Rapid and automated on-line solid phase extraction HPLC-MS/MS with peak focusing for the determination of ochratoxin
Luca Campone1, Anna Lisa Piccinelli2, Rita Celano2
1Dipartimento di Farmacia, Università degli studi di Salerno, Via Giovanni Paolo II, 84084 Fisciano, SA, Italy; Dipartimento di Agraria, Università Mediterranea di Reggio Calabria, loc. Feo di Vito, 89122 Reggio Calabria, RC, Italy.
Abstract:
This study reports a fast and automated analytical procedure based on an on-line SPE-HPLC-MS/MS method for the automatic pre-concentration, clean up and sensitive determination of OTA in wine. The amount of OTA contained in 100μL of sample (pH≅5.5) was retained and concentrated on an Oasis MAX SPE cartridge. After a washing step to remove matrix interferents, the analyte was eluted in back-flush mode and the eluent from the SPE column was diluted through a mixing Tee, using an aqueous solution before the chromatographic separation achieved on a monolithic column. The developed method has been validated according to EU regulation N. 519/2014 and applied for the analysis of 41 red and 17 white wines. The developed method features minimal sample handling, low solvent consumption, high sample throughput, low analysis cost and provides an accurate and highly selective results.
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