Research Journal of Pharmaceutical Dosage Form and Technology

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

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

Abstract

Simple and sensitive spectophotometric method for determination of sumatriptan (Sum.) and zolmitriptan (Zol.) in pure form and in dosage form has been developed. The charge transfer (CT) reactions between sumatriptan and zolmitriptan as n-electron donor and 2,3-dichloro-5,6-dicyano-1,4- benzoquinone (DDQ), 7,7,8,8-tetracyanoquinodimethane (TCNQ) and tetracyanoethylene (TCNE) as π acceptors have been spectrophotometrically studied. The absorbance is measured at λ_max= 459, 843 and 415 for DDQ, TCNQ and TCNE, respectively. The optimum experimental conditions for these CT reactions have been studied carefully. Beers law is obeyed in the range of 10-80 μg/ml, 10-50 μg/ml and 10-40 μg/ml for DDQ, TCNQ and TCNE respectively with zolmitriptan drug and in range of 10-100 μg/ml,10- 100 μg/ml and 10-70 μg/ml for DDQ, TCNQ and TCNE respectively with sumatriptan drug. Sandell's sensitivity is calculated. Relative standard deviations were obtained for five replicates of the cited drugs with the mentioned reagents. The results obtained by the three reagents with the two drugs are comparable with those obtained by reported methods in raw materials and in dosage forms. The proposed methods are applied successfully for the determination of the drugs in pure form and in commercial dosage forms.

Keywords

Sumatriptan, Zolmitriptan, 7,7,8,8- Tetracyanoquinodimethane (TCNQ), Tetracyanoethylene(TCNE), 2,3- Dichloro-5,6-Dicyano-1,4-Benzoquinone(DDQ).

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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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Abd El-Aziz B. Abd El-Aleem ¹, Mamdouh R. Rezk ¹, Shaban M. Khalile ², 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

Two simple, sensitive and precise methods were developed and validated for determination of diazinon, chlorpyrifos and temefos pesticides in bulk powder and dosage forms. The spectrophotometric method involves the oxidation of these pesticides with potassium iodate in acidic medium with the liberation of iodine and subsequent extraction with cyclohexane followed by measuring the absorbance at λ=520 nm. Beer`s law is obeyed in the concentration range of 0.05-1.00 mg ml^-1 for diazinon and chlorpyrifos and 0.05-0.6 mg ml^-1 for temefos. The apparent molar absorbitivities of the resulting coloured products are found to be 0.539x10³, 0.368x10³ and 0.474x10³ L mol^-1 cm^-1 for diazinon, chlorpyrifos and temefos, respectively, whereas Sandell sensitivities are 0.5647, 0.9527 and 0.9841 μg cm^-2, respectively. The potentiometric method involves the direct titration of the studied pesticides with N-bromosuccinimide in acidic medium and the end point is determined potentiometricallyusing platinum indicator electrode. The ratio of drug: NBS was 1:3 for diazinon andchlorpyrifos and 1:6 for temefos. The proposed methods were successfully applied to the analysis of the studied pesticides in bulk powder and in dosage forms without interference from other additives.

Keywords

Diazinon, Chlorpyrifos, Temefos, Spectrophotometry, Potentiometry.

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