Home
Resources
Publications
Development and Validation of a UHPLC UV Method for the In-Process Control of Bosentan Monohydrate Synthesis

Development and Validation of a UHPLC UV Method for the In-Process Control of Bosentan Monohydrate Synthesis

Marta Jatczak, Katarzyna Sidoryk, Magdalena Kossykowska, Wojciech Łuniewski, Joanna Zagrodzka, Elżbieta Lipiec-Abramska

Chromatographia. 2016;79(17):1131-1141.

PMID: 27616782

Abstract:

Bosentan monohydrate (4-tert-butyl-N-[6-(2-hydroxyethoxy)-5-(2-methoxyphenoxy)-2-(pyrimidin-2-yl) pyrimidin-4-yl]benzene-1-sulfonamide monohydrate) is a dual endothelin receptor antagonist (ERA) applied in the treatment of pulmonary arterial hypertension. To achieve effective process control of the bosentan monohydrate synthesis, it was necessary to develop a selective and not highly time-consuming method for ultra-high performance liquid chromatography (UHPLC). The method is characterized by adequate sensitivity, reproducibility and selectivity for the determination of bosentan monohydrate and related compounds from all synthetic stages. The UHPLC separation was carried out by reversed phase chromatography on the Acquity BEH C18 column (100 mm × 2.1 mm, 1.7 µm) with a mobile phase composed of solvent A (0.1 %, v/v, acetic acid in water) and solvent B (methanol), in the gradient mode at the flow rate of 0.4 mL min-1. Limits of detection and quantification for the compounds were ≤0.1 µg mL-1 and 0.3 µg mL-1, respectively. The linearity for all related compounds was investigated as in the range for the active pharmaceutical ingredient (API) and as in the range for the in-process control. The developed method was validated according to the current guidelines, proving the suitability of the method for its intended purpose.

Chemicals Related in the Paper:

Catalog Number	Product Name	Structure	CAS Number	Price
AP150728135	Bosentan Related Compound D		150728-13-5	Price

As a specialist in analytical chemical Products, Alfa Chemistry offers consumers a wealth of raw materials and a full range of technologies and services.

QUICK LINKS

HEADQUARTERS

Tel:

Fax:

Email: