食品科学

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超高效液相色谱串联质谱同时测定酒类产品中多种人工合成甜味剂

周 彬,吕任一,肖丽恒*,李 萍,何学梅,杨 芩,杨丽娜   

  1. 楚雄州质量技术监督综合检测中心,云南 楚雄 675000
  • 出版日期:2014-06-25 发布日期:2014-07-03
  • 通讯作者: 肖丽恒

Simultaneous Determination of Synthetic Sweeteners in Liquor Products by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

ZHOU Bin, LÜ Ren-yi, XIAO Li-heng*, LI Ping, HE Xue-mei, YANG Qin, YANG Li-na   

  1. Chuxiong Quality of the Technical Supervision and Inspection Center, Chuxiong 675000, China
  • Online:2014-06-25 Published:2014-07-03
  • Contact: XIAO Li-heng

摘要:

建立超高效液相色谱-电喷雾电离串联质谱(ultra performance liquid chromatography-electro spray ionizationtandem mass spectrometry,UPLC-ESI-MS-MS)同时测定酒类产品中安赛蜜、糖精钠、甜蜜素、三氯蔗糖、阿斯巴甜、阿力甜和纽甜人工合成甜味剂的分析方法。方法采用ZORBAX Eclipse XDB-C18柱(100 mm×4.6 mm,1.8 μm)色谱柱,柱温50 ℃。流动相由A(甲醇)和B(体积分数0.1%甲酸和20 mmol/L甲酸铵溶液,pH 4.0)组成,流速为0.5 mL/min,梯度洗脱。在ESI负离子模式下,采用多反应监测模式进行测定,可以在12.5 min内完成7 种人工合成甜味剂的检测。安赛蜜、糖精钠、甜蜜素、三氯蔗糖、阿斯巴甜、阿力甜和纽甜在10~5 000 μg/L范围内有良好的线性关系,相关系数大于0.999。安赛蜜、糖精钠、甜蜜素、三氯蔗糖、阿斯巴甜、阿力甜和纽甜检出限分别为4、6、4、8、4、4、2 μg/L,回收率在88.3%~98.3%之间,相对标准偏差为2.1%~6.7%。该方法快速、准确,灵敏度高,适用于酒类产品中低含量人工合成甜味剂的测定。

关键词: 超高效液相色谱-串联质谱, 质谱法, 酒类产品, 甜味剂

Abstract:

An ultra performance liquid chromatography-electrospray ionization tandem mass spectrometry (UPLC-ESIMS-
MS) method was developed for the simultaneous determination of seven synthetic sweeteners, acesulfame-K, sodium
saccharin, sodium cyclamate, sucralose, aspartame, alitame and neotame, in liquor products. ZORBAX Eclipse XDB-C18
column (100 mm × 4.6 mm, 1.8 μm) chromatographic column was used, and the solvent system was composed of mobile
phase A (methanol), and mobile phase B (0.1% formic acid and 20 mmol/L ammonium formate in water, pH 4.0). The flow
rate was 0.5 mL/min for gradient elution, and the column temperature was held at 50 ℃. In the ESI negative ion mode,
multiple reaction monitoring (MRM) was used for quantitation. The 7 kinds of artificial sweeteners were successfully
detected within 12.5 min. These sweeteners showed good linear relationships in the range of 10–5 000 μg/L with correlation
coefficients larger than 0.999. The limits of detection (LODs) for acesulfame-K, saccharin sodium, sodium cyclamate,
sucralose, aspartame, alitame and neotame were 4, 6, 4, 8, 4, 4 and 2 μg/L, respectively, and recovery rates for spiked
samples ranged from 88.3% to 98.3%, with relative standard deviations between 2.1% and 6.7%. A rapid, accurate and
sensitivity method has been developed in this study and this method has been successfully applied to the determination of
synthetic sweeteners at low levels in liquor products.

Key words: ultra performance liquid chromatography-electro spray ionization tandem mass spectrometry (UPLC-MS-MS), mass spectrometry, liquor products, synthetic sweeteners

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