Simple methods for HPTLC peak purity assessment and identification of the HPTLC peaks were presen... more Simple methods for HPTLC peak purity assessment and identification of the HPTLC peaks were presented. The spectrodensitograms -selected at different time intervals across the elution time of the HPTLC peak -were extracted and digital algorithms for manipulating the data were carried out in the wavelength domain. Three different methods were developed for testing the HPTLC peak purity using the mathematically transformed data of the spectrodensitograms. These included the method of relative absorption, the method of log A versus the wavelength plots and the derivative (first, second, third and fourth) method. The identification of the HPTLC peaks was based on the use of the derivative profile of the spectrodensitogram and the derivative ratios as fingerprints for the compounds. The wavelengths of absorbance and derivative (first, second, third and fourth) optima of the extracted spectrodensitograms were allocated. The data were compared with those obtained using the corresponding reference standard. The validity of the proposed methods was performed by chromatography of a mixture containing mebendazole and methylparaben as a model versus the winCATS ® spectral correlation method as a reference method. The study indicated that the proposed concept is a reliable non-confusing valuable tool for testing the purity and identity of the HPTLC peaks as the results are easily and rigorously interpreted.
Journal Association of Official Analytical Chemists, 1989
First (D1) and second (D2) derivative spectrophotometric methods are presented for the determinat... more First (D1) and second (D2) derivative spectrophotometric methods are presented for the determination of clotrimazole after its acid hydrolysis. Mixtures of clotrimazole with azidamfenicol and dexamethasone have been assayed using D2 measurement at 302 nm after acid hydrolysis for clotrimazole, D1 measurement at 288 nm for azidamfenicol, and D1 measurement at 436 nm after reaction with phenylhydrazinium sulfate for dexamethasone. Reproducible results with relative standard deviations of less than 2% are obtained. The proposed method has been successfully applied to the analysis of creams, topical solutions, and vaginal tablets.
Http Dx Doi Org 10 1080 00032719808002874, Aug 19, 2006
Abstract Fourier descriptor (FD) values computed from spectrophotometric measurements were used t... more Abstract Fourier descriptor (FD) values computed from spectrophotometric measurements were used to compute a purity index. The Fourier Descriptors calculated for a set of absorbencies are independent of concentration and is sensitive to the presence of ...
A simple and sensitive calorimetric method for the determination of some penicillins and cephalos... more A simple and sensitive calorimetric method for the determination of some penicillins and cephalosporins is presented. The method is based on reaction with 2-nitrophenylhydrazine hydrochloride in presence of dicyclohexylcarbodi-imide and pyridine. The violet colour of the resulting acid hydrazide is measured at the appropriate wavelength. The method has been applied to determination of these antibiotics in bulk and dosage forms, with a coefficient of variation less than 2%.
Simple methods for HPTLC peak purity assessment and identification of the HPTLC peaks were presen... more Simple methods for HPTLC peak purity assessment and identification of the HPTLC peaks were presented. The spectrodensitograms -selected at different time intervals across the elution time of the HPTLC peak -were extracted and digital algorithms for manipulating the data were carried out in the wavelength domain. Three different methods were developed for testing the HPTLC peak purity using the mathematically transformed data of the spectrodensitograms. These included the method of relative absorption, the method of log A versus the wavelength plots and the derivative (first, second, third and fourth) method. The identification of the HPTLC peaks was based on the use of the derivative profile of the spectrodensitogram and the derivative ratios as fingerprints for the compounds. The wavelengths of absorbance and derivative (first, second, third and fourth) optima of the extracted spectrodensitograms were allocated. The data were compared with those obtained using the corresponding reference standard. The validity of the proposed methods was performed by chromatography of a mixture containing mebendazole and methylparaben as a model versus the winCATS ® spectral correlation method as a reference method. The study indicated that the proposed concept is a reliable non-confusing valuable tool for testing the purity and identity of the HPTLC peaks as the results are easily and rigorously interpreted.
