Journal
JOURNAL OF CHROMATOGRAPHY A
Volume 1216, Issue 28, Pages 5340-5346Publisher
ELSEVIER SCIENCE BV
DOI: 10.1016/j.chroma.2009.05.040
Keywords
Clenbuterol; Metoprolol; Propranolol; Hollow fibre-protected liquid-phase microextraction; In situ derivatization
Funding
- National Nature Sciences Funding of China [20735002, 20675016, 20877019]
- Key Science and Technique Cultivation Fund of College Innovation Project
- Ministry of Education of China [708056]
- Key Special Purpose Funding of Physical Education Bureau of Fujian Province [HX2005-74]
- Nature Sciences Funding of Fujian Province [2007J0279]
- Research Foundation of Education Bureau of Fujian Province [2007F5067]
- Key Program of Science and Technology Department of Fujian Province [200710020, 2008Y0015]
- Plan of the University New Century Outstanding Talent of Fujian Province [HX2006-101]
- Agilent Technologies Co., Ltd.
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A method using hollow fibre-protected liquid-phase microextraction (HF-LPME) with in situ derivatization followed by gas chromatography/mass spectrometry (GC/MS) was established for the analysis of beta-agonists and beta-blockers in urine. Because it can simultaneously extract and derivatize compounds of interest by methylbenzol and N-methyl-N-(trimethylsilyl) trifluoroacetamide (MSTFA) in HF-LPME, the approach overcomes the drawbacks of considerable time-consuming and tedious operation, meanwhile improves enrichment multiple. The optimized conditions were extraction for 20 min at 35 degrees C with 5.0 mu L of mixed extraction solvent (methylbenzol/MSTFA=1:1, v/v) with stirring speed of 925 rpm in 5.0 mL sample under pH 12.0 and 14% (w/v) NaCl. The method provided very wide linear ranges (0.25-400 ng mL(-1)) and low detection limits in the range of 0.08-0.10 ng mL(-1) for clenbuterol, metoprolol and propranolol while enrichment factors reached up to 256. The analytes could be determined in spiked urine by the method with high extraction efficacy (93.79-109.04% recoveries) and precision (<9.70% RSD). It has a satisfactory result for metoprolol in practical human urine samples for a single-dose administration of 50 mg after 36 h. The proposed method only needs few microliters of organic solvent and derivatizing agent; the operation is simple, convenient and rapid for the trace analysis of beta-agonists and beta-blockers in biological fluids: it can be readily generalized for high sample throughput. So, it is hopeful that the study will facilitate the monitoring of beta-agonists and beta-blockers in the competition sports. (C) 2009 Elsevier B.V. All rights reserved.
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