Application of pH‐zone‐refining countercurrent chromatography in the chiral separation of two β‐adrenergic blocking agents

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EarlyView Article

  • Published: Dec 28, 2017
  • Author: Liqiong Lv, Zhisi Bu, Wenyu Sun, Chaoyue Wang, Cong Xu, Shengqiang Tong
  • Journal: Journal of Separation Science

Abstract

Two β‐adrenergic blocking agents, 1‐[(1‐methylethyl)amino]‐3‐phenoxy‐2‐propanol (1) and 1‐[(1‐methylethyl)amino]‐3‐(3‐methylphenoxy)‐2‐propanol (2; Toliprolol), were enantioseparated by pH‐zone‐refining countercurrent chromatography. A two‐phase solvent system composed of chloroform containing 0.10 mol/L of di‐n‐hexyl l‐tartrate/0.10 mol/L of boric acid aqueous solution (1:1, v/v) was selected, in which 20 mmol/L triethylamine was added in the organic phase as a retainer and 2 mmol/L HCl was added in the aqueous phase as an eluter. Fifty milligrams of each racemate was completely enantioseparated by pH‐zone‐refining countercurrent chromatography to yield each enantiomer with a purity of more than 98%, and the recovery of each separated enantiomer reached around 76–82%.

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