Determination and Control of Genotoxic Impurity in Vitamin E, Drug Substance

Authors(3) :-Rohidas Gilbile, Saleem Shaikh, Ritu Vyas

Vitamin E (alpha-tocopherol) is a lipid-soluble antioxidant. p-toluenesulfonic acid, used as reagent in the synthesis of alpha-tocopherol, has a sulphonate group, a well-known alerting function for genotoxic activity. Genotoxic impurities in pharmaceuticals at lower levels are of increasing concerns not only to pharmaceutical industries but also for the regulatory agencies due to their risks for human carcinogenesis and, thus, requiring manufacturers to pay extra attention for their analysis and control. Therefore, sensitive and sophisticated analytical methodologies are deemed necessary in order to be able to test and control genotoxic impurities in drug substances. This work describes a simple, accurate and sensitive reversed-phase liquid chromatography—UV method for determination of trace amount of p-toluenesulfonic acid in pharmaceutical materials. A gradient mobile phase consists of acetonitrile and 0.01M potassium dihydrogen orthophosphate in water adjusted pH 3.0 with 0.1% phosphoric acid. Chromatography was carried out at ambient temperature 25°C on a Waters HPLC column C18, 150 mm x 4.6 mm, 5?m. The detection was carried out using variable wavelength UV-Vis detector set at 222 nm. The compounds were eluted at a steady flow rate of 1.0 mL/min. P-toluenesulfonic acid retention time was about 6.0 min with an asymmetry factor of 1.0. A logarithmic calibration curve was obtained from 0.1 to 3 µg/mL (r > 0.9998). Within-day %RSD was 0.21 (n = 5, 0.002 mg/mL) and between-day %RSD was 0.35 Specificity/ selectivity experiments revealed the absence of interference, recovery from spiked samples was between 97.6–103.78 percent. The developed method was applied to the determination of p-toluenesulfonic acid in pharmaceutical drug substance and drug product.

Authors and Affiliations

Rohidas Gilbile
Department of Chemistry, Pacific Academy of Higher Education and Research University, Udaipur, Rajasthan, India
Saleem Shaikh
Ullmann Laboratories, Five Star Shendra ,MIDC Aurangabad, Maharashtra State, India.
Ritu Vyas
Department of Chemistry, Pacific Academy of Higher Education and Research University, Udaipur, Rajasthan, India

P-toluenesulfonic acid; alpha-tocopherol; Reverse phase chromatography; Gradient elution. Vitamin E

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Publication Details

Published in : Volume 3 | Issue 6 | September-October 2017
Date of Publication : 2017-10-31
License:  This work is licensed under a Creative Commons Attribution 4.0 International License.
Page(s) : 953-960
Manuscript Number : IJSRSET17386
Publisher : Technoscience Academy

Print ISSN : 2395-1990, Online ISSN : 2394-4099

Cite This Article :

Rohidas Gilbile, Saleem Shaikh, Ritu Vyas, " Determination and Control of Genotoxic Impurity in Vitamin E, Drug Substance , International Journal of Scientific Research in Science, Engineering and Technology(IJSRSET), Print ISSN : 2395-1990, Online ISSN : 2394-4099, Volume 3, Issue 6, pp.953-960, September-October-2017.
Journal URL : http://ijsrset.com/IJSRSET17386

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