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

Affiliations
1 Medicinal Chemistry Department, Zagazig University, EG

Abstract

Two simple, sensitive and extractive spectrophotometric methods have been developed for the determination of gatifloxacin, levofloxacin HCl and lomefloxacin HCl in pure form and in pharmaceutical formulations. The methods are based on the formation of yellow and blue coloured ion-pair extractable complexes between the three drugs and two dyes, bromophenol red and fast green FCF with absorption maxima at 426-430 nm and 631 nm for both dyes, respectively. The stoichiometry of the complex in either cases was found to be 1:1. Beer's law was obeyed in the range of 10-55 μg/ml for gatifloxacin and 10-70 μg/ml for levofloxacin HCl and lomefloxacin HCl in case of bromophenol red method and in the range of 0.2-1.8 μg/ml for the three drugs in case of fast green FCF method. Various analytical parameters have been evaluated and the results were validated according to ICH guidelines. The proposed methods have been applied successfully to the analysis of drugs in pure form and in its dosage forms and no interference was observed from common excipients present in pharmaceutical formulations.

Keywords

Gatifloxacin, Levofloxacin HCl, Lomefloxacin HCl, Ion-Pair Complexes, Bromophenol Red, Fast Green FCF.

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

Affiliations
1 Medicinal Chemistry Department, Zagazig University, EG

Abstract

Three simple and sensitive spectrophotometric methods are described for determination of levofloxacin HCl, lomefloxacin HCl and sparfloxacin in bulk and pharmaceutical dosage forms using bromate-bromide as the oxidimetric reagent. Drugs are treated with known excess of insitu generated bromine and residual unreacted bromine is determined by treating with fixed amount of either methylene blue, methyl orange or thymol blue then measuring absorbances at 678 nm, 510 nm 545 nm, respectively. The amount of bromine reacted corresponds to the amount of each drug. Beer's law was obeyed in the range of 0.05-1.0 μg.ml^-1 for levofloxacin HCl and lomefloxacin HCl and 0.1-1.4 μg.ml^-1 for sparfloxacin in case of methylene blue, of 0.1-1.0 μg.ml^-1 for levofloxacin HCl and lomefloxacin HCl and 0.1-1.8 μg.ml^-1 for sparfloxacin in case of methyl orange and of 0.25-2.75 μg.ml^-1 for levofloxacin HCl and lomefloxacin HCl and 1.0-5.5 μg.ml^-1 for sparfloxacin in case of thymol blue. Various analytical parameters have been evaluated such as effect of acidity, bromate - bromide volume and time, on the absorption and the results were validated according to ICH guidelines. 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

Levofloxacin HCI, Lomefloxacin HCI, Sparfloxacin, Bromate-Bromide, Methylene Blue, Methyl Orange, Thymol Blue.

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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 four fluoroquinolones including levofloxacin HCl, lomefloxacin HCl, gatifloxacin and sparfloxacin in pure form or in presence of some impurities within 5 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 μμg/mL for all drugs. The retention time of levofloxacin HCl, lomefloxacin HCl, gatifloxacin and sparfloxacin was noted to be 1.11, 2, 2.98, and 4.3 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. It was successfully applied for the analysis of these drugs in marketed formulations and could be effectively used for the routine analysis of formulations containing any one of the above drugs, or a combination, without any alteration in the chromatographic conditions.

Keywords

RP-HPLC, Levofloxacin HCl, Iomefloxacin HCl, Gatifloxacin, Sparfloxacin.

Full Text

     

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 sparfloxacin, gatifloxacin, metronidazole and tinidazole in pure form or in presence of some impurities within 5 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 all drugs. The retention time of sparfloxacin, gatifloxacin, metronidazole and tinidazole was noted to be 4.3, 3, 1.8 and 1.2 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. It was successfully applied for the analysis of these drugs in marketed formulations and could be effectively used for the routine analysis of formulations containing any one of the above drugs, or a combination, without any alteration in the chromatographic conditions.

Keywords

RP-HPLC, Sparfloxacin, Gatifloxacin, Metronidazole, Tinidazole.

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