凝胶渗透色谱净化-高效液相色谱荧光法检测生肉中15种多环芳烃  

Determination of 15 kinds of polycyclic aromatic hydrocarbons in fresh meat by online gel permeation chromatography purification-high performance liquid chromatography

作　　者：王溪 阮丽萍[1] 李放[1] 陈蓓[1] 刘华良[1] WANG Xi;RUAN Li-ping;LI Fang;CHEN Bei;LIU Hua-liang(Jiangsu Provincial Center for Disease Control and Prevention,Jiangsu Nanjing 210009,China)

机构地区：[1]江苏省疾病预防控制中心

出　　处：《江苏预防医学》2019年第3期259-261,279,共4页Jiangsu Journal of Preventive Medicine

基　　金：江苏省医学重点学科-流行病学(ZDXKA2016008)

摘　　要：目的建立生肉中欧盟优控15种多环芳烃的检测方法。方法采用装有Bio-Beads S-X3填料的凝胶渗透色谱净化分离柱(300mm×20mm),收集16~43min流出组分,在线浓缩近干,1mL乙腈复溶,采用PAH C18反相键合固定相色谱柱(250mm×4.6mm,5μm)分离,水和乙腈梯度洗脱,高效液相色谱荧光检测器检测。结果15种多环芳烃在0.2~20.0ng/mL质量浓度范围内[苯并(j)荧蒽:0.5~20.0ng/mL]线性良好(r>0.998),该方法检出限为0.04~0.49μg/kg,定量限为0.12~1.51μg/kg。在生鱼肉、鸡肉、猪肉和牛肉4种基质中分别添加3个水平混合标准溶液(0.5、2.0、10.0μg/kg),平均回收率为61.0%~101.7%,相对标准偏差(RSD)为0.4%~11.5%(n=6)。结论该方法能同时检测生肉中欧盟优控的15种多环芳烃,满足定量分析要求。Objective To establish a method for determination of 15kinds of polycyclic aromatic hydrocarbons(PAHs) controlled by European Union with priority in fresh meat.Methods Separation column filled with Bio-Beads S-X3(300mm × 20mm)was used to collect fractions from 16to 43min,which was evaporated online and re-dissolved by 1mL acetonitrile solution and subjected to separation via PAH C18reversed-phase bonded stationary phase chromatography column(250mm×4.6 mm,5μm)by gradient elution of water and acetonitrile and analyzed by high performance liquid chromatography with fluorescence detector.Results The 15kinds of PAHs showed good linear relationships in the mass concentration range of 0.2- 20.0ng/mL[Benzo(j)fluoranthene:0.5-20.0ng/mL]with all correlation coefficients r>0.998.The limits of detection were 0.04-0.49μg/kg and the limits of quantitation were 0.12-1.51μg/kg.The average recoveries in fresh fish,chicken,pork and beef were 61.0%-101.7%at 3spiked levels of 0.5,2.0and 10.0μg/kg with the relative standard deviations of 0.4%- 11.5%(n=6).Conclusion The established method could be used to determine 15kinds PAHs simultaneously controlled by European Union with priority in fresh meat and satisfy quantitative requirement.

关 键 词：凝胶渗透色谱 多环芳烃 高效液相色谱 生肉 

分 类 号：R113[医药卫生—公共卫生与预防医学]