GC Analysis of Phthalate Esters in Extra Virgin Olive Oil (Spiked) on SLB®-5ms after SPME using 100 μm PDMS Fiber

Materials
accessory
related product
used together
SPME Fiber Assembly
100 μm PDMS, Fused Silica (1 cm), needle size 24 ga, Manual Holder, pk of 3, red hubCONDITIONS
sample/matrix
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 fiber
SPME Assembly, 100μm PDMS FS, 24 GA Manual (57300-U)
extraction
direct-immersion, 20 min, constant stirring at 500 rpm
desorption process
280 °C for 5 min, splitless
column
SLB-5ms, 10 m x 0.10 mm I.D., 0.10 μm (28465-U)
oven
90 °C (5 min), 30 °C/min to 310 °C, 50 °C/min to 350 °C (3 min)
inj. temp.
280 °C
detector
MS (triple quadrupole), ion source: 220 °C; ionization mode: EI (70 eV); acquisition mode: MRM
MSD interface
280 °C
carrier gas
helium, 50 cm/sec
Description
Analysis Note
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.
Legal Information
SLB is a registered trademark of Merck KGaA, Darmstadt, Germany