Chromatographic determination of clotrimazole, ketoconazole and fluconazole in pharmaceutical formulations

Abdel-Moety, Ezzat M.; Khattab, Fatma I.; Kelani, Khadiga M.; AbouAl-Alamein, A.M

doi:10.1016/s0014-827x(02)01270-3

Cited by 79 publications

(35 citation statements)

References 13 publications

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“…2). 42) Complete degradation of CL, MN and EN was achieved by refluxing with hydrochloric acid for 5 h. On the other hand, the degradation products of KT were isolated using preparative TLC plates after refluxing for at least 5 h with hydrochloric acid.…”

Section: Resultsmentioning

confidence: 99%

“…They include volumetric, 3) spectrophotometric, [4][5][6][7][8][9][10][11][12][13][14][15][16][17][18] spectrofluorimetric methods, [19][20][21] capillary electrophoresis method, 22,23) thin layer chromatography, 24,25) gas chromatography 26,27) and high performance liquid chromatographic methods. [28][29][30][31][32][33][34][35][36][37][38][39][40] However, the imidazole antifungal derivatives are susceptible for the degradation due to the effect of temperature, oxygen, light and pH and the degraded products may be pharmacologically inactive.…”

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confidence: 99%

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Stability Indicating Methods for the Determination of some Anti-fungal Agents Using Densitometric and RP-HPLC Methods

Mousa

El-Kousy

El‐Bagary

et al. 2008

CHEMICAL & PHARMACEUTICAL BULLETIN

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There are more than 100000 different species of fungi, many of which are beneficial to food and fermentation industries; however, hundreds are pathogenic to plants and a few hundreds have been shown to cause infection in humans. 1)Treatment of fungal infections is considerably more difficult than that of a bacterial infection as many fungal infections occur in poorly vascularised or avascular tissues. 2)Ketoconazole (KT), clotrimazole (CL), miconazole nitrate (MN) and econazole nitrate (EN) (Fig. 1) are imidazole derivatives which represent a large and emerging group of synthetic antifungal agents.Several methods for the determination of ketoconazole, clotrimazole, miconazole nitrate and econazole nitrate, have been described in the literature. They include volumetric, 3) spectrophotometric, [4][5][6][7][8][9][10][11][12][13][14][15][16][17][18] spectrofluorimetric methods, [19][20][21] capillary electrophoresis method, 22,23) thin layer chromatography, 24,25) gas chromatography 26,27) and high performance liquid chromatographic methods. [28][29][30][31][32][33][34][35][36][37][38][39][40] However, the imidazole antifungal derivatives are susceptible for the degradation due to the effect of temperature, oxygen, light and pH and the degraded products may be pharmacologically inactive. In addition, there are many antifungal pharmaceutical preparations containing some corticosteroid hormones and the pharmacopeial methods don't report any method for the determination of these drugs either in presence of their degradation products or in presence of corticosteroid hormones.In this study simple, rapid precise and selective densitometric and HPLC method for the determination of some antifungal drugs KT, CL, MN, and EN in pure form or in the presence of their degradation products were developed. The methods were successfully applied to determine these drugs in pharmaceutical dosage forms and in presence of some corticosteroid hormones. ExperimentalMaterials and Reagents Ketoconazole (KT) Sedico Pharmaceutical Co., 6 October City-Egypt. The purity of the sample was found to be 99.82Ϯ1.157 applying a non-aqueous titration pharmacopoeial method. 3)Clotrimazole (CL) Pharcopharmaceuticals, Alexandria-Egypt. The purity of the sample was found to be 99.87Ϯ1.856 applying a non-aqueous titration pharmacopoeial method. 3)Miconazole nitrate (MN) Minapharm-Egypt. The purity of the sample was found to be 99.776Ϯ1.695 applying a non-aqueous titration pharmacopoeial method. Control and Research; Cairo, Egypt. Received February 26, 2007; accepted September 30, 2007; The HPLC method determined mixtures of CL or EN with their degradation products which were separated and quantified on a Zorbax C8 column. Elution was carried out using methanol : phosphate buffer pH 2.5 (65 : 35 v/v) as a mobile phase at a flow rate of 1.5 ml/min and UV detection at 220 nm for CL. For EN, a mixture of methanol : water containing 0.06 ml triethylamine pH 10 (75 : 25 v/v) was used as a mobile phase at a flow rate of 1.5 ml/min and UV detection at 225 nm. ...

