Confirmatory method for the determination of nandrolone and trenbolone in urine samples using immunoaffinity cleanup and liquid chromatography-tandem mass spectrometry

J Chromatogr A. 2009 Nov 13;1216(46):8059-66. doi: 10.1016/j.chroma.2009.04.075. Epub 2009 May 4.

Abstract

A confirmatory method for the simultaneous determination of nandrolone (alpha and beta) and trenbolone (alpha and beta) in urine samples by liquid chromatography electrospray mass spectrometry (LC-MS-MS) was developed. After an enzymatic deconjugation, the urine was subjected to a one-step cleanup on a commercially available immunoaffinity chromatography cartridge. The analytes were detected by liquid chromatography-positive ion electrospray tandem mass spectrometry using deuterium labelled internal standards. The analytical procedure was applicable to bovine and swine urine samples. The procedure was validated as a quantitative confirmatory method according to the Commission Decision 2002/657/EC criteria. The results obtained showed that the method was suitable for statutory residues testing regarding the following performance characteristics: instrumental linearity, specificity, precision (repeatability and intra-laboratory reproducibility), recovery, decision limit (CCalpha), detection capability (CCbeta) and ruggedness. The decision limits (CCalpha) obtained, were between 0.54 and 0.60 microg L(-1); the recovery was above 64% for all the analytes. Repeatability was between 1.6% and 5.7% and within-laboratory reproducibility between 1.6% and 6.0% for all the steroids.

Publication types

  • Evaluation Study

MeSH terms

  • Animals
  • Cattle
  • Chromatography, Affinity / methods*
  • Chromatography, Affinity / veterinary
  • Chromatography, Liquid / methods*
  • Chromatography, Liquid / veterinary
  • Nandrolone / urine*
  • Swine
  • Tandem Mass Spectrometry / methods*
  • Tandem Mass Spectrometry / veterinary
  • Testosterone Congeners / urine*
  • Trenbolone Acetate / urine*

Substances

  • Testosterone Congeners
  • Nandrolone
  • Trenbolone Acetate