Separation of ephedrine and pseudoephedrine enantiomers using a polysaccharide-based chiral column: A normal phase liquid chromatography-high-resolution mass spectrometry approach.

Chiral considerations are found to be very much relevant in various aspects of forensic toxicology and pharmacology. In forensics, it has become increasingly important to identify the chirality of doping agents to avoid legal arguments and challenges to the analytical findings. The scope of this study was to develop an liquid chromatography-mass spectrometry (LCMS) method for the enantiomeric separation of typical illicit drugs such as ephedrines (ie, 1S,2R(+)-ephedrine and 1R,2S(-)-ephedrine) and pseudoephedrine (ie, R,R(-)-pseudoephedrine and S,S(+)-pseudoephedrine) by using normal phase chiral liquid chromatography-high-resolution mass spectrometry technique. Results show that the Lux i-amylose-1 stationary phase has very broad and balancing-enantio-recognition properties towards ephedrine analogues, and this immobilized chiral stationary phase may offer a powerful tool for enantio-separation of different types of pharmaceuticals in the normal phase mode. The type of mobile phase and organic modifier used appear to have dramatic influences on separation quality. Since the developed method was able to detect and separate the enantiomers at very low levels (in pico grams), this method opens easy access for the unambiguous identification of these illicit drugs and can be used for the routine screening of the biological samples in the antidoping laboratories.