Journal of Pharmaceutical and Biomedical Analysis, 1993
Two spectrophotometric methods are described for the determination of guanethidine sulphate (I), ... more Two spectrophotometric methods are described for the determination of guanethidine sulphate (I), guanfacine hydrochloride (II), guanoclor sulphate (III), guanoxan sulphate (IV) and debrisoquine sulphate (V). The first method involves ion-pair formation of the selected compounds (I-V) with bromocresol purple at pH 3.8. The yellow ion pair is extracted with chloroform and the absorbance is measured at about 415 nm. The second method is based on the reaction of the basic guanidino compounds (I, III-V) with iodine in chloroform to give molecular charge-transfer complexes with maximum absorbance at 292 and 345 nm. Beer's law was obeyed for both methods and the relative standard deviations were found to be less than 2%. The apparent molar absorptivities were found to be 2.1 x 10(4) to 6.9 x 10(4) l mol-1 cm-1 using bromocresol purple and 0.7 x 10(4) to 2.4 x 10(4) l mol-1 cm-1 using iodine. The investigated drugs were assayed in tablets. The mean percentage recoveries were found to be 99.8-100.8% by the acid-dye method and around 100.4% by the charge-transfer complexation method.
Journal of Pharmaceutical and Biomedical Analysis, 2003
Two sensitive and fast spectrophotometric methods using batch and flow-injection procedures for t... more Two sensitive and fast spectrophotometric methods using batch and flow-injection procedures for the determination of cimetidine (CMT) are proposed. The methods are based on the formation of a green complex between this drug and Cu(II) in acetic/acetate medium of pH 5.9. The calibration graphs resulting from measuring the absorbance at 330 nm are linear over the ranges 2.5 )10 (6 Á/1.0 )10 (3 and 5)10 (6 Á/2.0 )10 (3 M with detection limits of 9.5 )10 (7 and 2.1 )10 (6 for batch and flow-injection methods, respectively. The methods are applied to the routine analysis of CMT in pharmaceuticals and human urine. #
Journal of Clinical Pharmacy and Therapeutics, 1985
A simple and rapid colorimetric method for the determination of imipramine hydrochloride and desi... more A simple and rapid colorimetric method for the determination of imipramine hydrochloride and desipramine hydrochloride in their tablet formulations and in biological fluids is presented. The method is based on the reaction of these drugs with 3-methyl-2-benzothiazolone hydrazone in the presence of ferric chloride, with direct measurement at 635 nm. Cyclohexane was used to extract these drugs from serum and urine, at basic pH, by a single manual extraction. The method can detect 0.5 microgram/ml of each drug. The main advantages of this method are its simplicity and high sensitivity.
Granisetron is a selective 5-HT3 receptor antagonist used in prevention and treatment of chemothe... more Granisetron is a selective 5-HT3 receptor antagonist used in prevention and treatment of chemotherapy-induced nausea and vomiting. The drug is available in tablet dosage form and parenteral dosage form containing benzyl alcohol as a preservative. The main route of degradation of granisetron is through hydrolysis. The present work describes the development of a simple, rapid, and reliable first derivative spectrophotometric method for the determination of granisetron in presence of its hydrolytic products as well as the formulations adjuvant and benzyl alcohol. The method is based on the measurement of the first derivative response of granisetron at 290 nm where the interference of the hydrolytic products, the co-formulated adjuvant and benzyl alcohol is completely eliminated. The proposed method was validated with respect to specificity, linearity, selectivity, accuracy, precision, robustness, detection, and quantification limits. Regression analysis showed good correlation between the first derivative response and the concentration of granisetron over a range of 8-16 μg ml(-1) . Statistical analysis proved the accuracy of the proposed method compared with a reference stability indicating high performance liquid chromatography method. The described method was successfully applied to the determination of granisetron in different batches of tablets and ampoules. The assay results obtained in this study strongly encourage us to apply the validated method for the quality control and routine analysis of tablets and parenteral preparations containing granisetron.
