色谱

色谱 ›› 2019, Vol. 37 ›› Issue (1): 87-92.DOI: 10.3724/SP.J.1123.2018.08013

• 研究论文 • 上一篇    下一篇

超高效液相色谱-四极杆/静电场轨道阱高分辨质谱非靶标筛查测定白酒和饮料中甜菊糖苷

冯峰1, 李伟明2, 孙燕1,3, 张峰1   

  1. 1. 中国检验检疫科学研究院食品安全研究所, 北京 100176;
    2. 番禺出入境检验检疫局综合技术服务中心实验室, 广东 广州 511400;
    3. 北京中医药大学, 北京 100029
  • 收稿日期:2018-09-18 出版日期:2019-01-08 发布日期:2014-11-29
  • 通讯作者: 张峰,Tel:(010)53898026,E-mail:fengzhang@126.com.
  • 基金资助:

    国家重点研发计划项目（2017YFC1601600）；贵州茅台酒股份有限公司研发项目（2016010）.

Non-targeted screening and determination of steviol glycosides in Chinese liquor and beverages by ultra high performance liquid chromatography-quadrupole/Orbitrap mass spectrometry

FENG Feng1, LI Weiming2, SUN Yan1,3, ZHANG Feng1   

  1. 1. Institute of Food Safety, Chinese Academy of Inspection and Quarantine, Beijing 100176, China;
    2. Technical Service Center Laboratory of Panyu Entry-Exit Inspection and Quarantine Bureau, Guangzhou 511400, China;
    3. Beijing University of Chinese Medicine, Beijing 100029, China
  • Received:2018-09-18 Online:2019-01-08 Published:2014-11-29
  • Supported by:

    National Key Research and Development Program of China (No. 2017YFC1601600); Research and Development Project of Kweichow Moutai Co., LTD (No. 2016010).

PDF

128

摘要：

建立了亲水作用色谱-超高效液相色谱-四极杆/静电场轨道阱质谱非靶向筛查测定白酒和饮料中甜菊糖苷的分析方法，并对甜菊糖苷类天然甜味剂的质谱裂解规律进行了研究。样品经水溶液适当稀释，过滤膜后经Waters Xbridge Amide色谱柱（150 mm×4.6 mm，3.5 μm）分离，超高效液相色谱-四极杆/静电场轨道阱质谱检测，电离模式为电喷雾电离源负离子模式，数据采集使用一级母离子全扫描和数据依赖的二级子离子扫描（full MS/dd-MS2）模式。基于8种甜菊糖苷标准品的碎片离子谱分析，识别出甜菊糖苷类化合物存在两个共性碎片离子，以这两个离子作为标识离子对样品中未知甜菊糖苷类化合物进行了非靶标筛查。通过方法学验证，8种甜菊糖苷标准品在10~1000 μg/L内线性关系良好，检出限为0.3~20 μg/L。添加量为10~100 μg/kg时，平均回收率为81.9%~106%，相对标准偏差为0.1%~9.3%（n=3）。该方法筛查范围广，结果准确，灵敏度高，可用于食品中甜菊糖苷的非靶标筛查测定。

关键词: 超高效液相色谱, 非靶标筛查, 高分辨质谱, 甜菊糖苷

Abstract:

A method for simultaneous screening and determination of steviol glycosides in Chinese liquor and beverages by hydrophilic interaction ultra-high performance liquid chromatography-quadrupole/Orbitrap high resolution mass spectrometry (HILIC-UHPLC-Q/Orbitrap HRMS) was developed. In addition, the MS fragment path ways of steviol glycosides were characterized. The sample was diluted and filtrated before analysis, separated by a Waters Xbridge Amide column (150 mm×4.6 mm, 3.5 μm), and determined via UHPLC-Q/Orbitrap HRMS. The analytes were electronic using electro spray ion source in the negative mode, and the data were collected using full mass scan and data-dependent MS2 scan. Good linear relationships (10-1000 μg/L) were obtained. The limits of detection ranged from 0.3 to 20 μg/L. The mean recoveries varied from 81.9% to 106% at the spiked levels of 10-100 μg/kg, and the relative standard deviations ranged from 0.1% to 9.3% (n=3). Two characteristic fragment ions of steviol glycosides were identified by the analysis of fragment ion spectra of eight types of steviol glycosides standards. Non-targeted screening of unknown steviol glycosides in samples was carried out on the basis of the identified characteristic fragment ions. The proposed method is comprehensive, accurate, and sensitive for rapid screening and determination of sweeteners in food samples.

Key words: high resolution mass spectrometry (HRMS), non-targeted screening, steviol glycosides, ultra high performance liquid chromatography (UHPLC)

中图分类号: