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On‐line preconcentration and enantioseparation of thalidomide racemates by CEC with the hyphenation of octyl and norvancomycin monoliths
Author(s) -
Tang AnNa,
Wang XiaoNan,
Ding GuoSheng,
Yan XiuPing
Publication year - 2009
Publication title -
electrophoresis
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.666
H-Index - 158
eISSN - 1522-2683
pISSN - 0173-0835
DOI - 10.1002/elps.200800303
Subject(s) - chemistry , chromatography , enantiomer , monolithic hplc column , detection limit , analytical chemistry (journal) , high performance liquid chromatography , solvent , stereochemistry , organic chemistry
A method was developed for simultaneous preconcentration and chiral separation of thalidomide enantiomers in human urine by CEC in combination with self‐concentration and solvent gradient effects. A 4 cm long octyl (C8) monolithic column was hyphenated with a 15 cm long norvancomycin (NVC)‐bonded monolithic column via a fluorinated ethylene–propylene interface. Sample solution was injected into the C8 monolithic column, the two thalidomide enantiomers were first preconcentrated on the C8 monolithic column, and then separated with a further concentration on the NVC‐bonded monolithic column by CEC. Injection of 34.8 mm plug of sample solution gave 278‐ and 298‐fold enhancement in sensitivity, and detection limits of 90 and 94 μg/L for the two thalidomide enantiomers. Peak areas of the two isomers were linear in a range of 0.5–50 mg/L. The precision for five replicate injections of 10 mg/L were 0.8–0.9 and 1.1–2.3% for the migration time and peak height, respectively. The developed method was applied to the determination of racemic thalidomide in spiked human urine samples.