Determination of Persistent Organic Pollutants (POPs) in Aquatic Products by Accelerated Solvent Extraction/Gel Permeation Chromatography/Gas Chromatography-tandem Mass Spectrometry
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Abstract:
An improved method based on accelerated solvent extraction/gel chromatography purification/gas chromatography-triple- quadrupole mass spectrometry was set up to detect 46 POPs in aquatic products. The aquatic products were freeze-dried at -105 ℃ and 100 mbar and then uniformly mixed with diatomaceous earth. The accelerated solvent extraction and gel chromatography purification were used to remove grease. The quantitation and qualification analysis of 16 kinds of polycyclic aromatic hydrocarbons and 30 kinds of organochlorines were performed by gas chromatography-triple-quadrupole mass spectrometry (GCMS/MS) in the multiple reaction monitoring (MRM) mode, using Naphthalene-d, Acenaphthene-d, Anthracene-d, Chrysene-d as internal standards. 46 organic contaminants were extracted with dichloromethane:hexane (1:1, V/V) at 100 ℃ and 1500 psi, and their distillate (7.5~16 min) was collected. The separation of 46 POPs was good, and the correlation coefficient R2 was above 0.99. The recoveries of low (10 μg/kg), medium (50 μg/kg) and high (100 μg/kg) levels were between 81.0% and 121.0%, the relative standard deviations (RSD, n=6) were between 4.1% and 11.0%, and the detection limit was 0.0185 μg/kg~0.7377 μg/kg (dry weight). This method, with accelerated solvent extraction and gel chromatography purification as pretreatments, has good stability, low detection limit, and a high recovery rate. It is a promising method for analyzing trace POPs in aquatic products.
