高效液相色谱法测定蔬菜和水果中15种欧盟优控多环芳烃

Determination of 15 European Priority Controlled Polycyclic Aromatic Hydrocarbons in Vegetables and Fruits by High Performance Liquid Chromatography

采用高效液相色谱-荧光检测技术,建立蔬菜和水果中15种欧盟优控多环芳烃(European priority controlled polycyclic aromatic hydrocarbons ,EU-PAHs)的同时测定方法。利用超声波辅助乙腈提取蔬菜和水果中的15种欧盟优控多环芳烃,加入N-丙基乙二胺(primary secondary amine,PSA)和无水MgSO4净化,经0.22 μm滤膜过滤,用Waters PAH色谱柱分离,柱温35 ℃,用乙腈-水作流动相梯度洗脱,流速为1.2 mL/min,采用荧光检测器测定15种欧盟优控多环芳烃的含量;进样体积为20 μL。按照选定的色谱条件,15种EU-PAHs在50 min内达到基线分离,方法的精密度为4.2 %~12.0 %,方法回收率83.6 %~97.2 %。15种EU-PAHs的线性范围为0.2 μg/kg^8.0 μg/kg,相关系数均大于0.999以上。

A method for the simultaneous determination of 15 European priority controlled polycyclic aromatic hydrocarbons (EU-PAHs) in vegetables and fruits by high performance liquid chromatography with fluorescence detector was developed. Ultrasound assisted acetonitrile extraction of EU-PAHs from vegetables and fruits samples, purified by primary secondary amine(PSA) and MgSO4,filtered with 0.22 μm millipore filter.A total of 15 EU-PAHs were chromatographically separated on a PAH column,the column temperature was 35 ℃,and gradiently eluted by the mobile phase composed of acetonitrile and aqueous solution. The flow rate was 1.2 mL/min.15 European priority controlled polycyclic aromatic hydrocarbons was detected by fluorescence detector.The injection volume was 20 μL.After optimization of chromatographic conditions, 15 kinds of EU-PAHs achieved baseline separation within 50 min. The precision of the method was 4.2 %-12.0 %, and the method recovery rate was 83.6 %-97.2 %. The linear range of the other 15 kinds of EU-PAHs was 0.2 μg/kg-8.0 μg/kg. The correlation coefficients were all greater than 0.999.