Chiral separation of aliphatic primary amino alcohols as o‐phthaldialdehyde/mercaptoethanol derivatives on polysaccharide‐based chiral stationary phases

Abstract

A sensitive chiral high performance liquid chromatography (HPLC) method for the determination of aliphatic primary amino alcohol isomers with ophthaldialdehyde/mercaptoethanol precolumn derivatization has been developed and validated. Seven chiral columns were tested in a reversed phase mode. Excellent enantioseparation with the resolution more than 2.0 was achieved on Chiralcel OJ-3R. The effect of various chromatographic conditions including column temperature, acetonitrile content in the mobile phase, buffer pH, buffer concentration, and buffer type in the mobile phase on the retention and the selectivity was investigated. The final mobile phase consisted of binary mixture of 20mM ammonium formate solution with acetonitrile (75:25; v/v).The analyses were performed at mobile phase flow rate of 1.0 mL/min and the column temperature of 40°C. The fluorescence detection was performed at excitation wavelength of 345 nm and emission wavelength of 450 nm. The developed method was fully validated in terms of linearity, sensitivity, accuracy, precision, intermediate precision, and selectivity according to International Council for Harmonisation of Technical Requirements for Pharmaceuticals for Human Use guidelines using internal normalization procedure. The proposed chiral method was proved to be highly sensitive, simple, and rapid and was successfully applied to the determination of D-Valinol content in commercially available samples of L-Valinol.

Simultaneous analysis of 44 frequently abused corticosteroid drugs using polysaccharide‐based chiral column‐HRMS approach

“…To support drug metabolism and pharmacokinetic studies of chiral drugs, it is necessary to mix the physical phenomenon of HPLC with the sensitivity of mass spectrometric techniques. Recently, methods using LC‐MS/MS are found to be promising techniques for solving the matter of corticosteroid analysis 19–25 …”

“…Recently, methods using LC‐MS/MS are found to be promising techniques for solving the matter of corticosteroid analysis. 19 , 20 , 21 , 22 , 23 , 24 , 25 …”

“…Recently, methods using LC-MS/MS are found to be promising techniques for solving the matter of corticosteroid analysis. [19][20][21][22][23][24][25] Polysaccharide columns offer a large range of chiral separations of racemic components. [26][27][28][29][30]…”

Influence of phenyl group number on enantioseparation performance of chitosan‐based materials

“…Till now, chiral stationary phases (CSPs) based on polysaccharide derivatives still attract much more attention because this kind of materials exerts high performance for enantioseparation. [1][2][3][4][5][6][7] Initially, polysaccharides used to prepare CSPs were cellulose and amylose, [8][9][10][11] and some chiral columns for high-performance liquid chromatography (HPLC) have been marketed.…”