Determination of the hormonal growth promoter 17alpha-methyltestosterone in food-producing animals: bovine hair analysis by HPLC-MS/MS

Meat Sci. 2010 Jan;84(1):196-201. doi: 10.1016/j.meatsci.2009.08.047. Epub 2009 Aug 28.

Abstract

This paper describes the development, validation and application of a confirmatory method to detect 17alpha-methyltestosterone (MT) in bovine hair, to aid in controlling the administration of this growth promoter in meat-producing animals. After cryogenic grinding, MT was removed from the hair matrix using a single step extraction procedure with acetonitrile. Hydroxylamine derivatisation was used to enhance analyte determination with an electrospray ionisation (ESI) source. Determination was carried out using a triple quadrupole liquid chromatography tandem mass spectrometer (LC-MS/MS) in multiple reaction monitoring mode (MRM). The method was validated in accordance with the criteria defined in Commission Decision 2002/657/EC and using deuterated testosterone (T-d(3)) as the internal standard. The decision limit (CCalpha) was 0.07 ng g(-1) and the detection capability (CCbeta) was 0.12 ng g(-1). Repeatability was CV% (7%), within-laboratory reproducibility was CV% (11.0%), and trueness was (87%). Applicability of the method was demonstrated in an animal study. Samples obtained from animal experiments were analyzed and the presence of MT was confirmed.

Publication types

  • Research Support, Non-U.S. Gov't
  • Validation Study

MeSH terms

  • Anabolic Agents / analysis*
  • Anabolic Agents / chemistry
  • Anabolic Agents / isolation & purification
  • Anabolic Agents / pharmacokinetics
  • Analytic Sample Preparation Methods
  • Androgens / analysis
  • Androgens / chemistry
  • Androgens / isolation & purification
  • Androgens / pharmacokinetics
  • Animals
  • Calibration
  • Cattle*
  • Chromatography, High Pressure Liquid / methods
  • Drug Residues / analysis
  • Drug Residues / chemistry
  • Drug Residues / isolation & purification
  • Drug Residues / pharmacokinetics
  • Food Contamination / prevention & control
  • Hair / chemistry*
  • Hydroxylamine / chemistry
  • Limit of Detection
  • Methyltestosterone / analysis*
  • Methyltestosterone / chemistry
  • Methyltestosterone / isolation & purification
  • Methyltestosterone / pharmacokinetics
  • Pigmentation
  • Reproducibility of Results
  • Spectrometry, Mass, Electrospray Ionization / methods*
  • Tandem Mass Spectrometry

Substances

  • Anabolic Agents
  • Androgens
  • Hydroxylamine
  • Methyltestosterone