Enantiomeric separation of some common controlled stimulants by capillary electrophoresis with contactless conductivity detection

Electrophoresis. 2012 Jan;33(2):388-94. doi: 10.1002/elps.201100370. Epub 2011 Dec 13.

Abstract

CE methods with capacitively coupled contactless conductivity detection (C(4)D) were developed for the enantiomeric separation of the following stimulants: amphetamine (AP), methamphetamine (MA), ephedrine (EP), pseudoephedrine (PE), norephedrine (NE) and norpseudoephedrine (NPE). Acetic acid (pH 2.5 and 2.8) was found to be the optimal background electrolyte for the CE-C(4)D system. The chiral selectors, carboxymethyl-β-cyclodextrin (CMBCD), heptakis(2,6-di-O-methyl)-β-cyclodextrin (DMBCD) and chiral crown ether (+)-(18-crown-6)-2,3,11,12-tetracarboxylic acid (18C6H(4)), were investigated for their enantioseparation properties in the BGE. The use of either a single or a combination of two chiral selectors was chosen to obtain optimal condition of enantiomeric selectivity. Enantiomeric separation of AP and MA was achieved using the single chiral selector CMBCD and (hydroxypropyl)methyl cellulose (HPMC) as the modifier. A combination of the two chiral selectors, CMBCD and DMBCD and HPMC as the modifier, was required for enantiomeric separation of EP and PE. In addition, a combination of DMBCD and 18C6H(4) was successfully applied for the enantiomeric separation of NE and NPE. The detection limits of the enantiomers were found to be in the range of 2.3-5.7 μmol/L. Good precisions of migration time and peak area were obtained. The developed CE-C(4)D method was successfully applied to urine samples of athletes for the identification of enantiomers of the detected stimulants.

Publication types

  • Research Support, Non-U.S. Gov't

MeSH terms

  • Acetic Acid / chemistry
  • Amphetamines / chemistry*
  • Amphetamines / isolation & purification
  • Amphetamines / urine
  • Central Nervous System Stimulants / chemistry*
  • Central Nervous System Stimulants / isolation & purification
  • Central Nervous System Stimulants / urine
  • Crown Ethers / chemistry
  • Electric Conductivity
  • Electrophoresis, Capillary / instrumentation
  • Electrophoresis, Capillary / methods*
  • Humans
  • Limit of Detection
  • Propanolamines / chemistry*
  • Propanolamines / isolation & purification
  • Propanolamines / urine
  • Reproducibility of Results
  • Stereoisomerism
  • beta-Cyclodextrins / chemistry

Substances

  • Amphetamines
  • Central Nervous System Stimulants
  • Crown Ethers
  • Propanolamines
  • beta-Cyclodextrins
  • carboxymethyl-beta-cyclodextrin
  • 18-crown-6 2,3,11,12-tetracarboxylic acid
  • heptakis(2,6-O-dimethyl)beta-cyclodextrin
  • Acetic Acid