Projets de recherche

Code: 22A10JP

There is a high demand for rapid screening methods using mass spectrometry (MS) that can decrease the turnaround time, cost, and limits of quantitation of existing methodologies. It is important to emphasize that appropriate sample preparation is required to perform proper sample cleanup and analyte enrichment. We are focused on using matrix-compatible SPME-based devices for direct immersion extraction of small molecules from biofluids and direct coupling to MS. In this context, matrix-compatible SPME-based devices have extraction phases comprised of high-capacity sorbent embedded in a polyacrylonitrile binder that ensures small molecules can be extracted while minimizing the co-extraction of macromolecules. This provides better performance and more sensitive analysis of a wide range of small molecules including many of those found on the 2022 Prohibited List. Futhermore, we are focused on couple SPME-based devices to MS via the microfluidic open interface (MOI) and coated blade spray (CBS) technology, as well as developing more efficient ways to separate isobaric/isomeric analytes in the gas phase before MS detection using ion mobility spectrometry (IMS). These developments are critical to decrease the detection limits and discern between permitted and prohibited substances while increasing the speed of analysis and the range of screened and quantified molecules. In this proposal, we build on this success and propose applying SPME technologies directly to MS which have been recently developed in our laboratory to further improve the speed of screening directly during sports events. In the long term, the goal of the team's research is to take advantage of ongoing advances to develop powerful new analytical technologies to assist in the ongoing fight against doping in sport, with an emphasis on lowering the detection limits to better distinguish between permitted from prohibited use, as well as improving the detection window of prohibited substances.

Code: 22A08XT

For substances produced endogenously and included in the WADA Prohibited List, its abuse is based on: 10 identification of the best biomarker of abuse to be applied at the ITP level and 2) confirmation by a procedure able to demonstrate the application of the drug or its origin. Usually, this is performed by establishing the population distribution of the biomarker in ITP and the application isotope ratio mass spectrometry (IRMS) as a confirmatory procedure. This has been applied successfully using the steroidal module of the ABP and GC-IRMS.
In addition to steroidal hormones, several other prohibited compounds may benefit from a similar approach. We intend to investigate the application of IRMS coupled to liquid chromatography to the confirmation of compounds that because of their physicochemical properties cannot be analyzed by GC and for which a definiticive confirmation procedure does not exist.
The analysis of AICAR by GC-C-IRMS has been described after silylation and its comparison with a steroid (pregnanediol) as an endogenous reference compound (ERC). The current limitations of this approach can be overcome by the use of LC-IRMS, allowing the underivatized compound analysis and the use of an ERC closer to its metabolic path.
The main 2-phenethylamine and octopamine target analytes are excreted as sulfates, whose hydrolysis is not obvious. The confirmation by GC-C-IRMS is impaired by the high interaction with GC systems. The direct analysis of their sulfated conjugates by LC-IRMS will unambiguously confirm their origin. The main objective is to prove the applicability for antidoping purposes of LC-IRMS in the analyses of intact sulfates.
For IGF-1 the main objective is the use of LC-IRMS for the analysis of recombinant preparations and preparations of human origin, to prove its applicability for anti-doping purposes. The protein will be analyzed intact or after trypsin digestion.

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