Abstract

Determination and Quantification of an N-nitroso-Betaxolol in the Betaxolol Hydrochloride Active Pharmaceutical Ingredient by LC-MS/MS

A Liquid Chromatography-Tandem Mass Spectrometry (LC-MS/MS) method was developed for the quantification of N-nitroso-betaxolol in the betaxolol hydrochloride active pharmaceutical ingredient. Chromatographic separation was achieved using a waters acquity BEH C18 column, with 0.1% formic acid in water and Methanol as mobile phase in gradient elution mode at a 0.25 ml/ min flow rate. Quantification of impurities was carried out using triple quadrupole mass detection with electrospray ionization in the multiple reaction monitoring modes. The method was validated with good linearity over the concentration range of 0.0042 ppm-0.0210 ppm of the betaxolol hydrochloride test concentration for Nnitroso- betaxolol. The correlation coefficient obtained in each case was>0.9990. The recoveries were found to be satisfactory over the range between 80.0 and 120.0 % for N-nitroso-betaxolol. The developed method was able to quantitate N-nitroso-betaxolol at a concentration level of 0.014 ppm with respect to 30 mg mL^-1 betaxolol hydrochloride.

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