高效液相色谱荧光检测法快速测定天然生育酚中痕量苯并[a]芘
Rapid Determination of Traces of Benzo[a]pyrene in Natural Tocopherols by High-Performance Liquid Chromatography with Fluorescence Detection
摘 要
建立了一种快速、新颖的高效液相色谱荧光检测法测定天然生育酚中痕量苯并[a]芘.天然生育酚样品经中性氧化铝柱色谱富集和净化后在XDB-C18反相柱上,采用水-乙腈(体积比20比80)为流动相进行分离,采用荧光检测器进行检测,其激发波长为260 nm,发射波长为408 nm.苯并[a]芘的定量下限为0.50 ng·g-1.加标回收率大于77.9%.分析了3个不同试样,测定结果的相对标准偏差在3.0%~10.6%之间.
天然生育酚
氧化铝柱色谱
高效液相色谱
Benzo[a]pyrene
Natural tocopherol
Alumina column chromatography
HPLC
Abstract
A rapid and novel method was developed for the determination of trace amounts of benzo[a]pyrene in natural tocopherol (TP) products by reversed-phase high-performance liquid chromatography (HPLC) with fluorescence detection. Benzo[a]pyrene was enriched and purified on neutral alumina column,and separated on XDB-C18 column using acetonitrile-water (20+80) as mobile phase. The excitation wavelength is 260 nm,and emission wavelength is 408 nm. The limit of quantification of benzo[a]pyrene was 0.50 ng·g-1.The recoveries found by standard addition were greater than 77.9%. The method was applied to determination benzo[a]pyrene in three different kinds of natural tocopherol products,giving values of RSD′s (n=5) between 3.0% to 10.6%.
中图分类号 O657.37
所属栏目 试验与研究
基金项目
收稿日期 2007/6/4
修改稿日期
网络出版日期
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备注董新艳(1976-),女,河北衡水人,讲师,硕士,主要从事天然产物分离及分析研究工作.
引用该论文: DONG Xin-yan,YANG Yi-wen. Rapid Determination of Traces of Benzo[a]pyrene in Natural Tocopherols by High-Performance Liquid Chromatography with Fluorescence Detection[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2008, 44(1): 5～7
董新艳,杨亦文. 高效液相色谱荧光检测法快速测定天然生育酚中痕量苯并[a]芘[J]. 理化检验－化学分册, 2008, 44(1): 5～7
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参考文献
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【2】Vazque-Troche S,García -Falcoón M S,González-Amigo S,et al. Enrichment of benzo[a]pyrene in vegetable oils and determination by HPLC-FL[J]. Talanta,2000,51(6):1069-1076．
【3】Barranco A,Alonso-Salces R M,Berrueta L A,et al. Comparison of two sample clean-up methodologies for the determination of polycyclic aromatic hydrocarbons in edible oils[J]. Journal of Separation Science,2003,26(17):1554-1562．
【4】Moret S,Conte L S. Off-line LC-LC determination of PAHs in edible oils and lipidic extracts[J]. Journal of the High Resolution Chromatography,1998,21(44):253-257．
【5】Moret S,Dudine A,Conte L S. Processing effects on the polyaromatic hydrocarbon content of grapeseed oil[J]. Journal of the American Oil Chemists Society,2000,77(12):1289-1292．
【6】Barranco A,Alonso-Salces R M,Bakkali A,et al. Solid-phase clean-up in the liquid chromatographic determination of polycyclic aromatic hydrocarbons in edible oil[J]. Journal of Chromatography A,2003,988(1):33-40．(下转第11页)
【7】Bogusz M J,El-Hajj S A,Ehaideb Z,et al. Rapid determination of Benzo(a)pyrene in olive oil samples with solid-phase extraction and low-pressure,wide-bore gas chromatography-mass spectrometry and fast liquid chromatography with fluorescence detection[J]. Journal of Chromatography A,2004,1026(1):1-7．
【8】虎,盛良全,刘少民,等.卷烟主流烟气中多环芳烃的提取、纯化及检测方法综述[J].烟草科技,2003,4:25-28．
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