Detection of clenbuterol residues in beef sausages and its enantiomeric analysis using UHPLC–MS/MS: A risk of unintentional doping in sport field

Abstract

Clenbuterol (Clb) can be present in Mexico often but not all over the world in animal tissues and organs, therefore, potentially is derived from animal sources as well. The aims of this study were to develop and validate a method for detecting traces of clenbuterol in beef sausages. A calibration curve showed linearity in the range of 20-500 pg ml À1 . The limit of detection (LOD) and lower limit of quantification (LLOQ) were 5 and 10 pg g À1 , respectively. The analyte recovery was from 95.70% to 100.40% with an intraday relative standard deviation (RSD%) of 0.99%-2.10% and an interday RSD% of 0.54%-2.34%, R 2 = 0.9998. The methodology developed was applied successfully in 15 samples of beef sausage, and 73.3% of the samples tested contained racemic clenbuterol in concentrations between 30 and 471 pg g À1 .The UHPLC-MS/MS method developed combines high sensitivity with good selectivity and short chromatographic run time. Additionally, the enantiomeric analysis of clenbuterol performed in beef sausages showed a 59% for R-(À)-Clb and 41% for S-(+)-Clb. The presence of clenbuterol in beef sausages could represent a risk of unintentional doping in sport field, because the clenbuterol is a banned substance included in the World Anti-Doping Agency's (WADA) list of prohibited substances.

Annual banned‐substance review—Analytical approaches in human sports drug testing 2021/2022–

“…All zilpaterol concentrations, except for one occasion in the 5 × 50 μg study group, were found below 5 ng/ml, which is an important finding in consideration of WADA's Technical Letter TL23 concerning the minimum reporting level (MRL) for potential meat contaminants 111 . Moreover, no enantiomeric depletion was observed, in contrast to reports published for clenbuterol contamination scenarios 53,54 and urinary elimination profiles.…”

“…In order to provide additional data into elimination profiles of frequently observed SARMs, LGD-4033 and RAD140 (Figure 1, 2 and 4) were each administered to five male volunteers in single and multiple microdoses of 1, 10, and 50 μg, and urine was collected up to 47 days after administration. 50,51 The studies aimed at mimicking scenarios of contamination, where individuals (e.g., athletes) are exposed to low amounts of prohibited substances and how such an exposure is Moreover, no enantiomeric depletion was observed, in contrast to reports published for clenbuterol contamination scenarios 53,54 and urinary elimination profiles.…”

Quantification and enantiomeric distribution of clenbuterol in several bovine tissues using UHPLC–tandem mass spectrometry: Evaluation of a risk factor associated with meat contamination

“…The transition m / z 286 → 204 was used to monitor the 2 H 9 ‐Clb standard. This methodology has been described previously by our working group 23 …”

Detection of lean meat powder residues in pig liver based on TLC-SERRS

“…At present, more than 10 compounds such as terbutaline, salbutamol, clenbuterol, clorprenaline, bambuterol are collectively referred to as clenbuterol. [1][2][3][4][5] Various analytical techniques used for the determination of such drugs have been developed, such as enzyme-linked immunosorbent assay (ELISA), 6 capillary electrophoresis (CE), 7 high performance liquid chromatography (HPLC), 8 high performance liquid chromatography-mass spectrometry (HPLC-MS) [9][10][11][12] and so on. However, the above methods have some limitations, such as high cost, high operational requirements, and dependence on extraction.…”