Simultaneous determination of pharmaceuticals and metabolites in fish tissue by QuEChERS extraction and UHPLC Q/Orbitrap MS analysis

• Published in: Analytical and bioanalytical chemistry 2021-11, Vol.413 (28), p.7129-7140
• Main Authors: Kalogeropoulou, Aggeliki G., Kosma, Christina I., Albanis, Triantafyllos A.
• Format: Article
• Language: English
• Subjects: Analytical Chemistry; Animal tissues; Animals; Antibiotics; Aquaculture; Aquatic organisms; Biochemistry; Bream; Characterization and Evaluation of Materials; Chemistry; Chemistry and Materials Science; Chromatography, High Pressure Liquid - methods; Drugs; Fishes; Food Science; Health risks; High performance liquid chromatography; Identification and classification; Laboratory Medicine; Liquid chromatography; Mass spectrometry; Mass Spectrometry - methods; Mass spectroscopy; Metabolites; Methods; Monitoring/Environmental Analysis; Optimization; Pharmaceutical Preparations - metabolism; Reproducibility of Results; Research Paper; Salts; Sea Bream - metabolism; Separation (Technology); Sorbents; Trimethoprim
• ISSN: 1618-2642; 1618-2650
• DOI: 10.1007/s00216-021-03684-y

In recent years, the occurrence, fate, and adverse effects of pharmaceutically active compounds (PhACs) in aquatic organisms have become a noteworthy issue. In the present study, a rapid and sensitive multiresidue analytical method was developed for the determination of 18 parent PhACs and 5 metabolites in sea bream ( Sparus aurata ), by combining a modified QuEChERS (quick, easy, cheap, effective, rugged and safe) procedure with ultra-high performance liquid chromatography-Orbitrap-mass spectrometry (UHPLC-Orbitrap-MS). The method development involved optimization of extraction solvent, extraction salts, clean-up sorbents, and amount of sample evaluation, while identification on Orbitrap MS was based on accurate mass and further confirmation with MS/MS fragmentation. The developed method was validated, and linearity was higher than 0.99. Recoveries in all cases ranged between 62 and 107% (at 10, 50, and 100 ng g −1 ), while intra-day and inter-day precision, expressed as relative standard deviation, RSD, was lower than 4% and 7%, respectively. In addition, limits of quantification (LOQs) ranged between 0.5 and 19 ng g −1 . The compounds presented a low matrix effect, between − 13 and 4%, while the expanded uncertainty U % estimated at the three spiking levels 10, 50, and 100 ng g −1 was found below 49% in all cases. Finally, the validated method was applied to sea bream samples from an aquaculture farm located in the Mediterranean Sea, with one positive finding for the antibiotic trimethoprim at a concentration of 26 ng g −1 , presenting negligible human health risk. Graphical abstract