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The present invention relates to an optical spectroscopic method for determining in absence of enantiopure standards of a target molecule whether a mixture of enantiomers of said molecule in a test composition is non-racemic. the method relies upon the combination of cold ion spectroscopy and mass spectroscopy detection. the method includes formation of diastereoisomers of the target molecule with each of the l- and d- enantiomers of a chiral reporter molecule and comparison of the photofragmentation spectra recorded for said diastereoisomers.