采用新型固相萃取柱快速测定食用植物油中苯并[a]芘  

Rapid Determination of Benzo[a]pyrene in Edible Vegetable Oil Using a New Type of Solid Phase Extraction Column

作　　者：何强 孔祥虹 李建华 赵洁[2] 张莹[1] 

机构地区：[1]陕西出入境检验检疫局检验检疫技术中心,陕西西安710068 [2]西安理工大学理学院,陕西西安710054

出　　处：《分析测试学报》2012年第6期710-714,共5页Journal of Instrumental Analysis

基　　金：陕西省农业攻关项目(2010K01-19-4);国家质检总局科研项目(2009IK285);陕西出入境检验检疫局科研项目(2010IK001)

摘　　要：研究了Bond Elut ENV新型固相萃取柱在食用植物油中苯并[a]芘快速检测中的应用,建立了快速测定食用植物油样品中苯并[a]芘残留量的固相萃取/液相色谱/荧光检测法。样品用正己烷溶解,固相萃取净化,SUPELCOSILTMLC-PAH(25 cm×4.6 mm,5μm)色谱柱分离,以乙腈-水(95∶5)为流动相,荧光检测(λex=297 nm,λem=408 nm),外标法定量。苯并[a]芘的检出限为0.3μg/kg,在1.0～50.0μg/L范围内线性关系良好,相关系数为0.999 6,方法的回收率为79%～102%,相对标准偏差不高于9.4%。该方法准确、实用、简便、快速,在食用植物油的苯并[a]芘残留量检测方面有广泛的应用前景。A new type of solid phase extraction column（ Bond Elut ENV）was used for the rapid determination of benzo[ a ] pyrene in edible vegetable oil. And a solid phase extraction purification and high performance liquid chromatography/fluorescence detection method was developed for the determination of benzo[ a ] pyrene in edible vegetable oil. Samples were dissolved in n-hexane and then purified by solid phase extraction. Chromatographic analysis was performed on a SUPELCOSILTM LC - PAH （25 cm ×4.6 ram, 5μm） column using acetonitrile - water （95 ： 5 ） as mobile phase. Quantitation analysis was carried out by the external standard method using fluorescence detecter at λex = 297 nm and λ em =408 nm. The calibration curve was linear over the benzo[ a ] pyrene concentration in the range of 1.0 - 50.0μg/L （ r = 0. 999 6 ） with detection limit of 0. 3 μg/kg. The recoveries ranged from 79% to 102% with relative standard deviations no more than 9.4%. The method is accurate, practical, simple and fast, and has an extensive application prospect in the determination of benzo[a ] pyrene residues in edible vegetable oil.

关 键 词：BOND Elut ENV固相萃取柱 食用植物油 苯并[A]芘 硅胶固相萃取柱 液相色谱/荧光检测 

分 类 号：O657.72[理学—分析化学] TQ612.1[理学—化学]