Fast analysis of 19 anabolic steroids in bovine tissues by high performance liquid chromatography with tandem mass spectrometry

Abstract

For the detection of 19 steroid hormones in bovine muscle, a fast and sensitive liquid chromatography with electrospray ionization tandem mass spectrometry method was developed using both positive and negative ionization mode. Chromatographic separation on Poroshell 120‐EC C18 column was achieved in less than 10 min using isocratic elution of mobile phase of acetonitrile/methanol/water. The compounds were extracted from muscle tissue using ethyl acetate and quick, easy, cheap, effective, rugged, and safe technique. The purification of the obtained extract was performed by dispersive solid‐phase extraction with sorbents C18, primary secondary amine and magnesium sulphate. The method was validated in accordance with the Commission Decision 2002/657/EC. For all steroids tested good recoveries were obtained (from 51.2 to 121.4%) in the concentration range from decision limits until 5 µg/kg. The values of decision limits and the detection capabilities for individual compounds were in the range 0.10–0.48 and 0.17–0.95 µg/kg, respectively. The method was characterized by satisfactory linearity for most compounds (correlation coefficients > 0.99) and the reproducibility was lower than 35%. The elaborated procedure has met the criteria for confirmatory methods and is currently used in the official control of hormones.

Determination of anabolic androgenic steroids in dietary supplements and external drugs by magnetic solid‐phase extraction combined with high‐performance liquid chromatography–tandem mass spectrometry

“…A comparison of the developed method and those reported previously is listed in Table S2 in the Supporting Information. As seen, compared with Wozniak's work [14] and Shin's work [34], the proposed MSPE method was much simpler with lower LODs than QuEChERS or SPE methods. In contrast with Shimko's study [35], no isotopic internal standards were required in the proposed method, and the LODs obtained in this study were comparable with those obtained by Shimko.…”

“…Arthur et al [11] developed a field asymmetric waveform ion mobility spectrometry combined with LC-MS for the analysis of metabolites of AASs in urine. Aqai et al [13] developed a generic highthroughput bioaffinity LC-MS method for the screening and identification of steroids in dietary supplements; Wozniak et al combined LC-MS/MS with liquid-phase extraction (LPE) and dispersive SPE for the determination of 19 steroid hormones in bovine muscle [14]. However, the composition of the sample matrix prepared for analysis is complicated, which would influence the determination of AASs.…”

Hormones and Hormonal Anabolics: Residues in Animal Source Food, Potential Public Health Impacts, and Methods of Analysis

“…is method is able to conduct screening and quantification assay of the compounds by producing precursors and product ions and finally quantifying and detecting each compound by using charge-to-mass ratio of each molecule, which is specific as a fingerprint for any target molecules captured on the mass detector [85,86].…”

Development of a method for the determination of sedatives in bovine and porcine urine and kidneys by liquid chromatography–tandem mass spectrometry

“…Out of concern for consumer safety, the EU requires testing for many substances that should not be present in food of animal origin ( 5 , 10 – 12 , 16 , 30 , 31 , 32 – 34 , 37 ). In order to best protect consumers, the EU frequently lengthens the list of substances monitored in member states.…”