Florisil固相萃取-HPLC-FLD法测定烤肉中15种多环芳烃

Determination of 15 Kinds of Polycyclic Aromatic Hydrocarbons in Barbecue by Florisil SPE-HPLC-FLD

建立一种Florisil固相萃取-HPLC-FLD法同时测定烤肉中15种多环芳烃(PAHs)的方法。样品经超声提取,Florisil固相萃取柱净化,通过高效液相色谱分离,外标法定量。结果表明, 15种PAHs的质量浓度在1~50 ng/mL范围内与色谱峰面积呈良好线性关系,线性相关系数(r)大于0.999 5;在5, 10和20μg/kg的加标水平下,平均回收率分别为73.1%~87.5%, 78.2%~93.3%和85.3~97.5%,相对标准偏差为2.0%~5.0%, 1.8%~5.0%和1.1%~3.1%;检出限(S/N=3)与定量限(S/N=10)分别为0.33~3.3μg/kg和1.0~10μg/kg。

A method for simultaneous determination of 15 kinds of polycyclic aromatic hydrocarbons(PAHs)in barbecue by Florisil SPE-HPLC-FLD was developed.The sample was extracted by ultrasonic extraction,purified by Florisil SPE,separated by HPLC,and quantified by external standard method.The results showed that the concentration of 15 kinds of PAHs was linear with chromatographic peak area in the range of 1-50 ng/mL.The linear correlation coefficients(r)were more than 0.999 5.At the spiking level of 5,10 and 20μg/kg,the average recovery was from 73.1%to 87.5%,from 78.2%to 93.3%and from 85.3%to 97.5%,and the relative standard deviation was from 2.0%to 5.0%,from 1.8%to 5.0%and from 1.1%to3.1%.The detection limits(S/N=3)were from 0.33 to 3.3μg/kg and the quantitative limits(S/N=10)were from 1.0 to 10μg/kg.