食品科学

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液相色谱-四极杆-飞行时间质谱法筛查食品中6 种人工合成甜味剂

王建华1,杨 君2,刘 琳1,颜冬云2,李 立3,刘靖靖1   

  1. 1.山东出入境检验检疫局检验检疫技术中心,山东 青岛 266002;2.青岛大学化学科学与工程学院
    (环境科学与工程学院),山东 青岛 266071;3.中国检验检疫科学研究院,北京 100123
  • 出版日期:2014-04-25 发布日期:2014-05-13
  • 基金资助:

    质检公益性行业科研专项(2012424012-2)

Analysis of 6 Synthetic Sweeteners in Foods by Liquid Chromatography-Quadrupole-Time-of-Flight Mass Spectrometry

WANG Jian-hua1, YANG Jun2, LIU Lin1, YAN Dong-yun2, LI Li3, LIU Jing-jing1   

  1. 1. Technical Center of Inspection and Quarantine, Shandong Entry-Exit Inspection Quarantine Bureau, Qingdao 266002, China;
    2. College of Chemical Engineering, Qingdao University, Qingdao 266071, China;
    3. Chinese Academy of Inspection and Quarantine, Beijing 100123, China
  • Online:2014-04-25 Published:2014-05-13

摘要:

应用高效液相色谱-四极杆-飞行时间质谱建立固体样品中甜味剂的筛查。样品经前处理后采用Eclispe XDB-C18色谱柱,以0.1%甲酸-10 mmol/L甲酸铵溶液-甲醇为流动相,梯度洗脱,电喷雾负离子模式分析检测。在 全扫描采集模式下,以准分子离子峰的峰面积定量,以化合物精确分子质量定性。各化合物在0.02~2.0 mg/L范围 内均呈现良好的线性关系,相关系数均大于0.998。样品平均添加回收率为74.5%~120.1%,相对标准偏差均小于 10.4%。本方法可满足现行法规的限量要求。

关键词: 液相色谱-四极杆飞行时间串联质谱, 人工合成甜味剂, 筛查, 食品

Abstract:

A new method was established for the determination of 6 synthetic sweeteners (sodium saccharin, cyclamate,
acesulfame-K, aspartame, neotame, and sucralose) in food samples by using liquid chromatography-quadrupole-time
of flight mass spectrometry (LC-Q-TOF-MS). The extract was measured directly by LC-Q-TOF-MS with electrospray
ionization in the negative mode. The compounds were separated by an Eclispe XDB-C18 column with acetonitril-10 mmol/L
ammonium formate-0.1% formic acid as the mobile phase. A detailed fragmentation study for these 6 synthentic sweeteners
was carried out by time-of-flight. The 6 compounds behaved linearly in the concentration range of 0.02–2.0 mg/L, with a
correlation coefficient > 0.998. The recoveries were 74.5%–120.1%, with relative standard deviation below 10.4%. The
method illustrated is suitable for routine qualitative and quantitative analyses of synthetic sweeteners in food samples.

Key words: liquid chromatography quadrupole-time of flight mass spectrometry, artificial sweeteners, screening, food

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