title: [Solid-phase microextraction coupled with capillary electrophoresis for doping analysis of propranolol enantiomers in urine using a sol-gel derived calix [4] arene fiber].
abstract: 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.
authors.affiliation: College of Chemistry and Molecular Sciences, Wuhan University, Wuhan 430072, China.
authors.forename: Xingwang
authors.initials: X
authors.lastname: Zhou
authors.forename: Xiujuan
authors.initials: X
authors.lastname: Li
authors.forename: Zhaorui
authors.initials: Z
authors.lastname: Zeng
mesh_terms: D000818:Animals; D047250:Calixarenes / Q000737:chemistry*; D002241:Carbohydrates / Q000737:chemistry; D019075:Electrophoresis, Capillary / Q000379:methods*; D005782:Gels / Q000737:chemistry; D006863:Hydrogen-Ion Concentration; D057230:Limit of Detection; D008956:Models, Chemical; D011161:Porifera; D011433:Propranolol / Q000031:analogs & derivatives / Q000737:chemistry* / Q000652:urine; D012015:Reference Standards; D012680:Sensitivity and Specificity; D052617:Solid Phase Microextraction / Q000379:methods*; D013237:Stereoisomerism; D013696:Temperature
chemical_list: D002241:Carbohydrates; D005782:Gels; D047250:Calixarenes; D011433:Propranolol