色谱

色谱 ›› 2014, Vol. 32 ›› Issue (6): 582-585.DOI: 10.3724/SP.J.1123.2014.02029

• 研究论文 • 上一篇    下一篇

液相色谱-串联质谱法测定食用植物油中的棉酚

张文华1, 黄超群1, 谢文1, 沈立2   

  1. 1. 浙江出入境检验检疫局, 浙江 杭州 310016;
    2. 上海出入境检验检疫局, 上海 200135
  • 收稿日期:2014-02-28 修回日期:2014-04-04 出版日期:2014-06-08 发布日期:2014-05-22
  • 通讯作者: 谢文
  • 基金资助:

    出入境检验检疫行业标准制（修）订项目（2012B308r）.

Determination of gossypol in edible vegetable oil with high performance liquid chromatography-tandem mass spectrometry

ZHANG Wenhua1, HUANG Chaoqun1, XIE Wen1, SHEN Li2   

  1. 1. Zhejiang Entry-Exit Inspection and Quarantine Bureau, Hangzhou 310016, China;
    2. Shanghai Entry-Exit Inspection and Quarantine Bureau, Shanghai 200135, China
  • Received:2014-02-28 Revised:2014-04-04 Online:2014-06-08 Published:2014-05-22

PDF

343

被引次数

2

摘要：

建立了食用植物油中棉酚的液相色谱-串联质谱（LC-MS/MS）分析方法。待测物经无水乙醇涡旋振荡提取，C18色谱柱分离，以乙腈和0.1%（v/v）甲酸水溶液为流动相进行梯度洗脱，LC-MS/MS测定，外标法定量。方法的测定低限（S/N>10）为1 mg/kg；在添加浓度为1、2和200 mg/kg水平下，棉酚的加标回收率为87.4%~100%，相对标准偏差为3.9%~12.2%。结果表明，本方法灵敏度高，测定结果准确，回收率稳定，可用于食用植物油中棉酚残留的确证检测。

关键词: 棉酚, 食用油, 液相色谱-串联质谱

Abstract:

A liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed for the determination of gossypol in edible vegetable oil. The sample was extracted with ethyl alcohol by vortex-excited oscillation. The extract was cleaned up by 0.22 μm filter membrane and centrifuged for 5 min at 4 000 r/min after standing in a fridge at 4 ℃ for 30 min. The compound was separated on a C18 column (100 mm×2.1 mm, 3.5 μm) with acetonitrile and 1% (v/v) formic acid aqueous solution as mobile phase. The detection of gossypol was carried out by LC-MS/MS with positive electrospray ionization under multiple reaction monitoring (MRM) mode using external standard method. The limits of quantification (S/N>10) of gossypol in edible vegetable oil was 1 mg/kg. The recoveries were from 87.4% to 100% at the spiked levels of 1, 2, 200 mg/kg of gossypol in edible vegetable oil with the relative standard deviations (RSDs) between 3.9% and 12.2%. The method, with high sensitivity, good precision and high recovery, was suitable for the confirmation and quantification of gossypol residue in edible vegetable oil.

Key words: edible oil, gossypol, liquid chromatography-tandem mass spectrometry (LC-MS/MS)

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