Chiral separation of clandestine amphetamine type stimulants and cathinone derivatives by HPLC-MS/MS.

摘要

The abuse of illicit drugs, such as amphetamine type stimulants and cathinone derivatives, has been a major cause of concern in the State of Tennessee, as well as throughout the world. Including chirality in the chemical fingerprint database can potentially allow for rapid determination of starting materials used for synthesis, but can also provide identity to a specific clandestine chemist, in theory. The objective of this research was to incorporate needed enantiomeric resolution data of seized clandestine drugs in the regional chemical fingerprint database to further differentiate between clandestine chemists. The separation of enantiomers was carried out by means of liquid chromatography coupled to a triple quadrupole mass spectrometer. Two different columns, Cellulose-2 and CHIRALPAK-CBH with cellulose tris(3-chloro-4-methylphenylcarbamate) and protein cellobiohydrolase as chiral selectors, respectively, were analyzed for enantioseparation ability. A chromatography method for simultaneous enantioseparation of ten different analytes using standards was optimized on the CHIRALPAK-CBH column, which proved to be the one that allowed sufficient enantioseparation ability. Instrument parameters such as retention time, resolution, intraday %RSD of retention times, interday %RSD of retention times, detection limit and quantitation limit were determined. Confiscated clandestine samples provided by the Cookeville Police Department were extracted and analyzed using the optimized HPLC method.