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Combination of liquid chromatography/tandem mass spectrometry and gas chromatography/mass spectrometry for the detection of 21 anabolic steroid residues in bovine urine.
J Mass Spectrom. 2005 Jun; 40(6):731-8.JM

Abstract

For the detection of anabolic steroid residues in bovine urine, a highly sensitive liquid chromatographic/electrospray ionization tandem mass spectrometric (LC/ESI-MS/MS) method was developed using both positive and negative ionization. For four compounds the ESI mode was not sensitive enough and gas chromatographic/mass spectrometric GC/MS detection was therefore still necessary as a complementary method. The sample clean-up consisted of solid-phase extraction (SPE) on a C(18) column followed by enzymatic hydrolysis and a second solid-phase extraction on a combination of a C(18) and a NH(2) column. After this last SPE clean-up, the eluate was split into two equal aliquots. One aliquot was further purified and after derivatization used for GC/MS analysis. The other aliquot was analyzed with LC/MS/MS in both ESI+ and ESI- modes. The method was validated according to the European Commission Decision 2002/657/EC. Decision limits (CCalpha) were between 0.16 and 1 ng ml(-1) for the compounds detected with the LC/MS/MS method. The developed method is used in routine analysis in our laboratory.

Authors+Show Affiliations

Ghent University, Laboratory of Food Analysis, Harelbekestraat 72, B-9000 Ghent, Belgium. christof.vanpoucke@ugent.beNo affiliation info availableNo affiliation info available

Pub Type(s)

Journal Article

Language

eng

PubMed ID

15782394

Citation

Van Poucke, Christof, et al. "Combination of Liquid Chromatography/tandem Mass Spectrometry and Gas Chromatography/mass Spectrometry for the Detection of 21 Anabolic Steroid Residues in Bovine Urine." Journal of Mass Spectrometry : JMS, vol. 40, no. 6, 2005, pp. 731-8.
Van Poucke C, Van De Velde M, Van Peteghem C. Combination of liquid chromatography/tandem mass spectrometry and gas chromatography/mass spectrometry for the detection of 21 anabolic steroid residues in bovine urine. J Mass Spectrom. 2005;40(6):731-8.
Van Poucke, C., Van De Velde, M., & Van Peteghem, C. (2005). Combination of liquid chromatography/tandem mass spectrometry and gas chromatography/mass spectrometry for the detection of 21 anabolic steroid residues in bovine urine. Journal of Mass Spectrometry : JMS, 40(6), 731-8.
Van Poucke C, Van De Velde M, Van Peteghem C. Combination of Liquid Chromatography/tandem Mass Spectrometry and Gas Chromatography/mass Spectrometry for the Detection of 21 Anabolic Steroid Residues in Bovine Urine. J Mass Spectrom. 2005;40(6):731-8. PubMed PMID: 15782394.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Combination of liquid chromatography/tandem mass spectrometry and gas chromatography/mass spectrometry for the detection of 21 anabolic steroid residues in bovine urine. AU - Van Poucke,Christof, AU - Van De Velde,Mario, AU - Van Peteghem,Carlos, PY - 2005/3/23/pubmed PY - 2005/8/5/medline PY - 2005/3/23/entrez SP - 731 EP - 8 JF - Journal of mass spectrometry : JMS JO - J Mass Spectrom VL - 40 IS - 6 N2 - For the detection of anabolic steroid residues in bovine urine, a highly sensitive liquid chromatographic/electrospray ionization tandem mass spectrometric (LC/ESI-MS/MS) method was developed using both positive and negative ionization. For four compounds the ESI mode was not sensitive enough and gas chromatographic/mass spectrometric GC/MS detection was therefore still necessary as a complementary method. The sample clean-up consisted of solid-phase extraction (SPE) on a C(18) column followed by enzymatic hydrolysis and a second solid-phase extraction on a combination of a C(18) and a NH(2) column. After this last SPE clean-up, the eluate was split into two equal aliquots. One aliquot was further purified and after derivatization used for GC/MS analysis. The other aliquot was analyzed with LC/MS/MS in both ESI+ and ESI- modes. The method was validated according to the European Commission Decision 2002/657/EC. Decision limits (CCalpha) were between 0.16 and 1 ng ml(-1) for the compounds detected with the LC/MS/MS method. The developed method is used in routine analysis in our laboratory. SN - 1076-5174 UR - https://www.unboundmedicine.com/medline/citation/15782394/Combination_of_liquid_chromatography/tandem_mass_spectrometry_and_gas_chromatography/mass_spectrometry_for_the_detection_of_21_anabolic_steroid_residues_in_bovine_urine_ DB - PRIME DP - Unbound Medicine ER -