色谱

色谱

• 研究论文 • 上一篇    下一篇

固相萃取-高效液相色谱/串联质谱法测定食醋中的3种甜味剂

尹峰1*, 丁召伟1, 曹雪1, 高洁1, 姜德铭1, 匡登辉2, 顾燕平1, 何国亮1   

  1. 1. 国家副食品质量监督检验中心, 北京 100070; 2. 南开大学, 天津 300071
  • 收稿日期:2011-01-28 修回日期:2011-03-11 出版日期:2011-06-28 发布日期:2011-07-25
  • 通讯作者: 尹峰,硕士,工程师,主要从事兽药残留、食品添加剂的检验工作. Tel: (010)63722146

Determination of three sweeteners in vinegars by solid phase extraction-high performance liquid chromatography/tandem mass spectrometry

YIN Feng1*, DING Zhaowei1, CAO Xue1, GAO Jie1, JIANG Deming1, KUANG Denghui2, GU Yanping1, HE Guoliang1   

  1. 1. State Non-Staple Food Quality Supervision and Test Center, Beijing 100070, China; 2. Nankai University, Tianjin 300071, China
  • Received:2011-01-28 Revised:2011-03-11 Online:2011-06-28 Published:2011-07-25

PDF

589

被引次数

38

摘要： 建立了食醋中3种甜味剂的固相萃取-高效液相色谱/串联质谱分析方法。样品经酸性水稀释,弱阴离子固相萃取柱净化,Pursuit C18色谱柱分离,10 mmol/L醋酸铵(含0.1%氨水)和乙腈为流动相梯度洗脱,电喷雾负离子模式下多反应监测(MRM)模式检测。糖精钠、安赛蜜、甜蜜素的定量限分别为10、5、5 μg/kg,回收率为72.1%～96.8%,相对标准偏差小于15%。该方法准确、灵敏度高,可用于食醋中甜味剂的定性定量检验。

关键词: 高效液相色谱-串联质谱, 固相萃取, 食醋, 甜味剂

Abstract: A solid phase extraction-high performance liquid chromatography/electrospray ionization-tandem mass spectrometry (SPE-HPLC/ESI-MS/MS) method for the determination of 3 sweeteners (acesulfame (AK), sodium saccharin (SA), sodium cyclamate (SC)) in vinegars has been developed. The sample was diluted with acidic water, then purified and enriched with a weak anion exchange SPE column. The HPLC separation was performed on a Pursuit C18 column (150 mm×2.0 mm, 3 μm) by gradient elution with 10 mmol/L ammonium acetate containing 0.1%(v/v) ammonia water and acetonitrile as the mobile phases. The analytes were detected by ESI~-MS/MS in multiple reaction monitoring (MRM) mode to satisfy qualitative and quantitative detections. Good linearities (r2＞0.99) were obtained over the range of 0.01~0.50 mg/L. The limits of quantification (LOQs) for SA, AK and SC were 10, 5 and 5 μg/kg, respectively. The average recoveries ranged from 72.1% to 96.8% at the spiked levels of 0.01 and 0.1 mg/L with the relative standard deviations (RSDs) less than 15%. This method is accurate, highly sensitive for qualitative and quantitative analysis of the 3 sweeteners in vinegars.

Key words: high performance liquid chromatography/tandem mass spectrometry (HPLC/MS/MS), sweeteners, vinegars, solid phase extraction