SFE Plus C18 Lipid Cleanup Method for Selective Extraction and GC/MS Quantitation of Polycyclic Aromatic Hydrocarbons in Biological Tissues

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Abstract
Lipid material represents a potential interference for determination of nonpolar compounds (e.g., polycyclic aromatic hydrocarbons) in biological tissue samples. This study reports the development of a selective extraction method using supercritical CO2 that allows the GC/MS quantitation of PAHs in the presence of a substantial lipid background. Selective extraction of PAHs relies upon addition of C18 adsorbent beads to the initial sample slurry. The dried mixture, including C18 adsorbent, is placed in the supercritical fluid extraction (SFE) chamber. During the SFE process, lipids are preferentially retained on the C18 beads. This “SFE plus C18” procedure was developed by first optimizing SFE conditions (100 °C, 350 bar) for recovery of PAH standards. PAHs containing added model lipid compounds (stearic acid and cholesterol) were then subjected to SFE plus C18 treatment followed by GC/MS analysis. Using this approach, a recovery of 94−100% of PAHs was obtained while only 9−17% of the lipid material present was coextracted from the same test sample. The developed method is demonstrated to permit efficient recovery and detection of PAHs spiked into crab tissue, a matrix with a high lipid content.

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