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Analysis of beta-agonists and beta-blockers in urine using hollow fibre-protected liquid-phase microextraction with in situ derivatization followed by gas chromatography/mass spectrometry.
J Chromatogr A. 2009 Jul 10; 1216(28):5340-6.JC

Abstract

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 microL 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.

Authors+Show Affiliations

The Sport Science Research Center, Ministry of Education Key Laboratory of Analysis and Detection for Food Safety, Fuzhou University, Fuzhou, Fujian 350002, China.No affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info available

Pub Type(s)

Journal Article
Research Support, Non-U.S. Gov't

Language

eng

PubMed ID

19501827

Citation

Liu, Wei, et al. "Analysis of Beta-agonists and Beta-blockers in Urine Using Hollow Fibre-protected Liquid-phase Microextraction With in Situ Derivatization Followed By Gas Chromatography/mass Spectrometry." Journal of Chromatography. A, vol. 1216, no. 28, 2009, pp. 5340-6.
Liu W, Zhang L, Wei Z, et al. Analysis of beta-agonists and beta-blockers in urine using hollow fibre-protected liquid-phase microextraction with in situ derivatization followed by gas chromatography/mass spectrometry. J Chromatogr A. 2009;1216(28):5340-6.
Liu, W., Zhang, L., Wei, Z., Chen, S., & Chen, G. (2009). Analysis of beta-agonists and beta-blockers in urine using hollow fibre-protected liquid-phase microextraction with in situ derivatization followed by gas chromatography/mass spectrometry. Journal of Chromatography. A, 1216(28), 5340-6. https://doi.org/10.1016/j.chroma.2009.05.040
Liu W, et al. Analysis of Beta-agonists and Beta-blockers in Urine Using Hollow Fibre-protected Liquid-phase Microextraction With in Situ Derivatization Followed By Gas Chromatography/mass Spectrometry. J Chromatogr A. 2009 Jul 10;1216(28):5340-6. PubMed PMID: 19501827.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Analysis of beta-agonists and beta-blockers in urine using hollow fibre-protected liquid-phase microextraction with in situ derivatization followed by gas chromatography/mass spectrometry. AU - Liu,Wei, AU - Zhang,Lan, AU - Wei,Zhenyi, AU - Chen,Shengping, AU - Chen,Guonan, Y1 - 2009/05/21/ PY - 2009/02/06/received PY - 2009/05/09/revised PY - 2009/05/14/accepted PY - 2009/6/9/entrez PY - 2009/6/9/pubmed PY - 2009/9/15/medline SP - 5340 EP - 6 JF - Journal of chromatography. A JO - J Chromatogr A VL - 1216 IS - 28 N2 - 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 microL 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. SN - 1873-3778 UR - https://www.unboundmedicine.com/medline/citation/19501827/Analysis_of_beta_agonists_and_beta_blockers_in_urine_using_hollow_fibre_protected_liquid_phase_microextraction_with_in_situ_derivatization_followed_by_gas_chromatography/mass_spectrometry_ L2 - https://linkinghub.elsevier.com/retrieve/pii/S0021-9673(09)00775-4 DB - PRIME DP - Unbound Medicine ER -