Enantiomeric separation of new cathinone derivatives designer drugs by capillary electrochromatography using a chiral stationary phase, based on amylose tris(5-chloro-2-methylphenylcarbamate).
In this study, a chiral CEC method for the enantiomeric separation of ten cathinone derivatives, by means of a polysaccharide-based chiral stationary phase, has been developed. Capillary columns of 100 μm id packed with amylose tris(5-chloro-2-methylphenylcarbamate) coated on silica, also called Sepapak 3 or Lux Amylose-2, were used to achieve the enantioseparation of the studied designer drugs. Enantioresolution, chromatographic retention, and separation efficiency were evaluated in dependence of mobile-phase composition in terms of the content of the organic modifier, nature, and pH buffer. To obtain a sensitivity improvement, a field-amplified sample injection was evaluated optimizing the sample solvent composition and injection time. The LODs and LOQs values were in the range 25-100 and 50-150 ng/mL, respectively, for all the racemic compounds. Good results in terms of resolution (Rs ), separation efficiency (N/m), and short analysis times were obtained using a mixture of ACN/methanol/sodium acetate pH 9 (89/10/1, v/v/v). Applying a voltage of 10 kV and a temperature of 20°C, the analyzed cathinone derivatives were separated in their enantiomers in less than 10 min. A study, concerning the method precision, in terms of intra- and interday repeatability and column-to-column reproducibility was carried out in accordance with the analytical procedures for method validation. Intra- and interday repeatability provided RSD values in the ranges 1.1-1.7, 1.3-2.3% for retention time and 1.3-2.6, 2.1-3.4% for peak area, respectively.
Institute of Chemical Methodologies, Italian National Research Council, Monterotondo, Rome, Italy.
Zeineb
Z
Aturki
Martin G
MG
Schmid
Bezhan
B
Chankvetadze
Salvatore
S
Fanali
D000470:Alkaloids / Q000032:analysis / Q000737:chemistry* / Q000302:isolation & purification*; D000688:Amylose / Q000031:analogs & derivatives* / Q000737:chemistry; D053801:Capillary Electrochromatography / Q000295:instrumentation* / Q000379:methods; D002219:Carbamates / Q000737:chemistry*; D015198:Designer Drugs / Q000032:analysis / Q000737:chemistry* / Q000302:isolation & purification*; D006863:Hydrogen-Ion Concentration; D015203:Reproducibility of Results; D013237:Stereoisomerism; D013696:Temperature
D000470:Alkaloids; D002219:Carbamates; D015198:Designer Drugs; C582281:amylose-tris-(5-chloro-2-methylphenylcarbamate); C023665:cathinone; D000688:Amylose
Capillary electrochromatography; Cathinone derivatives; Enantiomeric separation; Polysaccharide-based chiral stationary phase