色谱

色谱 ›› 2018, Vol. 36 ›› Issue (4): 351-355.DOI: 10.3724/SP.J.1123.2017.10023

• 研究论文 • 上一篇    下一篇

亲水相互作用色谱-串联质谱法测定液体食品中14种甜味剂

范广宇1,2, 冯峰1, 张峰1, 高飞1, 李晓明3, 梁振纲4   

  1. 1. 中国检验检疫科学研究院食品安全研究所, 北京 100176;
    2. 连云港出入境检验检疫局, 江苏 连云港 222042;
    3. 济南出入境检验检疫局, 山东 济南 250014;
    4. 海南出入境检验检疫局技术中心, 海南 海口 570311
  • 收稿日期:2017-10-24 出版日期:2018-04-08 发布日期:2014-02-26
  • 通讯作者: 张峰,Tel:(010)53898008,E-mail:fengzhang@126.com
  • 基金资助:

    中央级公益性科研院所基本科研业务费专项资金项目（2016JK028）；贵州茅台酒股份有限公司研发项目（2016010）.

Determination of 14 sweeteners in liquid foods by hydrophilic interaction liquid chromatography-tandem mass spectrometry

FAN Guangyu1,2, FENG Feng1, ZHANG Feng1, GAO Fei1, LI Xiaoming3, LIANG Zhengang4   

  1. 1. Institute of Food Safety, Chinese Academy of Inspection and Quarantine, Beijing 100176, China;
    2. Lianyungang Entry-Exit Inspection and Quarantine Bureau, Lianyungang 222042, China;
    3. Jinan Entry-Exit Inspection and Quarantine Bureau, Jinan 250014, China;
    4. Technology Center of Hainan Entry-Exit Inspection and Quarantine Bureau, Haikou 570311, China
  • Received:2017-10-24 Online:2018-04-08 Published:2014-02-26
  • Supported by:

    Fundamental Research Fund of Central Public Welfare Research Institution (No. 2016JK028); Research and Development Project of Kweichow Moutai Co., Ltd. (No. 2016010).

PDF

106

摘要：

建立了亲水相互作用色谱-三重四极杆质谱（HILIC-MS/MS）同时测定液体食品中6种人工合成甜味剂和8种甜菊糖苷类天然甜味剂的分析方法。样品经Waters Xbridge Amide色谱柱（150 mm×5.0 mm，3.5 μm）分离，以乙腈-10 mmol/L甲酸铵溶液（65：35，v/v）为流动相，流速为0.4 mL/min，柱温为35℃，然后以电喷雾电离（ESI）源，在多反应监测（MRM）、负离子模式下进行三重四极杆质谱检测。14种甜味剂在各自的范围内线性关系良好，相关系数均大于0.995，检出限为0.03~0.7 mg/kg，定量限为0.1~2.2 mg/kg。在2、5和20 mg/kg添加水平下，14种甜味剂的平均回收率为80.8%~108.7%，相对标准偏差为1.5%~7.7%（n=6）。该方法样品前处理操作简单，准确度高，灵敏度高，可用于液体食品中14种甜味剂的同时测定。

关键词: 亲水相互作用色谱, 人工合成甜味剂, 三重四极杆质谱, 甜菊糖苷, 液体食品

Abstract:

A method for the simultaneous determination of six artificial sweeteners and eight steviol glycosides in liquid food samples by hydrophilic interaction liquid chromatography-tandem mass spectrometry (HILIC-MS/MS) was developed.The sweeteners in the samples were separated by a Waters Xbridge Amide column (150 mm×5.0 mm, 3.5 μm) at 35℃, and eluted with acetonitrile-10 mmol/L ammonium formate (65:35, v/v) at a flow rate of 0.4 mL/min.Then, the analytes were detected using an electrospray ion source in negative mode (ESI-) under multiple reaction monitoring (MRM) mode.Good linear relationships were obtained, and the correlation coefficients (r2) of the 14 sweeteners were greater than 0.995.The limits of detection (LODs, S/N=3) and the limits of quantification (LOQs, S/N=10) ranged from 0.03 to 0.7 mg/kg and 0.1 to 2.2 mg/kg, respectively.The average recoveries varied from 80.8% to 108.7% at spiked levels of 2, 5 and 20 mg/kg, and the relative standard deviations (RSDs) ranged from 1.5% to 7.7%(n=6).The proposed method is simple, accurate and sensitive for the simultaneous determination of the 14 sweeteners in liquid food samples.

Key words: artificial sweeteners, hydrophilic interaction liquid chromatography (HILIC), liquid food, steviol glycosides, triple quadrupole mass spectrometry

中图分类号: