食品科学 ›› 2009, Vol. 30 ›› Issue (8 ): 272-274.doi: 0.7506/spkx1002-6630-200908062

• 分析检测 • 上一篇    下一篇

蜂王浆中氟胺氰菊酯与氟氯苯氰菊酯残留的提取净化及超高效液相色谱测定方法研究

董盛月   

  1. 北京市海淀区疾病预防控制中心
  • 收稿日期:2009-03-16 出版日期:2009-04-15 发布日期:2010-12-29
  • 通讯作者: 董盛月 E-mail:dshy2008@sina.com

Study on Extraction, Clean-up and Ultra-performance Liquid Chromatographic Analysis of Fluvalinate and Flumethrin Residues in Royal Jelly

DONG Sheng-yue   

  1. (Haidian District of Beijing Centers for Disease Prevention and Control, Beijing 100080, China)
  • Received:2009-03-16 Online:2009-04-15 Published:2010-12-29
  • Contact: DONG Sheng-yue E-mail:dshy2008@sina.com

摘要:

本实验对蜂王浆中氟胺氰菊酯与氟氯苯氰菊酯残留的提取净化及超高效液相色谱检测方法进行了研究。蜂王浆样品用水溶解后经正已烷-二氯甲烷(1:1,V/V)提取,无水乙醇破除乳化,样液经离心后,用反相固相萃取柱富集与净化,用乙腈洗脱后,氮吹至近干,用80%乙腈水溶液溶解,经0.22μm滤膜过滤后,采用超高效液相色谱梯度洗脱与紫外检测器分析蜂王浆中的氟胺氰菊酯与氟氯苯氰菊酯残留。以XTerra Shield RP18柱(2.1mm×50mm,1.7μm)为色谱柱,以水和乙腈为流动相,两种菊酯残留在4min中内实现了较好的分离,方法快速准确,灵敏度高,是一种较好的定性和定量方法。所研究的提取净化方法及色谱分离条件能有效排除蜂王浆中的杂质干扰,添加回收率在75.7%~82.8%之间,方法检出限为10μg/kg。

关键词: 蜂王浆, 氟胺氰菊酯, 氟氯苯氰菊酯, 超高效液相色谱

Abstract:

In this article, a study on extraction, clean-up and ultra-performance liquid chromatographic analysis was carried out. The samples were dissolved using water and extracted by dichloromethane / hexane (1:1,V/V). The sample emulsification was removed by absolute ethanol and was cleaned up by reverse-phase column, while the two residues were eluted off via SPE cartridge with acetonitrile and evaporate to dryness on nitrogen dry evaporator, and residues were dissolved in 80% acetonitrile (acetonitrile/water, 80:20,V/V) and passed through 0.22 μm filter for determination by a ultra-performance liquid chromatography UV detection. A XTerra Shield RP18 column(2.1mm×50mm,1.7μm)was as chromatographic separation column, water and acetonitrile were as mobile phase under gradient elution. The total analysis time was less than 4 min. The recoveries is 75.7%~82.8%. The limit of detection for the method was 10μg/kg.

Key words: royal jelly, fluvalinate, flumethrin, ultra-performance liquid chromatography

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