The determination of common anabolic steroid and stimulants in nutritional supplements by HPLC-DAD and LC-MS

J Chromatogr Sci. 2020 Apr 23;58(4):355-361. doi: 10.1093/chromsci/bmz121.

Abstract

A high-performance liquid chromatography method employing a diode-array detector and mass spectrometry detector was developed, validated and implemented for determining Synephrine, Caffeine, Clenbuterol, Nandrolone, Testosterone and Methylhexaneamine in Nutritional supplements. The use of Nutritional supplements is widespread. Hazards relating to concentration, composition, individual contaminants, supplements interactions as well as positive doping results among athletes present increasing concerns regarding nutritional supplement consuming. The proposed method was validated according to the International Conference on the Harmonization of the Technical Requirements for Registration of Pharmaceuticals for Human Use (ICH) standards. The proposed method observed to be accurate, linear, precise, sensitive, required minimal sample preparation and uncomplicated mobile phase. The implementation of the proposed method on nine commercial supplements shows that inaccurate labeling for some supplements regarding the concentration of the ingredients.

Keywords: Caffeine; Clenbuterol; Doping; HPLC-DAD; LC-MS; Methylhexaneamine; Nandrolone; Nutritional supplements contamination; Synephrine; Testosterone.

MeSH terms

  • Amines / analysis
  • Caffeine / analysis
  • Central Nervous System Stimulants / analysis
  • Chromatography, High Pressure Liquid / methods*
  • Chromatography, Liquid / methods
  • Clenbuterol / analysis
  • Dietary Supplements / analysis*
  • Mass Spectrometry / methods*
  • Nandrolone / analysis
  • Reproducibility of Results
  • Synephrine / analysis
  • Testosterone Congeners / analysis*

Substances

  • Amines
  • Central Nervous System Stimulants
  • Testosterone Congeners
  • methylhexaneamine
  • Caffeine
  • Nandrolone
  • Synephrine
  • Clenbuterol