Chiral separation of β‐blockers by supercritical fluid chromatography using Chiralpak‐IG and Chiralpak IBN‐5 columns

Abstract

Chiral separation of β‐blockers is performed by utilizing the supercritical fluid chromatographic method. The chiral columns utilized were Chiralpak IG and Chiralpak IBN‐5. The finest mobile phase was CO2 −0.2% TEA in methanol (60:40). The values atenolol enantiomers retention factors were 6.39 and 8.98. These values for propranolol enantiomers were 3.39 and 4.06. These values for betaxolol enantiomers were 4.08 and 4.68. The separation and resolution factor values for atenolol, propranolol, and betaxolol were 1.41 and 3.33, 1.19 and 2.23, and 1.15 and 1.87, separately and respectively. By comparison, it was observed that Chiralpak IG column is better than Chiralpak IBN‐5 column. Supercritical fluid chromatography has been found as the best analytical technique due to its high speed, being eco‐friendly, and being economic. The various most probable interactions responsible for the chiral resolution are hydrogen bonding, dipole–dipole interactions, steric effect, and π–π interactions. The reported methods are effective, efficient, and reproducible and may be used to separate and identify atenolol, propranolol, and betaxolol in any unknown samples.

Recent Advances in Separation and Analysis of Chiral Compounds

“…Hayes et al built a microscale SFC-based purification platform via the alteration of fluid channel and introduction of gas–liquid separators for the discovery and analysis of pharmaceuticals on ChiralPak Column (Westchester). More drug racemates of β2-agonist of terbutaline, β-blockers, antidepressant drug of paroxetine hydrochloride, and borneol lipid (candidate drug for cerebrovascular disease) were also efficiently resolved by SFC. − The coupling of different chiral columns can provide great opportunity to increase the separation efficiency of SFC . A two-dimensional chiral SFC based on two different CSPs of amylose tri-(3,5-dimethylphenylcarbamate) and cellulose tris (4-methyl-benzoate) was applied to chiral separation of aliphatic acid derivatives …”