectively.Results: The effects of analytical parameters on the reported systems were investigated. Beer's law of SIL was obeyed in the range of (0.4-12) μg ml-1and (0.6-16) μg ml-1. Molar absorptivity was found to be (67.659 ×103) lmol/cmand (37.955×103) lmol/cm at 288 nm, 351 nm respectively. Beer's law of VAR was obeyed in the range of (0.2-13) μg/mland (0.5-40) μg/ml. Moreover, molar absorptivity’s were found to be (68.719 ×103) l mol-1 cm-1and (26.691×103) l mol-1 cm-1 at 285 nm, 351 nm respectively.Conclusion: The proposed method has been applied to determine the components in dosage forms with an average recovery of 98.15% to 103.45% and the results have been found in good agreement with those results obtained by the reference methods.


2006 ◽  
Vol 89 (6) ◽  
pp. 1524-1531 ◽  
Author(s):  
Samah S Abbas ◽  
Lories I Bebawy ◽  
Laila A Fattah ◽  
Heba H Refaat

Abstract Five simple and sensitive methods were developed for the determination of leflunomide (I) in the presence of its degradates 4-trifluoromethyl aniline (II) and 3-methyl-4-carboxy isoxazole (III). Method A was based on differential derivative spectrophotometry by measuring the △1D value at 279.5 nm. Beer's law was obeyed in the concentration range of 2.0020.00 μg/mL with mean percentage accuracy of 100.07 1.32. Method B depended on first-derivative spectrophotometry and measuring the amplitude at 253.4 nm. Beer's law was obeyed in the concentration range of 2.0016.00 μg/mL with mean percentage accuracy of 98.42 1.61. Method C was based on the reaction of degradate (II) with 2,6-dichloroquinone-4-chloroimide (Gibbs reagent). The colored product was measured at 469 nm. Method D depended on the reaction of degradate (II) with para-dimethyl aminocinnamaldehyde (p-DAC). The absorbance of the colored product was measured at 533.4 nm. Method E utilized 3-methyl-2-benzothiazolinone hydrazone in the presence of cerric ammonium sulfate with degradate (II). The green colored product was measured at 605.5 nm. The linearity range was 40.00-280.00, 2.40-24.00, and 30-250 μg/mL with mean percentage accuracy of 100.75 1.21, 100.13 1.45, and 99.74 1.39 for Methods CE, respectively. All variables were studied to optimize the reaction conditions. The proposed methods have been successfully applied to the analysis of leflunomide in pharmaceutical dosage forms and the results were statistically compared with that previously reported.


1985 ◽  
Vol 68 (1) ◽  
pp. 91-95
Author(s):  
Mohamed I Walash ◽  
Abed Abou Ouf ◽  
Fatma B Salem

Abstract The chromogenic reagent p-dimethylaminocinnamaldehyde (PDAC) is introduced for the determination of the sympathomimetic amines methyldopa and noradrenaline. The method is based on measurement of the orange color developed when the alkaline solution of methyldopa and noradrenaline is allowed to react with PDAC at pH 5.0. The color developed obeys Beer's law in the concentration range 0.1-1.5 mL of 2 x 103M solution of noradrenaline and methyldopa. The results are compared with those obtained with another chromogenic reagent, pdimethylaminobenzaldehyde (PDAB). Determinations on dosage forms of the drugs, using PDAC and PDAB reagents, agreed well with results of determinations by official pharmacopoeia! methods.


1981 ◽  
Vol 64 (5) ◽  
pp. 1145-1148
Author(s):  
Ramesh T Sane ◽  
Sudhir S Kamat ◽  
Amulya D Pandit

Abstract A method is described for the determination of ethanol in the presence of methanol without pre-separation. The sample is oxidized to give acetaldehyde and formaldehyde. 2-Thiobarbituric acid reagent is added and selectively forms a pink adduct with acetaldehyde, but not with formaldehyde. The method is sensitive, obeys Beer’s law in the concentration range 18–80 μg/mL, and has an advantage over other methods because it does not detect any “apparent normal value” of alcohol in blood.


