Scientific Publications by FDA Staff

Chemosphere 2020 Oct;256:127023

New approach for removing co-extracted lipids before mass spectrometry measurement of persistent of organic pollutants (POPs) in foods.

Hayward DG, Traag W

Persistent organic pollutants (POPs) methods for foods and animal feeds require sufficient sample intake followed by an extensive removal of interfering matrix components and concentration before a gas chromatographic mass spectrometry (GC-MS) method can be applied. The extraction dissolves associated lipids in animal foods or feeds. Methods must eliminate all co-extracted lipids before determination by GC-MS. A new approach for removing lipids is presented using basic silica gel or metal ion immobilized silica gel (Ag+) in a single step. Absorbent order, adsorbent amounts, and flow rates were found to be essential for consistent results. KOH/silica gel or Ag(+) ion (AgNO(3)) silica gel were both shown to retain 75-85% of the co-extracted lipids without using sulfuric acid. KOH/silica gel method applied to butter fortified at 7.3 pg TEQ/g lipid with polychlorinated dibenzo-p-dioxins/dibenzofurans (PCDD/Fs) produced accurate results for all fortified congeners with 20% of predicted (n = 6). Ag(+) silica gel incorporated into the Miura GO-EHT automated system produced similar results fortified at 3 pg TEQ/g lipid. During PCDD/F fortifications of butter with PCDD/Fs (n = 6), labeled standard recoveries for PCDD/Fs and planar polychlorinated biphenyls (PCBs) were all acceptable (52-99%) averaging 77% using the Miura system. A reduction in the amounts of sulfuric acid silica gel needed was possible in the completion of co-extractant removal. PCDD/F spikes into butter and for a spiked sunflower oil (PCDD/Fs and coplanar PCBs) were within ± 20% of the predicted using the Miura system; suitable for current methods criteria for foods including criteria in EU legislation.