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Hyphenation of coupled-column liquid chromatography and thermospray tandem mass spectrometry for the rapid determination of beta 2-agonist residues in bovine urine using direct large-volume sample injection. Set-up of single-residue methods for clenbuterol and salbutamol.
J Mass Spectrom. 1996 Apr; 31(4):418-26.JM

Abstract

In a previous work, coupled-column LC (LC/LC) with direct large-volume sample injection for the analysis of beta 2-agonists in bovine urine was investigated, in view of its combination with thermospray (TSP) tandem mass spectrometric (MS/MS) detection. In this work, the potential of both conventional LC and LC/LC coupled to TSP-MS/MS for the rapid determination of beta 2-agonists in bovine urine was evaluated. It was first established that, in order to avoid disturbances in TSP-MS/MS detection due to changes in pressure and flow rate of the mobile phase, LC/LC is preferable to conventional LC. Then, selecting clenbuterol and salbutamol as model compounds for the class of beta 2-agonists, two single-residue LC/LC/TSP-MS/MS methods were developed, permitting the determination of the analytes in bovine urine samples with a limit of quantification of at least 0.1 ng, ml-1, with a sample throughput of 4 h-1. The methods were validated by analysing both spiked urine samples and samples containing clenbuterol or salbutamol residues. Mean recoveries from urine samples spiked with clenbuterol at levels of 5 and 0.22 ng ml-1 were 107% (n = 9, RSD = 7.4%) and 102% (n = 6, RSD = 14%), respectively. A bovine urine sample containing 1.28 ng ml-1 clenbuterol residue (previously quantified by GC/MS) was re-analysed by LC/LC/TSP-MS/MS on four different days (n = 3, each day) and yielded a mean concentration of 1.31 ng ml-1, with a reproducibility of 8.4%. Bovine urine samples spiked with salbutamol at levels of 10.8 and 0.55 ng ml-1 yielded mean recoveries of 101% (n = 3, RSD = 1%) and 89% (n = 3, RSD = 13%), respectively. In bovine urine samples containing salbutamol residues, the concentrations of unconjugated salbutamol were found to be in the range 8-57 ng ml-1.

Authors+Show Affiliations

National Institute of Public Health and Environmental Protection (RIVM), Bilthoven, The Netherlands.No 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

8799286

Citation

Hogendoorn, E A., et al. "Hyphenation of Coupled-column Liquid Chromatography and Thermospray Tandem Mass Spectrometry for the Rapid Determination of Beta 2-agonist Residues in Bovine Urine Using Direct Large-volume Sample Injection. Set-up of Single-residue Methods for Clenbuterol and Salbutamol." Journal of Mass Spectrometry : JMS, vol. 31, no. 4, 1996, pp. 418-26.
Hogendoorn EA, van Zoonen P, Polettini A, et al. Hyphenation of coupled-column liquid chromatography and thermospray tandem mass spectrometry for the rapid determination of beta 2-agonist residues in bovine urine using direct large-volume sample injection. Set-up of single-residue methods for clenbuterol and salbutamol. J Mass Spectrom. 1996;31(4):418-26.
Hogendoorn, E. A., van Zoonen, P., Polettini, A., & Montagna, M. (1996). Hyphenation of coupled-column liquid chromatography and thermospray tandem mass spectrometry for the rapid determination of beta 2-agonist residues in bovine urine using direct large-volume sample injection. Set-up of single-residue methods for clenbuterol and salbutamol. Journal of Mass Spectrometry : JMS, 31(4), 418-26.
Hogendoorn EA, et al. Hyphenation of Coupled-column Liquid Chromatography and Thermospray Tandem Mass Spectrometry for the Rapid Determination of Beta 2-agonist Residues in Bovine Urine Using Direct Large-volume Sample Injection. Set-up of Single-residue Methods for Clenbuterol and Salbutamol. J Mass Spectrom. 1996;31(4):418-26. PubMed PMID: 8799286.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Hyphenation of coupled-column liquid chromatography and thermospray tandem mass spectrometry for the rapid determination of beta 2-agonist residues in bovine urine using direct large-volume sample injection. Set-up of single-residue methods for clenbuterol and salbutamol. AU - Hogendoorn,E A, AU - van Zoonen,P, AU - Polettini,A, AU - Montagna,M, PY - 1996/4/1/pubmed PY - 2000/6/22/medline PY - 1996/4/1/entrez SP - 418 EP - 26 JF - Journal of mass spectrometry : JMS JO - J Mass Spectrom VL - 31 IS - 4 N2 - In a previous work, coupled-column LC (LC/LC) with direct large-volume sample injection for the analysis of beta 2-agonists in bovine urine was investigated, in view of its combination with thermospray (TSP) tandem mass spectrometric (MS/MS) detection. In this work, the potential of both conventional LC and LC/LC coupled to TSP-MS/MS for the rapid determination of beta 2-agonists in bovine urine was evaluated. It was first established that, in order to avoid disturbances in TSP-MS/MS detection due to changes in pressure and flow rate of the mobile phase, LC/LC is preferable to conventional LC. Then, selecting clenbuterol and salbutamol as model compounds for the class of beta 2-agonists, two single-residue LC/LC/TSP-MS/MS methods were developed, permitting the determination of the analytes in bovine urine samples with a limit of quantification of at least 0.1 ng, ml-1, with a sample throughput of 4 h-1. The methods were validated by analysing both spiked urine samples and samples containing clenbuterol or salbutamol residues. Mean recoveries from urine samples spiked with clenbuterol at levels of 5 and 0.22 ng ml-1 were 107% (n = 9, RSD = 7.4%) and 102% (n = 6, RSD = 14%), respectively. A bovine urine sample containing 1.28 ng ml-1 clenbuterol residue (previously quantified by GC/MS) was re-analysed by LC/LC/TSP-MS/MS on four different days (n = 3, each day) and yielded a mean concentration of 1.31 ng ml-1, with a reproducibility of 8.4%. Bovine urine samples spiked with salbutamol at levels of 10.8 and 0.55 ng ml-1 yielded mean recoveries of 101% (n = 3, RSD = 1%) and 89% (n = 3, RSD = 13%), respectively. In bovine urine samples containing salbutamol residues, the concentrations of unconjugated salbutamol were found to be in the range 8-57 ng ml-1. SN - 1076-5174 UR - https://www.unboundmedicine.com/medline/citation/8799286/Hyphenation_of_coupled_column_liquid_chromatography_and_thermospray_tandem_mass_spectrometry_for_the_rapid_determination_of_beta_2_agonist_residues_in_bovine_urine_using_direct_large_volume_sample_injection__Set_up_of_single_residue_methods_for_clenbuterol_and_salbutamol_ L2 - https://doi.org/10.1002/(SICI)1096-9888(199604)31:4<418::AID-JMS315>3.0.CO;2-F DB - PRIME DP - Unbound Medicine ER -