Solid-phase microextraction coupled with capillary electrophoresis for doping analysis of propranolol enantiomers in urine using a sol-gel derived calix [4] arene fiber
Zhou, X.; Li, X.; Zeng, Z.
Se Pu 24(1): 1-4
2006
ISSN/ISBN: 1000-8713 PMID: 16827299 Document Number: 604169
A new type fiber coated with diglycidyloxy calix [4] arene/hydroxy-terminated silicone oil (diglycidyloxy-C [4] arene/OH-TSO) made by sol-gel method was prepared for capillary electrophoresis (CE) sample pretreatment. By using headspace solid-phase microextraction (HS-SPME) combined with a novel back-extraction facility coupled off-line to capillary zone electrophoresis (CZE), the determination of propranolol enantiomers in urine was achieved with combination of ultrasonic back-extraction and field amplified sample injection (FASI) technologies. Extraction and back-extraction parameters were optimized. The clean-up effect and preconcentration effect were realized without derivatization during the SPME process in terms of this strongly polar and thermally stable compound. Preconcentration of the sample by calix [4] arene fiber increased the sensitivity, yielding a limit of detection (LOD) of 0.01 mg/L by CZE-diode array detection (DAD). Method repeatability (relative standard deviations (RSD) < 6.5%) and fiber reusability (> 150 extraction procedures) were observed over a wide linear range of propranolol (0.05 - 10 mg/L) in urine samples. Compared with commercial SPME stationary phases, the new coating showed higher extraction efficiency and this SPME-CZE-DAD procedures could meet the demand of minimum required performance limits (MRPL) set by the World Anti-Doping Agency (WADA) for the detection of propranolol in urine samples.