色谱 ›› 2015, Vol. 33 ›› Issue (3): 250-255.DOI: 10.3724/SP.J.1123.2014.11018

• 研究论文 • 上一篇    下一篇

超高效液相色谱-串联质谱法同时测定食品中4种常用香精

杨华梅, 杭莉   

  1. 泰州市疾病预防控制中心, 江苏 泰州 225300
  • 收稿日期:2014-11-13 修回日期:2015-01-06 出版日期:2015-03-08 发布日期:2015-02-12
  • 通讯作者: 杨华梅

Determination of four frequently-used essences in foods by ultra performance liquid chromatography-tandem mass spectrometry

YANG Huamei, HANG Li   

  1. Taizhou Center for Disease Control and Prevention, Taizhou 225300, China
  • Received:2014-11-13 Revised:2015-01-06 Online:2015-03-08 Published:2015-02-12

摘要:

建立了超高效液相色谱-串联质谱法同时测定食品中香兰素、乙基香兰素、麦芽酚和乙基麦芽酚4种香精的方法。样品用水提取,固相萃取小柱净化,目标化合物采用UPLCTMBEH C18色谱柱(50 mm×2.1 mm, 1.7 μm)分离,以甲醇和含0.002 mol/L乙酸铵及0.1%(v/v)甲酸的水溶液为流动相进行梯度洗脱,采用电喷雾离子源电离、正离子多反应监测模式质谱检测。4种香精在5~500 μg/L或10~1000 μg/L质量浓度范围内线性良好,相关系数均在0.9995~0.9998之间;回收率为75.8%~116%,相对标准偏差(RSD, n=6)为1.58%~4.01%。该方法灵敏、准确,检测范围广,分析速度快,适合食品中香兰素、乙基香兰素、麦芽酚和乙基麦芽酚4种香精的检测。

关键词: 超高效液相色谱-电喷雾电离串联质谱法, 麦芽酚, 食品, 香兰素, 乙基麦芽酚, 乙基香兰素

Abstract:

A method has been developed for the simultaneous determination of vanillin, ethyl vanillin, maltol and ethyl maltol in foods by ultra performance liquid chromatography coupled with electrospray ionization tandem mass spectrometry (UPLC-ESI-MS/MS). The sample was extracted with ultrapure water, and purified with SPE column. The target compounds were separated on a C18 column with the gradient elution of methanol and water containing 0.002 mol/L ammonium acetate and 0.1%(v/v) formic acid. The four components were determined in the modes of electrospray positive ionization (ESI+) and multiple reaction monitoring (MRM). The linear ranges were 10-1000 μg/L for vanillin and maltol and 5-500 μg/L for ethyl vanillin and ethyl maltol, with the correlation coefficients more than 0.999. The recoveries of the four compounds ranged from 75.8% to 116%, with the relative standard deviations (RSDs) of 1.58%-4.01%. The method showed good extraction efficiency, high sensitivity and good reproducibility. It is suitable for the simultaneous detection of vanillin, ethyl vanillin, maltol and ethyl maltol in foods.

Key words: ethyl vanillin, ethyl vanillin, food, maltol, ultra performance liquid chromatography-electrospray ionization tandem mass spectrometry (UPLC-ESI-MS/MS), vanillin

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