Development of an UPLC-MS/MS approach to detect and quantify N-nitroso mirabegron in mirabegron.

In the mirabegron (MIR) synthesis, the N-nitroso mirabegron (NNM) is obtained during synthetic process of MIR; water is being used in reaction under acidic condition. Nitrite source is from water, and secondary amine source is from MIR as it has secondary amine; NNM is generated as an impurity during the synthesis of MIR. The presence of NNM in MIR could potentially affect its effectiveness.

Use of Stage-Wise AQbD and an Orthogonality Approach to Develop a Short-Runtime Method for the Simultaneous Quantification of Bosentan and Impurities using UPLC Equipped with PDA and ESI-MS.

Analytical quality by design (AQbD) and method orthogonality are comprehensive tools used to develop an analytical method based on statistical and graphical evaluation. These tools provide complete knowledge of the method and help to develop precise, accurate, and specific methods. The present work elaborates the development of a selective and precise method for the quantification of bosentan and its nine impurities with a short runtime of 10 min using a statistically driven stage-wise AQbD approach with proven orthogonality.