Research Journal of Pharmaceutical Dosage Form and Technology

Abd El-Aziz B. Abd El-Aleem ¹, Shaban M. Khalile ², Amr M. Badawy ¹, Omneya K. El-Naggar ²

Affiliations
1 Analytical Chemistry Department, Cairo University, Cairo, EG
2 National Organization for Drug Control And Research (NODCAR), Giza, EG

Abstract

This paper describes sensitive, accurate and precise TLC- densitometric and high performance liquid chromatographic (HPLC) methods for simultaneous determination of paracetamol and metoclopramide in pharmaceutical formulation. The TLC method employed aluminum TLC plates precoated with silica gel F254 as the stationary phase and ethylacetate/ methanol/ ammonia (85:10:5 v/v/v) as the mobile phase, where the chromatogram was scanned at 254 nm. The developed HPLC method used a Zorbax C18 column with isocratic elution. The mobile phase composed of phosphate buffer pH 4.0: methanol (75:25 v/v) at flow rate of 1.0 ml/min. Quantitation was achieved with UV detection at 273 nm. The methods were validated according to the International Conference on Harmonization (ICH) guidelines. The selectivity of the proposed methods was tested using laboratory-prepared mixtures. The developed methods were successfully applied for the determination paracetamol and metoclopramide in bulk powder and combined dosage form.

Keywords

High-Performance Liquid Chromatography, Thin Layer Chromatography, Antimigraine Drugs, Paracetamol, Metoclopramide.

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Abd El-Aziz B. Abd El-Aleem ¹, Shaban M. Khalile ², Amr M. Badawy ³, Omneya K. El-Naggar ⁴

Affiliations
1 Analytical Chemistry Department, Cairo University, Cairo, EG
2 National Organization for Drug Control and Research (NODCAR), Giza,, EG
3 Analytical Chemistry Department, Cairo University, Cairo, EG
4 National Organization for Drug Control and Research (NODCAR), Giza

Abstract

Two simple and accurate chromatographic methods were developed for the determination of zolmitriptan, and sumatriptan in raw material and in tablets. The first method uses isocratic high performance liquid chromatographic (HPLC) method. Analysis was performed on Agilent Zorbax C18 column using a mobile phase consisting of phosphate buffer pH3: acetonitrile: methanol (2:1:1, v/v/v) with a flow rate of 0.75 ml/ min and UV detection at 253 nm. The second method uses thin-layer chromatographic (TLC) separation of sumatriptan, zolmitriptan and eletriptan from their impurities followed by densitometric measurements of drug spots at 254 nm. The separation was carried out on silica gel 60 F254 using chloroform: ethylacetate: methanol: ammonia (72:10:18:2, v/v/v/v) as mobile phase. The methods were validated according to ICH guidelines and the acceptance criteria for linearity, accuracy, precision, specificity and system suitability were met in all cases. The methods were linear in the range of 10-40 μg/ml and 10-50 μg/ml for zol. and sum. respectively by HPLC method and in range of 1-20 μg/spot, 1-20 μg/spot and 1-10 μg/spot for ele., sum. and zol. respectively by TLC method. The proposed methods were successfully applied for the determination of zol., sum. and ele. in bulk and tablets forms. The results were compared statistically at 95% confidence level with reported methods. There was no significant difference between the mean percentage recoveries and precision of the methods.

Keywords

Zolmitriptan, Sumatriptan, Eletriptan, HPLC, TLC-Densitometry.

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