Determination of Polycyclic Aromatic Hydrocarbons in Smoked Fish and Smoked Meat by Online Solid phase Extraction and High Performance Liquid Chromatography
Determination of Polycyclic Aromatic Hydrocarbons in Smoked Fish and Smoked Meat by Online Solid phase Extraction and High Performance Liquid Chromatography[J]. 2016,35(7):805-810.
Determination of Polycyclic Aromatic Hydrocarbons in Smoked Fish and Smoked Meat by Online Solid phase Extraction and High Performance Liquid Chromatography[J]. 2016,35(7):805-810.DOI:
基于在线净化富集技术,建立了熏烤鱼和熏烤肉制品中15种欧盟优控多环芳烃的在线固相萃取/高效液相色谱-紫外/荧光(Online-SPE/HPLC-UV/FLD)检测方法。对提取溶剂和流动相进行优化,样品采用乙腈-丙酮(6∶4)匀浆处理,超声提取后,在线固相萃取柱ChromSpher Pi(80 mm×3 mm)净化富集,反相C18 PAH专用柱(250 mm×4.6 mm i.d.,5 μm)分离,水、乙腈和异丙醇梯度洗脱,紫外和荧光检测器检测。结果表明,15种多环芳烃在相应的浓度范围内线性良好(r2>0.999);检出限为0.03~8.33 μg/kg;熏烤鱼的回收率为67.4%~107.2%,相对标准偏差(RSD)为0.2%~7.7%;熏烤肉的回收率为71.8%~110.5%,RSD为0.8%~8.9%。经FAPAS质控样品验证,所测化合物种类和浓度范围均满足要求。
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∶4),and then extracted ultrasonically.The online purification-enrichment was performed on a solid phase extraction ChromSpher Pi column(80 mm×3 mm),and the separation was carried out on a C18 reversed phase PAH column(250 mm×46 mm i.d.,5 μm) 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 μg/kg and 8.33 μg/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.