Abstract Three simple, rapid and sensitive colorimetric methods for the assay of mebeverine hydro... more Abstract Three simple, rapid and sensitive colorimetric methods for the assay of mebeverine hydrochloride are described. The first method is based on the reaction of mebeverine with iodine to give a yellow molecular charge transfer complex in chloroform with a maximum ...
... Sci. Ed., &?, 26,1984. 26-M. AW el - H amid , MA K orany , and Mona Bedair, Acta Pharm. J... more ... Sci. Ed., &?, 26,1984. 26-M. AW el - H amid , MA K orany , and Mona Bedair, Acta Pharm. J ugosl . , 34,183,1984. 27-MA K orany , Mona B edair , H. Mahgoub, and MA E lsayed , J. Assoc. Off. Anal. Chem., %,608,1986. 28-C larke , EGC, "Isolation and Identification of Drugs", ...
Two simple, sensitive and economical spectrophotometric methods have been developed for the deter... more Two simple, sensitive and economical spectrophotometric methods have been developed for the determination of amiodarone hydrochloride in pure form and commercial dosage form. These methods (A and B) are based on the reaction of amiodarone base as n-electron donor with p-chloranilic acid and 2,3-dichloro-5,6-dicyano-1,4-benzoquinone (DDQ) as pi-acceptors to give highly colored complex species which absorb maximally at 535 and 570 nm, respectively. Beer's law is obeyed in the concentration ranges 10.0 - 360.0 and 2.0 - 65.0 microg ml(-1) for methods A and B, respectively. Application of the proposed methods to commercial pharmaceutical tablets are presented.
... derivative spectropnotometry, limit test. Magda 8. Barary, Fawzy A. El-Yazbi and Mona A. Beda... more ... derivative spectropnotometry, limit test. Magda 8. Barary, Fawzy A. El-Yazbi and Mona A. Bedair Department of Pharmaceutical Analytical Chemistry, ... aldehyde, if present in alcohol, was calculated using the c a1 i bra t i on curve s . Limit of Aldehydes in Alcohols : ...
Simple methods for HPTLC peak purity assessment and identification of the HPTLC peaks were presen... more Simple methods for HPTLC peak purity assessment and identification of the HPTLC peaks were presented. The spectrodensitograms -selected at different time intervals across the elution time of the HPTLC peak -were extracted and digital algorithms for manipulating the data were carried out in the wavelength domain. Three different methods were developed for testing the HPTLC peak purity using the mathematically transformed data of the spectrodensitograms. These included the method of relative absorption, the method of log A versus the wavelength plots and the derivative (first, second, third and fourth) method. The identification of the HPTLC peaks was based on the use of the derivative profile of the spectrodensitogram and the derivative ratios as fingerprints for the compounds. The wavelengths of absorbance and derivative (first, second, third and fourth) optima of the extracted spectrodensitograms were allocated. The data were compared with those obtained using the corresponding reference standard. The validity of the proposed methods was performed by chromatography of a mixture containing mebendazole and methylparaben as a model versus the winCATS ® spectral correlation method as a reference method. The study indicated that the proposed concept is a reliable non-confusing valuable tool for testing the purity and identity of the HPTLC peaks as the results are easily and rigorously interpreted.
Journal Association of Official Analytical Chemists, 1989
First (D1) and second (D2) derivative spectrophotometric methods are presented for the determinat... more First (D1) and second (D2) derivative spectrophotometric methods are presented for the determination of clotrimazole after its acid hydrolysis. Mixtures of clotrimazole with azidamfenicol and dexamethasone have been assayed using D2 measurement at 302 nm after acid hydrolysis for clotrimazole, D1 measurement at 288 nm for azidamfenicol, and D1 measurement at 436 nm after reaction with phenylhydrazinium sulfate for dexamethasone. Reproducible results with relative standard deviations of less than 2% are obtained. The proposed method has been successfully applied to the analysis of creams, topical solutions, and vaginal tablets.
