食品科学

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固相萃取净化-高效液相色谱法测定食品中α-细辛醚和β-细辛醚残留量

彭 芳1,雷美康1,许菲菲2,柴明青2,祝子铜1,徐倩倩1,李 东1,余 琪1   

  1. 1.衢州出入境检验检疫局,浙江 衢州 324002;2.义乌出入境检验检疫局,浙江 义乌 322000
  • 出版日期:2015-09-25 发布日期:2015-09-11
  • 基金资助:

    国家出入境检验检疫行业标准制修订项目(2009B527)

Determination of α-asarone and β-asarone Residues in Foods by Solid Phases Extraction-Liquid Chromatography

PENG Fang1, LEI Meikang1, XU Feifei2, CHAI Mingqing2, ZHU Zitong1, XU Qianqian1, LI Dong1, YU Qi1   

  1. 1. Quzhou Entry-Exit Inspection and Quarantine Bureau, Quzhou 324002, China;
    2. Yiwu Entry-Exit Inspection and Quarantine Bureau, Yiwu 322000, China
  • Online:2015-09-25 Published:2015-09-11

摘要:

建立用于测定乳粉、绿豆糕、猪肉、熏鱼肉、调味粉中白菖蒲油主要成分α-细辛醚和β-细辛醚含量的固相萃取-高效液相色谱分析方法。选择乙腈提取样品中的细辛醚,提取液经硅胶固相萃取小柱净化,采用配备荧光检测器的高效液相色谱仪进行分离测定,外标法定量。乳粉、绿豆糕、猪肉、熏鱼肉、调味粉中α-细辛醚和β-细辛醚的方法定量限均为0.01 mg/kg,在0.01~0.50 mg/kg的添加水平范围内,α-细辛醚的平均回收率在78.2%~99.4%之间,β-细辛醚的平均回收率在80.8%~105.6%之间,相对标准偏差为1.6%~10.3%。该方法能够满足食品中细辛醚的痕量检测要求。

关键词: &alpha, -细辛醚, &beta, -细辛醚, 食品, 固相萃取, 高效液相色谱法

Abstract:

A sensitive and selective method was developed for the determination of residues of α-asarone and β-asarone
as the main components of calamus oil in milk powder, mung bean cake, pork, smoked fish, and seasoning powder. The
residues of α-asarone and β-asarone in the test samples were extracted with acetonitrile. The extract was cleaned up with
a silica gel solid phase extraction column, analyzed by high performance liquid chromatography (HPLC) equipped with a
fluorescence detector, and quantified by external standard method. Milk powder, green bean cake, pork, smoked fish and
seasoning powder were chosen as the representative samples. The limit of quantification (LOQ) (RSN > 10) was 0.01 mg/kg
in all these samples. The average recoveries of α-asarone and β-asarone at three spiked levels (0.01, 0.05 and 0.50 mg/kg)
ranged from 78.2% to 99.4% and 80.8% to 105.6%, respectively, with relative standard deviations (RSDs) between 1.6%
and 10.3%. The method can meet the analytical requirements for trace asarones in foods.

Key words: α-asarone, β-asarone, food, solid phase extraction (SPE), high performance liquid chromatography (HPLC)

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