Vibrational extraction QuEChERS for analysis of antiparasitic agents in fish by liquid chromatography coupled with tandem mass spectrometry
A method was developed for the analysis of 22 antiparasitic residues belonging to the benzoylurea, organophosphate, pyrimidinamine, pyrethrin and pyrethroid classes in salmon by liquid chromatography coupled with tandem mass spectrometry. Samples were extracted with acetonitrile–water as the extraction solvent with use of a vibrational shaking apparatus with a ceramic homogenizer. After extraction, the acetonitrile extracts were cleaned up by incubation at low temperature (-20 °C, 1 h) to remove fat, followed by dispersive solid-phase extraction using Z-Sep+ and primary–secondary amine as sorbents. Validation was performed following the 2002/657/EC and SANTE/11813/2017 guidelines. The trueness of the method ranged from 87% to 121% and precision ranged from 4.1% to 23.7%, with the exception of cyphenothrin, dicyclanil and azamethiphos. The method developed is particularly advantageous because the use of a vibrational shaker allows unattended extraction of samples and eliminates a laborious tissue disruption step, which increases sample throughput in the laboratory. The sample preparation and chromatographic separations can be performed in 5 and 4 h, respectively, for 36 samples.
KeywordsAntiparasitic drug residues Fish Liquid chromatography–tandem mass spectrometry Dispersive solid-phase extraction Vibrational extraction
This research was funded by the CAPES PDSE scholarship programme (grant no. 88881.134557/2016-01). All the instrumentation and facilities were funded by Teagasc Food Research Centre (Ireland).
Compliance with ethical standards
Conflict of interest
The authors declare that they have no competing interests.
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