RAPID SEPARATION AND DETERMINATION OF RIZATRIPTAN N-OXIDE IMPURITY IN RIZATRIPTAN BENZOATE IN A BULK DRUG SUBSTANCE BY REVERSE PHASE LIQUID CHROMATOGRAPHY
Objective: The objective is described to develop and validate a simple, reliable, precise, and specific analytical method for rapid separation and determination of N-oxide impurity in rizatriptan Benzoate active pharmaceutical ingredient bulk drug substances by reverse phase liquid chromatography as per the International Conference on Harmonization (ICH) guidelines.
Methods: The methodology utilized as reverse phase liquid chromatography with gradient composition. The mobile phase proportion was compromised mobile A containing 0.25 mm potassium dihydrogen phosphate buffer pH 2.0 and methanol (95:5 v/v) and mobile B containing Acetonitrile. ODS 3V, 250 Ã— 4.6 mm, 5 Âµm. column. The flow rate is 1.0 ml/minute using an LC system detector at wavelength 280 nm, and the column oven temperature is 40Â°C. The chromatographic separation performed in reverse phase by the gradient composer over run time was 35 minute. The resolution between N-oxide and rizatriptan was recorded on the chromatogram was more than six. The developed analytical method was validated according to the ICH guidelines.
Results: Linearity was found in rizatriptan N-oxide over the concentration range of 450-11000 ng/ml, with the linear regression (Correlation coefficient R = 0.999) and proved to be robust. Limit of detection and limit of quantification of the rizatriptan N-oxide was found 150 and 450 ng/ml. The retention time of rizatriptan and rizatriptan N-oxide was recorded 22.6 and 24.7 minutes, respectively. The percentage recovery of N-oxide has been ranged from 96.0 to 102.0 in the bulk drug material sample. The proposed analytical method has been found suitable, precise, reliable, and accurate for the separation and quantitative determination.
Conclusion: A specific, simple, accurate, reliable, and rapid reproducible analytical method has been developed and validated for reverse phase high- performance liquid chromatography to determine N-Oxide impurity in rizatriptan benzoate from bulk drugs material as per ICH guideline.
Keywords: Rizatriptan benzoate, N-oxide impurity, High performance liquid chromatography, Reverse phase, ODS column and validation.
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