Author(s): Santosh Kumar Bhardwaj, K. Dwivedi, D. D. Agarwal
The paper reports a recent efforts to develop and validate an efficient and rapid analytical assay method by LC/ LCMS for a series of 2H-benzoxazinone based 3-aryl-3,4-dihydro-2H-benz[e]-1,3-oxazines. Such compounds posse’s potent pharmacological importance, and are of the class of efavirenz, a non-nucleoside reverse transcriptase inhibitor (NNRTI). Series of seven compounds were separated using ODS , 250×4.6mm, 5 µm column with a mobile phase -A consist of 90:10 (v/v) of 0.05M ammonium acetate buffer with pH 5.60 + 05, (pH adjusted with acetic acid) and acetonitrile. mobile phase -B consisting 90:10 .05M ammonium acetate buffer with pH 5.60 + 05, pH adjusted with ortho phosphoric acid with a timed gradient program. Detection was carried out at 245 nm and the flow rate 1.0 ml/min. The method has been validated in terms of suitability, specificity, linearity, intra and interday Precision, limits of detection and quantification The method found to be accurate in the concentration range of 1.0–10.0 µg mL-1 for all compounds. LOD and LOQ were from 0.024 to 0.048 µg mL-1 and 0.075 to 0.147 µg mL-1. Method is linear over concentration range 0.1 to 100 µg mL-1. The proposed method was found to be accurate, precise, specific, linear, rugged, robust, and stability indicating for the determination of a series of 3- aryl-3,4-dihydro-2H-benz[e]-1,3-oxazines and has shown to be convenient for routine analysis of 3-aryl-3,4-dihydro-2H-benz[e]-1,3- oxazine derivatives.