التفاصيل البيبلوغرافية
| العنوان: |
A Robust HPLC Method for Easily Oxidizable Phosphine Ligand Analysis. |
| المؤلفون: |
Weisel, Lauren, Corcoran, Liam, Castro, Steve, He, Yu |
| المصدر: |
Journal of Chromatographic Science; May/Jun2024, Vol. 62 Issue 5, p471-476, 6p |
| مصطلحات موضوعية: |
HIGH performance liquid chromatography, PHOSPHINE, PHOSPHINES, CHROMATOGRAPHIC analysis |
| مستخلص: |
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] |
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