Http Dx Doi Org 10 1080 00032719808002874, Aug 19, 2006
Abstract Fourier descriptor (FD) values computed from spectrophotometric measurements were used t... more Abstract Fourier descriptor (FD) values computed from spectrophotometric measurements were used to compute a purity index. The Fourier Descriptors calculated for a set of absorbencies are independent of concentration and is sensitive to the presence of ...
A simple and sensitive calorimetric method for the determination of some penicillins and cephalos... more A simple and sensitive calorimetric method for the determination of some penicillins and cephalosporins is presented. The method is based on reaction with 2-nitrophenylhydrazine hydrochloride in presence of dicyclohexylcarbodi-imide and pyridine. The violet colour of the resulting acid hydrazide is measured at the appropriate wavelength. The method has been applied to determination of these antibiotics in bulk and dosage forms, with a coefficient of variation less than 2%.
Simple methods for HPTLC peak purity assessment and identification of the HPTLC peaks were presen... more Simple methods for HPTLC peak purity assessment and identification of the HPTLC peaks were presented. The spectrodensitograms -selected at different time intervals across the elution time of the HPTLC peak -were extracted and digital algorithms for manipulating the data were carried out in the wavelength domain. Three different methods were developed for testing the HPTLC peak purity using the mathematically transformed data of the spectrodensitograms. These included the method of relative absorption, the method of log A versus the wavelength plots and the derivative (first, second, third and fourth) method. The identification of the HPTLC peaks was based on the use of the derivative profile of the spectrodensitogram and the derivative ratios as fingerprints for the compounds. The wavelengths of absorbance and derivative (first, second, third and fourth) optima of the extracted spectrodensitograms were allocated. The data were compared with those obtained using the corresponding reference standard. The validity of the proposed methods was performed by chromatography of a mixture containing mebendazole and methylparaben as a model versus the winCATS ® spectral correlation method as a reference method. The study indicated that the proposed concept is a reliable non-confusing valuable tool for testing the purity and identity of the HPTLC peaks as the results are easily and rigorously interpreted.
Journal of Pharmaceutical and Biomedical Analysis, 1993
Two spectrophotometric methods are described for the determination of guanethidine sulphate (I), ... more Two spectrophotometric methods are described for the determination of guanethidine sulphate (I), guanfacine hydrochloride (II), guanoclor sulphate (III), guanoxan sulphate (IV) and debrisoquine sulphate (V). The first method involves ion-pair formation of the selected compounds (I-V) with bromocresol purple at pH 3.8. The yellow ion pair is extracted with chloroform and the absorbance is measured at about 415 nm. The second method is based on the reaction of the basic guanidino compounds (I, III-V) with iodine in chloroform to give molecular charge-transfer complexes with maximum absorbance at 292 and 345 nm. Beer's law was obeyed for both methods and the relative standard deviations were found to be less than 2%. The apparent molar absorptivities were found to be 2.1 x 10(4) to 6.9 x 10(4) l mol-1 cm-1 using bromocresol purple and 0.7 x 10(4) to 2.4 x 10(4) l mol-1 cm-1 using iodine. The investigated drugs were assayed in tablets. The mean percentage recoveries were found to be 99.8-100.8% by the acid-dye method and around 100.4% by the charge-transfer complexation method.
Journal of Pharmaceutical and Biomedical Analysis, 2003
Two sensitive and fast spectrophotometric methods using batch and flow-injection procedures for t... more Two sensitive and fast spectrophotometric methods using batch and flow-injection procedures for the determination of cimetidine (CMT) are proposed. The methods are based on the formation of a green complex between this drug and Cu(II) in acetic/acetate medium of pH 5.9. The calibration graphs resulting from measuring the absorbance at 330 nm are linear over the ranges 2.5 )10 (6 Á/1.0 )10 (3 and 5)10 (6 Á/2.0 )10 (3 M with detection limits of 9.5 )10 (7 and 2.1 )10 (6 for batch and flow-injection methods, respectively. The methods are applied to the routine analysis of CMT in pharmaceuticals and human urine. #
Journal of Clinical Pharmacy and Therapeutics, 1985
A simple and rapid colorimetric method for the determination of imipramine hydrochloride and desi... more A simple and rapid colorimetric method for the determination of imipramine hydrochloride and desipramine hydrochloride in their tablet formulations and in biological fluids is presented. The method is based on the reaction of these drugs with 3-methyl-2-benzothiazolone hydrazone in the presence of ferric chloride, with direct measurement at 635 nm. Cyclohexane was used to extract these drugs from serum and urine, at basic pH, by a single manual extraction. The method can detect 0.5 microgram/ml of each drug. The main advantages of this method are its simplicity and high sensitivity.
