An approach for the microscale synthesis and screening of combinatorial lib
raries of chiral stationary phases (CSPs) is described. This technique offe
rs a number of advantages over previously described methods for the prepara
tion and evaluation of new CSPs: The stationary phases are made on 50 mg st
ale or less and need not be packed into columns to be evaluated; a solid ph
ase synthesis approach can be utilized to create diverse libraries of candi
date CSPs; evaluation of the CSPs directly reveals the best CSP for a parti
cular separation, consequently the screening results can be directly transl
ated to chromatographic performance.