1977 ◽  
Vol 60 (3) ◽  
pp. 531-535
Author(s):  
Griddaluru Ramana Rao ◽  
Surinder N Mahajan ◽  
Geeta Kanjilal ◽  
Katta R Mohan

Abstract A new colorimetric method has been developed for estimating folic acid. The British Pharmacopoeial method has been modified to reduce folic acid to 2,4,5-triamino-6-hydroxypyrimidine (TAHP), which is treated with nin-hydrin to yield a stable purple complex. Participation of 5-amino and 6-hydroxy groups of TAHP in the color reaction with ninhydrin is suggested on the basis of experimental evidence. The color obtained has an absorbance maximum at 555 nm and obeys Beer’s law in the concentration range of 4.5 to 45 μg folic acid/ml. The method has been successfully used for assaying folic acid, its tablets, and injections.


1990 ◽  
Vol 73 (6) ◽  
pp. 896-901 ◽  
Author(s):  
F Belal, ◽  
A El-Brashy ◽  
F Ibrahim

Abstract A simple semlmlcro titrimetric assay procedure Is described for determination of 6 semisynthetic penicillins, namely: ampiclllin, amoxicillin, benzylpenlclllin, epiclllln, hetaclllin, and phenoxymethylpenlcillln In addition to penicillamine. The method Involves the use of 2-lodoxybenzoate as a standard solution, whereby a known, excess volume Is added to the penicillins in acid medium and, after the specified time, the residual reagent is iodometrically determined. The molar ratio of the reaction Is assessed and a possible pathway for the mechanism of the reaction is suggested and confirmed through thin-layer chromatography (TLC) study of the reaction products. The proposed method is then applied to determination of the studied compounds In their dosage forms. Results obtained are in good agreement with those obtained by official methods.


1975 ◽  
Vol 58 (5) ◽  
pp. 875-878 ◽  
Author(s):  
Tulsidas R Baggi ◽  
Surinder N Mahajan ◽  
Griddaluru Ramana Rao

Abstract A colorimetric method is presented for the estimation of diazepam as the pure drug and in formulations. Diazepam is hydrolyzcd with 6N HC1 to 2-methyIamino-5-chlorobenzophenone, which is extracted with chloroform to give a yellow solution whose absorbance is measured at 410 nm against a solvent blank. The color obeys Beer's law in the concentration range of 0–30 μg/ml. In 5 determinations, recovery was 99.0±1.9%. The method is applicable to pure diazepam and its formulations for oral and parenteral use. No interferences were observed from pyridoxine hydrochloride and commonly used preservatives, vehicles, and colors.


1989 ◽  
Vol 72 (6) ◽  
pp. 885-889 ◽  
Author(s):  
Abdel-Maboud I Mohamed

Abstract A new spectrophotometric method for the determination of some unsubstituted benzene sulfonamides is presented. The method is based on the interaction of these derivatives with 7,7,8,8-tetracyanoquinodimethane at pH 9.0-9.5 to produce intense blue products. The quantitation of the products was carried out at 578 nm. Beer’s law was obeyed over a wide range of concentrations for all sulfonamide compounds studied. Optimum analytical conditions were determined, and the color produced was stable for at least 90 min at 25 °C. Analytical data for determination of sulfonamide compounds in pure form are presented together with application of the proposed method for analysis of some commercially available pharmaceutical preparations. The results are in good agreement with those obtained by official procedures.


2008 ◽  
Vol 4 (1) ◽  
pp. 278-287 ◽  
Author(s):  
Mohamed A. El Hamd ◽  
Sayed M. Derayeab ◽  
Osama H. Abdelmageedc ◽  
Hassan F. Askald

A simple, accurate and selective colorimetric method was developed and validated for determination of five 1,4-dihydropyridine drugs (1,4-DHP) using Tetrabutylammonium hydroxide reagent (TBAH). The proposed method was based on addition of TBAH to the studied drugs then produced yellow colors were measured spectrophotometrically. Different variables affecting the reactions conditions carefully studied and optimized and under the optimum conditions, Beer's law was obeyed in the concentration range of 2.50-40.0 µg/mL and the limits of detection were ranged from 0.750-1.956 µg/mL. The proposed method was successfully extended to pharmaceutical preparations tablets or capsules and the results which obtained were comparable with that obtained by the reference methods.


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