Granisetron is a selective 5-HT3 receptor antagonist used in prevention and treatment of chemothe... more Granisetron is a selective 5-HT3 receptor antagonist used in prevention and treatment of chemotherapy-induced nausea and vomiting. The drug is available in tablet dosage form and parenteral dosage form containing benzyl alcohol as a preservative. The main route of degradation of granisetron is through hydrolysis. The present work describes the development of a simple, rapid, and reliable first derivative spectrophotometric method for the determination of granisetron in presence of its hydrolytic products as well as the formulations adjuvant and benzyl alcohol. The method is based on the measurement of the first derivative response of granisetron at 290 nm where the interference of the hydrolytic products, the co-formulated adjuvant and benzyl alcohol is completely eliminated. The proposed method was validated with respect to specificity, linearity, selectivity, accuracy, precision, robustness, detection, and quantification limits. Regression analysis showed good correlation between the first derivative response and the concentration of granisetron over a range of 8-16 μg ml(-1) . Statistical analysis proved the accuracy of the proposed method compared with a reference stability indicating high performance liquid chromatography method. The described method was successfully applied to the determination of granisetron in different batches of tablets and ampoules. The assay results obtained in this study strongly encourage us to apply the validated method for the quality control and routine analysis of tablets and parenteral preparations containing granisetron.
Abstract Three simple, rapid and sensitive colorimetric methods for the assay of mebeverine hydro... more Abstract Three simple, rapid and sensitive colorimetric methods for the assay of mebeverine hydrochloride are described. The first method is based on the reaction of mebeverine with iodine to give a yellow molecular charge transfer complex in chloroform with a maximum ...
... Sci. Ed., &?, 26,1984. 26-M. AW el - H amid , MA K orany , and Mona Bedair, Acta Pharm. J... more ... Sci. Ed., &?, 26,1984. 26-M. AW el - H amid , MA K orany , and Mona Bedair, Acta Pharm. J ugosl . , 34,183,1984. 27-MA K orany , Mona B edair , H. Mahgoub, and MA E lsayed , J. Assoc. Off. Anal. Chem., %,608,1986. 28-C larke , EGC, "Isolation and Identification of Drugs", ...
Two simple, sensitive and economical spectrophotometric methods have been developed for the deter... more Two simple, sensitive and economical spectrophotometric methods have been developed for the determination of amiodarone hydrochloride in pure form and commercial dosage form. These methods (A and B) are based on the reaction of amiodarone base as n-electron donor with p-chloranilic acid and 2,3-dichloro-5,6-dicyano-1,4-benzoquinone (DDQ) as pi-acceptors to give highly colored complex species which absorb maximally at 535 and 570 nm, respectively. Beer's law is obeyed in the concentration ranges 10.0 - 360.0 and 2.0 - 65.0 microg ml(-1) for methods A and B, respectively. Application of the proposed methods to commercial pharmaceutical tablets are presented.
... derivative spectropnotometry, limit test. Magda 8. Barary, Fawzy A. El-Yazbi and Mona A. Beda... more ... derivative spectropnotometry, limit test. Magda 8. Barary, Fawzy A. El-Yazbi and Mona A. Bedair Department of Pharmaceutical Analytical Chemistry, ... aldehyde, if present in alcohol, was calculated using the c a1 i bra t i on curve s . Limit of Aldehydes in Alcohols : ...
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