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Determination of clenbuterol in bovine urine using gas chromatography-mass spectrometry following clean-up on an ion-exchange resin.
J Chromatogr B Biomed Sci Appl. 1999 May 14; 728(1):67-73.JC

Abstract

A gas chromatographic-mass spectrometric method was developed for the determination of residues of clenbuterol in bovine urine. The method involves a simple cation-exchange clean-up and concentration of clenbuterol in the acidified urine, followed by ethyl acetate extraction. The analyte is determined as the di-trimethylsilyl derivative and quantitated against an internal standard of penbutolol. Using a 5-ml sample of urine, a detection limit of 0.07 ng/ml can be achieved with recoveries close to 100% for fortification levels of 0.2 and 1 ng/ml. By increasing the sample volume to 50 ml, a detection limit below 0.01 ng/ml was achievable with recovery averaging 70%. The coefficient of variation of the assay ranged from 15% at 0.01 ng/ml (50-ml sample) to 6% at 1 ng/ml (5-ml sample). It was demonstrated that the method can detect the presence of clenbuterol in bovine urine at sub-ppb (ng/ml) levels using low resolution GC-MS with electron impact (EI) ionization.

Authors+Show Affiliations

Australian Government Analytical Laboratories, Pymble, NSW.No affiliation info available

Pub Type(s)

Journal Article

Language

eng

PubMed ID

10379658

Citation

Whaites, L X., and E J. Murby. "Determination of Clenbuterol in Bovine Urine Using Gas Chromatography-mass Spectrometry Following Clean-up On an Ion-exchange Resin." Journal of Chromatography. B, Biomedical Sciences and Applications, vol. 728, no. 1, 1999, pp. 67-73.
Whaites LX, Murby EJ. Determination of clenbuterol in bovine urine using gas chromatography-mass spectrometry following clean-up on an ion-exchange resin. J Chromatogr B Biomed Sci Appl. 1999;728(1):67-73.
Whaites, L. X., & Murby, E. J. (1999). Determination of clenbuterol in bovine urine using gas chromatography-mass spectrometry following clean-up on an ion-exchange resin. Journal of Chromatography. B, Biomedical Sciences and Applications, 728(1), 67-73.
Whaites LX, Murby EJ. Determination of Clenbuterol in Bovine Urine Using Gas Chromatography-mass Spectrometry Following Clean-up On an Ion-exchange Resin. J Chromatogr B Biomed Sci Appl. 1999 May 14;728(1):67-73. PubMed PMID: 10379658.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Determination of clenbuterol in bovine urine using gas chromatography-mass spectrometry following clean-up on an ion-exchange resin. AU - Whaites,L X, AU - Murby,E J, PY - 1999/6/24/pubmed PY - 1999/6/24/medline PY - 1999/6/24/entrez SP - 67 EP - 73 JF - Journal of chromatography. B, Biomedical sciences and applications JO - J. Chromatogr. B Biomed. Sci. Appl. VL - 728 IS - 1 N2 - A gas chromatographic-mass spectrometric method was developed for the determination of residues of clenbuterol in bovine urine. The method involves a simple cation-exchange clean-up and concentration of clenbuterol in the acidified urine, followed by ethyl acetate extraction. The analyte is determined as the di-trimethylsilyl derivative and quantitated against an internal standard of penbutolol. Using a 5-ml sample of urine, a detection limit of 0.07 ng/ml can be achieved with recoveries close to 100% for fortification levels of 0.2 and 1 ng/ml. By increasing the sample volume to 50 ml, a detection limit below 0.01 ng/ml was achievable with recovery averaging 70%. The coefficient of variation of the assay ranged from 15% at 0.01 ng/ml (50-ml sample) to 6% at 1 ng/ml (5-ml sample). It was demonstrated that the method can detect the presence of clenbuterol in bovine urine at sub-ppb (ng/ml) levels using low resolution GC-MS with electron impact (EI) ionization. SN - 1387-2273 UR - https://www.unboundmedicine.com/medline/citation/10379658/Determination_of_clenbuterol_in_bovine_urine_using_gas_chromatography_mass_spectrometry_following_clean_up_on_an_ion_exchange_resin_ DB - PRIME DP - Unbound Medicine ER -