Asian Journal of Pharmaceutical Analysis

Sobhy M. El-Adl ¹, Abdallah A. El-Shanawany ¹, Lobna M. Abdel-Aziz ¹, Ali F. Hassan ²

Affiliations
1 Department of Medicinal Chemistry, Zagazige University, Zagazig, EG
2 Department of Pharmaceutical Chemistry, Al-Azhar University, Assuit, EG

Abstract

An isocratic HPLC method had been developed for rapid simultaneous separation and determination of three ceohalosporins including Cefepime, Cefotriaxone and Cefotaxime in pure form or in presence of some impurities within 8 minutes. Separation was carried out on a Hypersil gold C18 (10um, 100x4.6mm) column. Effect of pH and composition of mobile phase was studied. Beer's law was obeyed in the range of 1-70 μg/ml for all drugs. The method was applied for the determination of drugs in both bulk and pharmaceutical forms and was validated when obtained results were compared with reference methods.

Keywords

Cefepime, Cefotriaxone, Cefotaxime, Hypersil Gold, Mobile Phase.

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Abdallah A. El-Shanawany ¹, Sobhy M. El-Adl ¹, Lobna M. Abdel-Aziz ¹, Ali F. Hassan ²

Affiliations
1 Department of Medicinal Chemistry, Zagazige University, Zagazig, EG
2 Department of Pharmaceutical Chemistry, Al –Azhar University, Assuit, EG

Abstract

Two spectrophotometric methods are described for determination of Cefepime, Cefoperasone andCefotriaxone in bulk and pharmaceutical dosage forms using insitu generated bromine as oxidizing agent and either methylene blue or methyl orange as chromogenic agents. Drugs are treated with known excess of bromine and residual unreacted bromine is determined by treating with fixed amount of either methylene blue or methyl orange then measuring absorbances at 678 nm and 510 nm, respectively. The amount of bromine reacted corresponds to the amount of each drug. Effect of acidity, bromate - bromide volume and reactiontime, on the absorption was studied. Calibration curves were linear over ranges of 1-3 μg.ml^-1 for Cefepime,0.4- 1.0 μg.ml^-1 for Cefoperazone and 0.3-0.8 μg.ml^-1 for Cefotriaxone in case of methylene blue and of 0.05-3.0 μg.ml^-1 for Cefepime, 0.75-2.0 μg.ml^-1 for Cefoperazone and 0.2-1.4 μg.ml^-1 for Cefotriaxone in case of methyl orange. The methods were satisfactory applied for the determination of drugs in both bulk and pharmaceutical forms and results were compared statistically with reference methods.

Keywords

Cefepime, Cefoperazone, Cefotriaxone, Methylene Blue and Methyl Orange.

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Abdallah A. El-Shanawany ¹, Sobhy M. El-Adl ¹, Lobna M. Abdel-Aziz ¹, Ali F. Hassan ²

Affiliations
1 Department of Medicinal Chemistry, Zagazige University, Zagazig, EG
2 Department of Pharmaceutical Chemistry, Al –Azhar University, Assuit, EG

Abstract

New simple, accurate and sensitive spectrophotometric method for determination of Cephradine and Captopril in bulk and dosage forms using O-phthaldhyde as a reagent. This method depends on the reaction of the two mentioned drugs with O-phthaldhyde in presence of borate buffer at pH 9.5 to form faint yellow color of isoindole derivative measured at 334 nm. Effect of pH, reagent concentration, temperature, buffer, time and addition sequence on the absorption was studied. Beer's law was obeyed in the range of 0.1-0.7 μg/ml for cefradine and 2-2.5 μg/ml for Captopril. The proposed methods were applied for determination of Cefradine and Captopril in pharmaceutical preparations and were validated when obtained results were compared with reference methods.

Keywords

Cephradine, Captopril, O-Phthaldhyde and Borate Buffer.

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Mahmoud M. Sebaiy ¹, Abdullah A. El-Shanawany ¹, Sobhy M. El-Adl ¹, Lobna M. Abdel-Aziz ¹, Hisham A. Hashem ²

Affiliations
1 Medicinal Chemistry Department, Zagazig University, EG
2 Analytical Chemistry Department, Zagazig University, EG

Abstract

An isocratic RP-HPLC method had been developed for rapid simultaneous separation and determination of norfloxacin and tinidazole in tablet dosage form and also in presence of some impurities within 2 minutes. Separation was carried out on a Chromolith® Performance RP-18e (100 x 4.6 mm) using a mobile phase of MeOH : 0.025M KH₂PO₄ adjusted to pH 3 using ortho - phosphoric acid (20:80, v/v) at ambient temperature. The flow rate was 4 ml/min and maximum absorption was measured at 290 nm. The standard curve was linear in the concentration range of 1-80 μg/mL for both drugs. The retention time of tinidazole and norfloxacin was noted to be 1.2, and 1.6 minutes respectively, indicating shorter analysis time. The method was validated according to ICH guidelines. The proposed method was found to be accurate, reproducible, and consistent which is useful for the routine determination of norfloxacin and tinidazole bulk drug and in its pharmaceutical dosage form.

Keywords

RP-HPLC, Rapid, Simultaneous, Norfloxacin, Tinidazole.

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