The prevalence of doping in sport continues to be a concern in society
Wastewater-based Tracing of Doping Use
The prevalence of doping 🔑 in sport and in the community at large continues to be a concern in many societies.
Numerous test protocols are in 🔑 place to test individuals but the increased sensitivity of modern analytical techniques and the purity of the ultrapure water available 🔑 to use in testing have opened the scope for screening communal wastewater for drugs and their metabolites.
Causanilles et al (1) 🔑 have successfully developed and tested a procedure for 15 substances from the groups of anabolic steroids (used to promote muscle 🔑 growth), weight loss products (used to increase metabolism by burning fat) and masking agents in wastewater using solid phase extraction 🔑 to increase sensitivity and reduce matrix effects followed by liquid-chromatography coupled to high resolution mass spectrometry.
50 ml of sample were 🔑 spiked with an isotope-labeled internal standard, filtered, and acidified before concentration on a mix-mode cationic polymer-based cartridge.
The cartridge was washed 🔑 repeatedly before elution with acetonitrile.
This was evaporated, redissolved in water and finally reconstituted in 90:10 water/methanol to give a volume 🔑 of 0.5 ml.
This was analysed by UPLC (Ultra Performance Liquid Chromatography) coupled to a time-of-flight high-resolution mass spectrometer with a 🔑 C18 column and a water/methanol mobile phase with the methanol content ranging from 20 to 100%.
Limits of detection ranged from 🔑 0.
2 ngL-1 for anastrozole to 20 ngL-1 for trenbolone, nandrolone and mibolerone.
Water from an ELGA PURELAB Chorus 1 was used 🔑 throughout this work.
The absence of trace organic contaminants in the water is critical as water is used repeatedly in the 🔑 sample preparation: in the hydrochloric acid used to acidify the sample, to condition the SPE cartridge and to rinse it 🔑 twice, to enhance the removal of acetonitrile
and, finally, to reconstitute the sample ready for UPLC.
Water is also used as a 🔑 mobile phase in the chromatography.
Samples were taken from the inlets to wastewater treatment plants in locations where sporting events of 🔑 various types were taking place, before and during the events.
24-hour composite samples were usually obtained.
It was found to be essential 🔑 to freeze the samples prior to analysis.
A wide variety of analytes of interest were detected
particularly weight loss products.
In many cases, 🔑 significantly higher levels were detected during and just before the sporting events.
The study was not exhaustive and was more intended 🔑 to demonstrate the feasibility of the approach.1) A.Causanilles, V.Nordmann, D.Vughs, E.Emke, O.De Hon, F.Hernandez and P.
De Voogt, „wastewater-based tracing of 🔑 doping use by the general population and
amateur athletes", Analytical and Bioanalytical Chemistry, 410, 1793-1803, 2018
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