Supramolecular solvents for making comprehensive liquid-liquid microextraction in multiclass screening methods for drugs of abuse in urine based on liquid chromatography-high resolution mass spectrometry
Author
González Rubio, S.
Caballero-Casero, Noelia
Ballesteros-Gómez, A.
Cuervo, Darío
Muñoz, Gloria
Rubio Bravo, Soledad
Publisher
ElsevierDate
2023Subject
Screening methodsSupramolecular solvents
LC-ESI-TOF
Doping control
Urine
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Show full item recordAbstract
Multiclass screening methods involving hundreds of structurally unrelated compounds are becoming es- sential in many control labs and research areas. Accurate mass screening of a theoretically unlimited number of chemicals can be undertaken using liquid chromatography coupled to high resolution mass spectrometry (LC –HRMS), but the lack of comprehensive sample treatments hinders this unlimited po- tential. In this research, the capability of supramolecular solvents (SUPRAS) for making comprehensive liquid-liquid microextraction (LLME) in multiclass screening methods based on LC –HRMS was firstly ex- plored. For this purpose, a SUPRAS made up of 1,2-hexanediol, sodium sulphate and water was synthe- sized directly in the urine and applied to compound extraction and interference removal in the screening of eighty prohibited substances in sports by LC-electrospray ionization-time of flight mass spectrometry. Selected substances included a wide range of polarities (log P from -2.4 to 9.2) and functionalities (e.g. alcohol, amine, amide, carboxyl, ether, ester, ketone, sulfonyl, etc.). No interfering peaks were observed for any of the 80 substances investigated. Around 84–93% of drugs were efficiently extracted (recover- ies 70–120%) and 83–94% of the analytes did not show matrix effects ( ±20%) in the ten tested urines. Method detection limits for the drugs were in the interval 0.002–12.9 ng mL −1 , which are in accordance with the Minimum Required Performance Levels values established by the World Anti-Doping Agency. The applicability of the method was evaluated by the screening of thirty-six blinded and anonymized urine samples, previously analyzed by gas or liquid chromatography-triple quadrupole. Seven of the sam- ples lead to an adverse analytical finding in line with the results obtained by the conventional methods. This research proves that LLME based on SUPRAS constitutes an efficient, economic, and simple sample treatment in multiclass screening methods, an application that is unaffordable for conventional organic solvents.