凝胶渗透色谱净化-高效液相色谱法测定润滑脂中苯并(a)芘含量
HPLC Determination of Benzo［a］pyrene in Grease after Purification with Gel Permeation Chromatography
摘 要
提出了高效液相色谱法测定润滑脂中苯并(a)芘含量的方法。样品用环己烷-乙酸乙酯(1+1)混合溶剂提取,所得提取液须经凝胶色谱净化大分子干扰物质。采用高效液相色谱分离后,用荧光检测器进行测定。苯并(a)芘的质量浓度在5.00~200 μg·L-1范围内与其峰面积呈线性关系,方法检出限(3S/N)为3 μg·L-1。在3个标准加入水平下进行了回收试验,所得回收率在85.6%~97.8%之间,相对标准偏差(n=6)小于3.0%。
高效液相色谱法
苯并(a)芘
润滑脂
Gel permeation chromatography
HPLC
Benzo［a］pyrene
Grease
Abstract
A method for determination of benzo［a］pyrene (BaP) in grease by HPLC was proposed. The samples was extracted with mixed solvent of n-hexane and ethyl acetate (1+1). The extract obtained was purified to remove the macromolecular impurities by gel permeation chromatography. The eluates were taken for separation by HPLC and the content of BaP was determined by fluorescence detector. Linear relationship between values of peak area and mass concentration of BaP was kept in the range of 5.00-200 μg·L-1, with detection limits (3S/N) of 3 μg·L-1. Tests for recovery were made by addition of standard solution at 3 different concentration levels, values of recovery found were in the range of 85.6%-97.8% with RSD (n=6) less than 3.0%.
中图分类号 O657.7
所属栏目 工作简报
基金项目 “十二五”国家科技支撑计划-食品添加剂制造关键技术研究(2011BAD23B00)
收稿日期 2012/2/15
修改稿日期
网络出版日期
作者单位点击查看
备注吉桂珍(1983-),女,河北邢台人,助理工程师,主要从事食品检测研究。
引用该论文: JI Gui-zhen,GAO Wei,ZHANG Qing-qing,WANG Lei. HPLC Determination of Benzo［a］pyrene in Grease after Purification with Gel Permeation Chromatography[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2013, 49(3): 294～296
吉桂珍,高伟,张青青,王磊. 凝胶渗透色谱净化-高效液相色谱法测定润滑脂中苯并(a)芘含量[J]. 理化检验－化学分册, 2013, 49(3): 294～296
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参考文献
【1】ALOMIRAH H， AL-ZENKI S, AL-HOOTI S, et al. Concentrations and dietary exposure to polycyclic aromatic hydrocarbons (PAHs) from grilled and smoked foods［J］. Food Control, 2011,22:2028-2035.
【2】ZHU S Q, LI L, THORNTON C, et al. Simultaneous determination of benzo［a］pyrene and eight of its metabolites in Fundulus heteroclitus bile using ultra-performance liquid chromatography with mass spectrometry［J］. Journal of Chromatography B, 2008,863:141-149.
【3】BORTOLATO S A, ARANCIBIA J A, ESCANDAR G M. A novel application of nylon membranes to the luminescent determination of benzo［a］pyrene at ultra trace levels in water samples［J］. Anal Chim Acta, 2008,613:218-227.
【4】AL-HADDAD A. A selective method for the determination of benzo［a］pyrene in soil using porous graphitic carbon liquid chromatography columns［J］. Talanta, 2003,59:845-848.
【5】ZUIN V G, SCHELLIN M, MONTERO L, et al. Comparison of stir bar sorptive extraction and membrane-assisted solvent extraction as enrichment techniques for the determination of pesticide and benzo［a］pyrene residues in Brazilian sugarcane juice［J］. Journal of Chromatography A, 2006,1114:180-187.
【6】ISLAM G A, GREIBROKK T, RISEL F, et al. Epimerization of benzowaxpyrene-tetrols after acid hydrolysis, implications for determination of benzowaxpyrene adducts in protein and DNA［J］. Mutation Research, 1999,423:47-54.
【7】FENG F, YIN J F, SONG M Y, et al. Preparation, identification and analysis of stereoisomeric anti-benzo［a］pyrene diol epoxide-deoxyguanosine adducts using phenyl liquid chromatography with diode array, fluorescence and tandem mass spectrometry detection［J］. Journal of Chromatography A, 2008,1183:119-128.
【8】方杰,王凯雄.气相色谱-离子阱质谱法测定海洋贝类中多残留有机氯农药、多氯联苯和多环芳烃［J］.分析化学, 2007,35(11):1607-1613.
【9】GB/T 21911-2008食品中邻苯二甲酸酯的测定［S］.
【10】谢维平,欧阳燕玲,黄盈煜,等.凝胶渗透色谱净化-高效液相色谱法测定鱼肉中的5种激素类药物残留［J］.色谱, 2010,28(4):388-392.
【11】GB/T 5009.27-2003食品中苯并(a)芘的测定［S］.
【2】ZHU S Q, LI L, THORNTON C, et al. Simultaneous determination of benzo［a］pyrene and eight of its metabolites in Fundulus heteroclitus bile using ultra-performance liquid chromatography with mass spectrometry［J］. Journal of Chromatography B, 2008,863:141-149.
【3】BORTOLATO S A, ARANCIBIA J A, ESCANDAR G M. A novel application of nylon membranes to the luminescent determination of benzo［a］pyrene at ultra trace levels in water samples［J］. Anal Chim Acta, 2008,613:218-227.
【4】AL-HADDAD A. A selective method for the determination of benzo［a］pyrene in soil using porous graphitic carbon liquid chromatography columns［J］. Talanta, 2003,59:845-848.
【5】ZUIN V G, SCHELLIN M, MONTERO L, et al. Comparison of stir bar sorptive extraction and membrane-assisted solvent extraction as enrichment techniques for the determination of pesticide and benzo［a］pyrene residues in Brazilian sugarcane juice［J］. Journal of Chromatography A, 2006,1114:180-187.
【6】ISLAM G A, GREIBROKK T, RISEL F, et al. Epimerization of benzowaxpyrene-tetrols after acid hydrolysis, implications for determination of benzowaxpyrene adducts in protein and DNA［J］. Mutation Research, 1999,423:47-54.
【7】FENG F, YIN J F, SONG M Y, et al. Preparation, identification and analysis of stereoisomeric anti-benzo［a］pyrene diol epoxide-deoxyguanosine adducts using phenyl liquid chromatography with diode array, fluorescence and tandem mass spectrometry detection［J］. Journal of Chromatography A, 2008,1183:119-128.
【8】方杰,王凯雄.气相色谱-离子阱质谱法测定海洋贝类中多残留有机氯农药、多氯联苯和多环芳烃［J］.分析化学, 2007,35(11):1607-1613.
【9】GB/T 21911-2008食品中邻苯二甲酸酯的测定［S］.
【10】谢维平,欧阳燕玲,黄盈煜,等.凝胶渗透色谱净化-高效液相色谱法测定鱼肉中的5种激素类药物残留［J］.色谱, 2010,28(4):388-392.
【11】GB/T 5009.27-2003食品中苯并(a)芘的测定［S］.
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