Simultaneous determination of six resorcylic acid lactones in feed using liquid chromatography–tandem mass spectrometry and multi-walled carbon nanotubes as a dispersive solid phase extraction sorbent

• A simple method was developed for six resorcylic acid lactones using dSPE with MWCNTs.
• The pH, extraction time, type and amount of MWCNTs were optimised.
• The proposed method was validated according to 2002/657/EC.
• The whole method was fast, reliable, convenient and sensitive.

A simple and cost-effective pre-treatment procedure was developed for six resorcylic acid lactones (RALs) in feed using dispersive solid phase extraction (dSPE) with multi-walled carbon nanotubes (MWCNTs). The sample was analysed after purification by ultra-high performance liquid chromatography–negative electrospray ionisation tandem mass spectrometry (UHPLC–ESI-MS/MS). After extraction with acetonitrile/water (80:20, v/v) and dilution with water, a dSPE procedure was carried out with MWCNTs. The pH value of the extract, the extraction time for MWCNTs, the type and amount of MWCNTs and the type of eluent were optimised to increase the sample throughput and the sensitivity. The samples were quantified using the internal standard zearalenone-D6. The absolute recoveries of the target compounds from feed samples were most efficient when using 100 mg of MWCNTs with an outer diameter of less than 8 nm and a length of 10–30 μm, and ethyl acetate was shown to be the most suitable solvent for desorbing the target compounds from the MWCNTs. The mean recoveries from fortified swine mixed feed samples ranged from 95.3% to 107.2% and had relative standard deviations lower than 10%; the limits of detection and quantification for RALs were in the ranges of 0.20–0.29 μg/kg and 0.54–0.78 μg/kg, respectively.