Determination of Polycyclic Aromatic Hydrocarbons in Smoked Fish and Smoked Meat by Online Solid phase Extraction and High Performance Liquid Chromatography

KeyWord:online solid phase extraction(online SPE)  polycyclic aromatic hydrocarbons(PAHs)  high performance liquid chromatography(HPLC)  smoked fish  smoked meat

Abstract:

      Based on on line purification-enrichment technology£¬a novel method was developed for the determination of 15 polycyclic aromatic hydrocarbons in smoked fish and smoked meat by online solid phase extraction and high performance liquid chromatography with ultraviolet/fluorescence detection(online-SPE/HPLC-UV/FL-D).Experimental parameters such as extraction solvent and mobile phase were optimized.The homogenized smoked samples were dissolved with acetonitrile-acetone(6¡Ã4),and then extracted ultrasonically.The online purification-enrichment was performed on a solid phase extraction ChromSpher Pi column(80 mm¡Á3 mm),and the separation was carried out on a C18 reversed phase PAH column(250 mm¡Á4ª±6 mm i.d.£¬5 ¦Ìm) using ultraviolet detection at 220 nm and fluorescence detection.Isopropyl alcohol£¬acetonitrile and water were served as mobile phases by gradient elution.The results showed that good linearities for 15 polycyclic aromatic hydrocarbons existd in corresponding concentration ranges with correlation coefficients(r2) more than 0.999.The limits of detection(LODs) were between 0.03 ¦Ìg/kg and 8.33 ¦Ìg/kg.The recoveries of 15 components at three spiked levels in smoked fish samples were in the range of 67.4%-107.2% with relative standard deviations(RSD£¬n=6) of 0.2%-7.7%.The recoveries of 15 components at three spiked levels in smoked meat samples were in the range of 71.8%-110.5% with relative standard deviations(RSD£¬n=6) of 0.8%-8.9%.Verified by FAPAS quality control samples,the types and concentration ranges of analytes could meet the requirements.