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采用新型固相萃取柱快速测定食用植物油中苯并[a]芘
引用本文:何强,孔祥虹,李建华,赵洁,张莹.采用新型固相萃取柱快速测定食用植物油中苯并[a]芘[J].分析测试学报,2012,31(6):710-714.
作者姓名:何强  孔祥虹  李建华  赵洁  张莹
作者单位:1.陕西出入境检验检疫局检验检疫技术中心;2.西安理工大学理学院
基金项目: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。

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

Rapid Determination of Benzo[a]pyrene in Edible Vegetable Oil Using a New Type of Solid Phase Extraction Column
HE Qiang,KONG Xiang-hong,LI Jian-hua,ZHAO Jie,ZHANG Ying.Rapid Determination of Benzo[a]pyrene in Edible Vegetable Oil Using a New Type of Solid Phase Extraction Column[J].Journal of Instrumental Analysis,2012,31(6):710-714.
Authors:HE Qiang  KONG Xiang-hong  LI Jian-hua  ZHAO Jie  ZHANG Ying
Institution:1(1.Inspection and Quarantine Technology Centre,Shaanxi Entry-Exit Inspection and Quarantine Bureau,Xi′an 710068,China;2.College of Science,Xi′an University of Technology,Xi′an 710054,China)
Abstract:A new type of solid phase extraction column(Bond Elut ENV)was used for the rapid determination of benzoa]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 benzoa]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 mm,5 μm) 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 λem=408 nm.The calibration curve was linear over the benzoa]pyrene concentration in the range of 1.0-50.0 μg/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 benzoa]pyrene residues in edible vegetable oil.
Keywords:Bond Elut ENV solid phase extraction column  edible vegetable oil  benzo[a]pyrene  silica gel solid phase extraction column  liquid chromatography with fluorescence detection
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