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Section: Resultsmentioning

confidence: 99%

mentioning

confidence: 99%

Stability Indicating Methods for the Determination of some Anti-fungal Agents Using Densitometric and RP-HPLC Methods

Mousa

El-Kousy

El‐Bagary

et al. 2008

CHEMICAL & PHARMACEUTICAL BULLETIN

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“…The present study is an attempt to develop LC/MS/MS method for the determination of both the genotoxic impurity and its precursor. The literature survey revealed that some spectrophotometric and HPLC methods were developed for the determination of fluconazole in formulations as well as bio samples [21][22][23][24][25][26][27][28], but no method has been found for the determination of genotoxic impurities at low levels (µg/g).…”

Section: Introductionmentioning

confidence: 99%

Method Development and Validation Study for Quantitative Determination of Genotoxic Impurity and Its Precursor in Fluconazole Sample by Liquid Chromatography–tandem Mass Spectrometry

Devanna

Reddy

2016

Int J Pharm Pharm Sci

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Objective: The objective of this work is method development and validation study for quantitative determination of 1-[2-(2,4-difluorophenyl)-2,3-epoxypropyl]-1H-1,2,4-triazole, a genotoxic impurity and its precursor in a fluconazole drug sample by liquid chromatography-tandem mass spectrometry.Methods: LC-MS/MS analysis of these impurities was performed on Hypersil BDS C18 (100 mm x 4.0 mm, 3 µm) column. 5 mmol ammonium acetate and acetonitrile in the ratio of 65:35 (v/v) was used as the mobile phase with a flow rate of 0.4 ml/min. The developed method was accomplished with a short run time of 10 min. Triple quadrupole mass detector coupled with positive electrospray ionization was used for the quantification of genotoxic impurities in multiple reaction monitoring (MRM). Results:The method was validated as per International Conference on Harmonization (ICH) guidelines. The method was linear in the range of 0.30 µg/g to 11.37 µg/g for impurity A and 0.30 µg/g to 11.34 µg/g for impurity B with a correlation coefficient of 0.999. The accuracy of the method was in the range of 98.25 % to 100.53 % for both impurities. Conclusion:A specific, selective, highly sensitive and more accurate analytical method using LC-MS/MS coupled with positive electrospray ionization has been developed for the quantification of genotoxic impurity (1-[2-(2,4-difluorophenyl)-2,3-epoxypropyl]-1H-1,2,4-triazole) and its precursor (1-(2,4-difluorophenyl)-2-[1,2,4]triazol-1-yl-ethanone) at 0.3 µg/g with respect to the 5.0 mg/ml of fluconazole.

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“…Different methods have been reported for its determination such as spectrophotometry [2][3][4][5], chromatography [6][7][8] and electrochemistry [9,10]. The oxidation of ketoconazole with cerium (Ce (IV)) has not been reported in literature before, therefore, a comprehensive investigation on the reaction conditions was found to be necessary.…”

Section: Introductionmentioning

confidence: 99%

Spectrophotometric Methods for the Determination of Ketoconazole in Pharmaceutical Dosage Forms

Fraihat¹,

Bahgat²

2014

Trop. J. Pharm Res

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Purpose: To develop simple, sensitive and economical methods for the determination of (KZ) in both pure samples and pharmaceutical formulations. Methods: The first method (A) was based on the oxidation of the studied drug by a known excess of cerium (IV) as an oxidizing agent and subsequent determination of unreacted oxidant by reacting it with indigo carmine (IN) dye. The second method (B) involved potassium permanganate as oxidant and methylene blue (MB) as dye. Spectrophotometry was used to determine the residual amount of the dyes by measuring the absorbance of the two dyes at 610 and 660 nm, respectively. Comparison was made with the British Pharmacopoeia 1998 method.

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Chromatographic determination of clotrimazole, ketoconazole and fluconazole in pharmaceutical formulations

Cited by 79 publications

References 13 publications

Stability Indicating Methods for the Determination of some Anti-fungal Agents Using Densitometric and RP-HPLC Methods

Stability Indicating Methods for the Determination of some Anti-fungal Agents Using Densitometric and RP-HPLC Methods

Method Development and Validation Study for Quantitative Determination of Genotoxic Impurity and Its Precursor in Fluconazole Sample by Liquid Chromatography–tandem Mass Spectrometry

Spectrophotometric Methods for the Determination of Ketoconazole in Pharmaceutical Dosage Forms

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