A novel protocol for molecularly imprinted polymer filaments online coupled to GC-MS for the determination of androgenic steroids in urine

J Sep Sci. 2013 Dec;36(24):3903-10. doi: 10.1002/jssc.201300874. Epub 2013 Nov 15.

Abstract

An online system that can perform dynamic microextraction, on-coating derivatization and desorption, and subsequent GC-MS analysis with a large-volume injection was developed. A derivatization cell as the conjunction of the online system was developed for the online extraction and derivatization. To evaluate the feasibility of the online system, methyltestosterone molecularly imprinted polymer filaments (MIPFs) were prepared for the selective online extraction of five androgenic steroids, namely, methyltestosterone, testosterone, epitestosterone, nandrolone, and metandienone. Under the optimized conditions, the detection limits of testosterone and epitestosterone were 0.09 and 0.12 μg/L, respectively, which were under the minimum required performance limits between 2 and 10 μg/L from the World Anti-Doping Agency. The detection limits of the other three androgenic steroids were varied from 0.04 to 0.18 μg/L. Finally, the MIPFs-GC-MS method was applied for the determination of androgenic steroids in urine, and satisfactory recovery (78.0-96.9%) and reproducibility (3.2-8.9%) were obtained. The proposed online coupling system offers an attractive alternative for hyphenation to GC instruments and could also be extended to other adsorptive materials.

Keywords: Androgenic steroids; Doping; GC-MS; Large volume injection; Molecularly imprinted polymers.

Publication types

  • Research Support, Non-U.S. Gov't

MeSH terms

  • Androgens / urine*
  • Epitestosterone / urine
  • Gas Chromatography-Mass Spectrometry / instrumentation
  • Gas Chromatography-Mass Spectrometry / methods*
  • Humans
  • Male
  • Methandrostenolone / urine
  • Methyltestosterone / urine
  • Molecular Imprinting*
  • Nandrolone / urine
  • Polymers / chemical synthesis
  • Polymers / chemistry*
  • Testosterone / urine

Substances

  • Androgens
  • Polymers
  • Testosterone
  • Epitestosterone
  • Nandrolone
  • Methandrostenolone
  • Methyltestosterone