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超高效液相色谱-串联质谱测定面制品中的呋喃西林代谢物

钟海娟 梁炽琼 王建伟 吴正双

现代食品科技2013,Vol.29Issue(2):416-421,6.
现代食品科技2013,Vol.29Issue(2):416-421,6.

超高效液相色谱-串联质谱测定面制品中的呋喃西林代谢物

Determination of Semicarbazide in Flour Products by Ultra Performance Liquid Chromatography-tandem Mass Spectrometry

钟海娟 1梁炽琼 1王建伟 1吴正双1

作者信息

  • 1. 佛山市质量计量监督检测中心,广东佛山528225
  • 折叠

摘要

Abstract

A method was developed for the determination of semicarbazide in flour products based on solid phase extraction-ultra performance liquid chromatography-tandem mass spectrometry (SPE-UPLC-MS/MS ) in the article. The samples were homogenized with 0.2mol/L HC1, derivatized with 2-notrobenzaldehyde, and the derivative was extracted with ethyl acetate. The extract was cleaned up by a solid phase extraction cartridge. The target analytes were separated on a UPLC BEH C18 column with gradient elution using acetonitrile and water containing 0.1% (V/V) formic acid as mobile phase. The identification and quantification were achieved by using ESI-MS/MS in positive ion mode and with multiple reactions monitoring (MRM). The linear range was from 1 to 100 μg /kg with the correlation coefficient r=0.9993 for semicarbazide. The limit of detection (LOD) was 0.4 μg/kg. The recoveries of the method were ranged from 85.8% to 112.6% at the spiked levels of 2, 10, 50μg /kg and the relative standard deviation was less than 9%. The method was suitable for the qualitative and quantitative of semicarbazide in different flour products.

关键词

超高效液相色谱-串联质谱/固相萃取/氨基脲/面制品

Key words

ultra performance liquid chromatography-tandem mass spectrometry/ solid-phase extract/ semicarbazide/ flour products

引用本文复制引用

钟海娟,梁炽琼,王建伟,吴正双..超高效液相色谱-串联质谱测定面制品中的呋喃西林代谢物[J].现代食品科技,2013,29(2):416-421,6.

基金项目

广东省质量技术监督局科技项目(2010ZB02) (2010ZB02)

现代食品科技

OA北大核心CSTPCD

1673-9078

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