0.5 g extra virgin olive weighed into a 10 mL glass centrifuge tube, spiked with phthalate esters at 2 mg/kg, 3 mL acetonitrile added (vortexed 30 sec, centrifuged 10 min at 3000 rpm, 1.5 mL acetonitrile from the top transferred to a 2 mL vial)
SPME Assembly, 100μm PDMS FS, 24 GA Manual (57300-U)
direct-immersion, 20 min, constant stirring at 500 rpm
280 °C for 5 min, splitless
SLB-5ms, 10 m x 0.10 mm I.D., 0.10 μm (28465-U)
90 °C (5 min), 30 °C/min to 310 °C, 50 °C/min to 350 °C (3 min)
280 °C
MS (triple quadrupole), ion source: 220 °C; ionization mode: EI (70 eV); acquisition mode: MRM
280 °C
helium, 50 cm/sec
Data provided by Giorgia Purcaro (1), Laura Barp (2), and Luigi Mondello (1,2) of (1) Chromaleont s.r.l., c/o “Scienze del Farmaco e Prodotti per la Salute” Department, University of Messina, viale Annunziata, 98168 Messina, Italy or (2) “Scienze del Farmaco e Prodotti per la Salute” Department, University of Messina, viale Annunziata, 98168 Messina, Italy.
This method uses SPME with minimal sample manipulation and permits robust, fast, and accurate GC-triple quadrupole MS (QqQ) determination of phthalate esters in olive oil after their separation on an SLB-5ms column.
SLB is a registered trademark of Merck KGaA, Darmstadt, Germany