在线固相萃取/高效液相色谱法检测熏烤鱼及熏烤肉制品中的多环芳烃

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

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Chrom Spher Pi（80 mm×3 mm）净化富集,反相C18PAH专用柱（250 mm×4.6 mm i.d.,5μm）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0.03～8.33μg/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。

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 detec- tion（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 - ac- etone（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 Cls reversed-phase PAH column（250 mm ×4. 6 mm i. d. , 5 μm） using ultraviolet detection at 220 nm and fluorescence detection. Isopropyl alcohol, acetonitrile and water were served as mo- bile phases by gradient elution. The results showed that good linearities for 15 polycyclic aromatic hy- drocarbons 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.