European Journal of Biomedical and Pharmaceutical Sciences

LC-MS/MS METHOD FOR THE DETERMINATION AND QUANTIFICATION OF A N-NITROSO-DORZOLAMIDE IN THE DORZOLAMIDE HYDROCHLORIDE ACTIVE PHARMACEUTICAL INGREDIENT

Vinayak T. Vele*, Kishor More, Mohan A., Chandavarkar, Shivaji Kadam, Sushil Singh and Amol Kumbhar

ABSTRACT

Background: Aim of the present study to developed and validate an UPLC-MS/MS method for the quantification of N-nitroso-Dorzolamide in Dorzolamide Hydrochloride drug substance. Results: This technique involves chromatographic separation with a Phenyl Hexyl column with 0.05 % ammonia solution in water as mobile phase A and equal acetonitrile as mobile phase B in gradient elution mode at a 0.40 ml/ min flow rate. Quantification of Nitrosamine impurity was carried out using triple quadrupole mass detection with electrospray ionization in the multiple reaction monitoring mode. The validation experiments involve the demonstration of system suitability, specificity, limit of detection, quantitation, linearity, precision and accuracy experiments. The results obtained were found to be within the acceptable limit. Conclusions: The proposed method is simple quality control tool for the identification and quantification of N-nitroso-Dorzolamide at low level in Dorzolamide Hydrochloride drug substance.

Keywords: Nitrosamine, N-nitroso-Dorzolamide, LCMS/MS, Method Validation, Dorzolamide Hydrochloride.