Abstract
The chiral separation of sibutramine enantiomers was resolved succesfully by capillary zone electrophoresis using cyclodextrins (CDs) as chiral selectors. A complex screening of several different native and derivatized, neutral and ionized cyclodextrine derivatives was performed. The effects of buffer type, concentration and pH, cyclodextrin type and concentration, applied voltage, capillary temperature and injection parameters on the chiral resolution were examined. The best results on a very short fused silica capillary of 30 cm × 50 μm were obtained using a 50 mmol L-1 phosphate buffer containing 10 mmol L-1 randomly methylated β-CD at a pH of 4.5, 15 kV of voltage, temperature of 15 °C, injection parameters of 30 mbar s−1 and ultraviolet (UV) detection at 220 nm. The analytical performances of the optimized method were verified in terms of linearity, precision and robustness, and limit of detection and quantification were calculated.
Highlights
Sibutramine [(±)-1-(p-chlorophenyl)a-isobutyl-N,N-dimethyl cyclobutane methylamine hydrochloride] is an oral anorexiant structurally related to amphetamine
In 2010, sibutramine was removed from the European market, based on new data from the Sibutramine Cardiovascular Outcomes Trial (SCOUT), which demonstrated an increased risk of cardiovascular events, such as stroke or heart attack
Preliminary studies were performed in order to find the suitable background electrolyte (BGE) and pH for the determination
Summary
Sibutramine [(±)-1-(p-chlorophenyl)a-isobutyl-N,N-dimethyl cyclobutane methylamine hydrochloride] is an oral anorexiant structurally related to amphetamine. Chiral separation of sibutramine was investigated by CE by screening different native and derivatized, neutral and ionized cyclodextrin (CD) derivatives as chiral selectors. All sample solutions and buffers were degassed by ultrasound for 5 min before use and filtered through a 0.25 μm membrane filter (Agilent Technologies, Santa Clara, CA, USA).
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