色谱

色谱 ›› 2010, Vol. 28 ›› Issue (08): 749-753.DOI: 10.3724/SP.J.1123.2010.00749

• 研究论文 • 上一篇    下一篇

高效液相色谱-串联质谱法测定葡萄酒中的5种人工合成甜味剂

嵇超1,2, 冯峰2, 陈正行1, 孙利2, 储晓刚2*   

  1. 1. 江南大学食品科学与技术国家重点实验室, 江苏 无锡 214036; 2. 中国检验检疫科学研究院食品安全研究所, 北京 100123
  • 收稿日期:2010-03-19 修回日期:2010-06-07 出版日期:2010-08-28 发布日期:2010-08-28
  • 通讯作者: 储晓刚,教授,博士生导师. Tel: (010)85791012, E-mail: xgangchu@163.com.
  • 基金资助:

    浙江省科学仪器设备协作共用平台科研计划项目(No. 2008F70020)

Determination of five synthetic sweeteners in wines using high performance liquid chromatography- tandem mass spectrometry

JI Chao1,2, FENG Feng2, CHEN Zhengxing1, SUN Li2, CHU Xiaogang2*   

  1. 1. State Key Laboratory of Food Science and Technology, Jiangnan University, Wuxi 214036, China; 2. Institute of Food Safety, Chinese Academy of Inspection and Quarantine, Beijing 100123, China
  • Received:2010-03-19 Revised:2010-06-07 Online:2010-08-28 Published:2010-08-28

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676

被引次数

101

摘要： 建立了测定葡萄酒中安赛蜜、糖精钠、甜蜜素、阿斯巴甜和纽甜等5种人工合成甜味剂的高效液相色谱-电喷雾电离串联质谱(HPLC-ESI MS/MS)分析方法。采用Ultimate C18色谱柱,对流动相的组成、柱温以及质谱的各种参数进行了优化和探讨。结果表明,以含0.1%(体积分数)甲酸的20 mmol/L甲酸铵缓冲液(pH 3.8)和甲醇为流动相,梯度洗脱,柱温为45 ℃下,可以在5 min内完成5种人工合成甜味剂的基线分离。在ESI负离子模式下,采用多反应监测模式进行测定时,安赛蜜、糖精钠、甜蜜素、阿斯巴甜和纽甜的检出限分别为0.6、5、1、0.8和0.2 μg/L,回收率为87.2%～103%,相对标准偏差不高于1.2%。该方法快捷、准确,灵敏度高,可用于葡萄酒及其他复杂基质食品中低剂量、复合甜味剂的测定。

关键词: 阿斯巴甜, 安赛蜜, 高效液相色谱-串联质谱法, 纽甜, 葡萄酒, 人造甜味剂, 糖精钠, 甜蜜素

Abstract: A high performance liquid chromatography-electrospray ionization tandem mass spectrometry (HPLC-ESI MS/MS) method for the determination of five synthetic sweeteners (acesulfame, sodium saccharin, sodium cyclamate, aspartame and neotame) in wines has been developed. The HPLC separation was carried out on an Ultimate C18 column (100 mm×2.1 mm, 3 μm). Several parameters, including the composition and pH of the mobile phase, column temperature and the monitor ions, were optimized for improving the chromatographic performance and the sensitivity of determination. The results demonstrated that the separation can be completed in less than 5 min by gradient elution with 20 mmol/L ammonium formate and 0.1%(v/v) formic acid (pH 3.8) and methanol as the mobile phase. The column temperature was kept at 45 ℃. When the analytes were detected by ESI--MS/MS under multiple reaction monitoring mode, the detection limits were 0.6, 5, 1, 0.8 and 0.2 μg/L for acesulfame, sodium saccharin, sodium cyclamate, aspartame and neotame, respectively. The average recoveries ranged from 87.2% to 103%. The relative standard deviations were not more than 1.2%. This method is rapid, accurate, highly sensitive and suitable for the quality control of low concentration of the synthetic sweeteners, which are illegally added to wines and other foods with complex matrices.

Key words: acesulfame, aspartame, neotame, sodium cyclamate, sodium saccharin, synthetic sweeteners, wines, high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS)