色谱 ›› 2016, Vol. 34 ›› Issue (7): 703-707.DOI: 10.3724/SP.J.1123.2016.03011

• 特别策划:出入境检验检疫系统专栏(2016) • 上一篇    下一篇

全自动固相萃取-高效液相色谱-串联质谱法测定食糖中的雌二醇

曾三妹, 徐敦明, 魏一婷, 钟莉萍   

  1. 厦门出入境检验检疫局检验检疫技术中心, 福建 厦门 361026
  • 收稿日期:2016-03-08 出版日期:2016-07-08 发布日期:2013-02-05
  • 通讯作者: 徐敦明
  • 基金资助:

    福建省自然科学基金项目(2014j01057).

Determination of estradiol in table sugar by auto-solid-phase extraction-high performance liquid chromatography-tandem mass spectrometry

ZENG Sanmei, XU Dunming, WEI Yiting, ZHONG Liping   

  1. Technical Center of Xiamen Entry-Exit Inspection and Quarantine Bureau, Xiamen 361026, China
  • Received:2016-03-08 Online:2016-07-08 Published:2013-02-05
  • Supported by:

    Natural Science Foundation of Fujian Province (No. 2014j01057).

摘要:

建立了全自动固相萃取-高效液相色谱-串联质谱检测食糖中雌二醇含量的方法。食糖样品经水溶解后,用碱化乙腈提取,经HLB固相萃取柱净化,采用高效液相色谱-串联质谱分析,内标法定量。质谱分析采用电喷雾电离(ESI)负离子扫描,多反应监测(MRM)模式。雌二醇定量离子对为271.1/144.8和271.1/183.2,内标D2-雌二醇定量离子对为273.2/147.0。实验表明,经SPE柱净化后基质效应明显降低,样品中添加0.5~10 μg/kg的雌二醇,其回收率为83.9%~95.1%,相对标准偏差(n=6)小于10%。雌二醇的检出限为0.1 μg/kg,定量限为0.5 μg/kg。该方法提取效果好,具有良好的灵敏度、回收率和重复性。

关键词: 雌二醇, 高效液相色谱-串联质谱, 全自动固相萃取, 食糖

Abstract:

A high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method was established for the determination of estradiol in table sugar. Sugar samples were dissolved in water, and extracted by alkaline acetonitrile, then cleaned-up using an HLB column. The resulting samples were detected under negative multiple reactions monitoring (MRM) mode, and quantified by the internal standard method. As the results showed, the matrix effects were depressed obviously after the purification. The limit of determination and the limit of quantification of the method were 0.1 μg/kg and 0.5 μg/kg, respectively. For all the tested samples, the average spiked recoveries ranged from 83.9% to 95.1%, and the relative standard deviations (RSDs, n=6) were lower than 10%. The method is quick, easy, effective, sensitive and accurate, and can meet the requirements of the determination of estradiol in table sugar.

Key words: auto-solid-phase extraction (auto-SPE), estradiol, high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS), table sugar

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