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A Robust HPLC Method for Easily Oxidizable Phosphine Ligand Analysis.
- Source :
-
Journal of Chromatographic Science . May/Jun2024, Vol. 62 Issue 5, p471-476. 6p. - Publication Year :
- 2024
-
Abstract
- Phosphine ligands are widely used in the manufacture of small molecule active pharmaceutical ingredients, for they play a key role in transition-metal-catalyzed cross-coupling. However, chromatographic analysis of phosphine ligands can be challenging because of the easily oxidizable nature of this class of compounds. This manuscript describes an out-of-specification (OOS) investigation study of XPhos raw material analysis by high performance liquid chromatography (LC). It is concluded that on-column degradation/oxidation is the culprit behind this OOS result. In addition, a slightly modified yet much improved new LC method is developed by adding a trace amount of tris(2-carboxyethyl)phosphine (TCEP) into the aqueous mobile phase. TCEP is also a phosphine compound and is commonly used as a reducing reagent in molecular biology. The trace amount of TCEP serves as a surrogate reagent to passivate the LC column and eliminate the on-column degradation/oxidation. As a result, a much more robust performance is achieved with greatly improved method precision and sensitivity. This is a general approach and can be applied to the LC analysis of many other phosphine ligands in the same manner. [ABSTRACT FROM AUTHOR]
Details
- Language :
- English
- ISSN :
- 00219665
- Volume :
- 62
- Issue :
- 5
- Database :
- Academic Search Index
- Journal :
- Journal of Chromatographic Science
- Publication Type :
- Academic Journal
- Accession number :
- 177611351
- Full Text :
- https://doi.org/10.1093/chromsci/bmad008