食品科学 ›› 2021, Vol. 42 ›› Issue (8): 283-287.doi: 10.7506/spkx1002-6630-20191030-333

• 安全检测 • 上一篇    下一篇

超高效液相色谱-高分辨质谱测定白酒中氨基甲酸乙酯含量

熊晓通,胡峰,尤小龙,尹艳艳,陈明学,程平言,钟方达   

  1. (贵州茅台酒厂(集团)习酒有限责任公司,贵州 习水 564622)
  • 出版日期:2021-04-25 发布日期:2021-05-14
  • 基金资助:
    贵州省科技重大专项(黔科合重大专项字([2015]6012)); 遵义市科技计划项目(遵市科合(2018)29号;遵市科合R&D(2019)4号)

Determination and Quantitation of Ethyl Carbamate in Chinese Baijiu by Ultra-high Performance Liquid Chromatography-High Resolution Mass Spectrometry

XIONG Xiaotong, HU Feng, YOU Xiaolong, YIN Yanyan, CHEN Mingxue, CHENG Pingyan, ZHONG Fangda   

  1. (Guizhou Maotai Distillery (Group) Xijiu Co. Ltd., Xishui 564622, China)
  • Online:2021-04-25 Published:2021-05-14

摘要: 利用氨基甲酸乙酯(ehthy carbamate,EC)源内裂解的特殊性质,在超高效液相色谱-高分辨质谱一级全扫描模式下,以EC母离子(m/z 90.05)及其子离子(m/z 62.02)作为定性离子,m/z?62.02作为定量离子,开发酱香型白酒中EC的一级子离子定量法,有效解决了一级母离子定量噪音较大、二级子离子定量响应较低的问题。结果表明,在12.2~244?μg/L内线性相关系数大于0.999,检出限为0.95?μg/L,加标回收率在83.46%~106.79%之间,相对标准偏差为0.67%~3.54%。该方法具有分析速度快、检出限低、准确度高等优点,适用于酱香型白酒中EC的监控。

关键词: 氨基甲酸乙酯;源内裂解;Q?Exactive?Focus质谱;一级子离子定量;酱香型白酒。

Abstract: A new method for the quantitation of ethyl carbamate (EC) in Maotai-flavor Baijiu was developed using ultra-high performance liquid chromatography-high resolution mass spectrometry with primary daughter ions. Based on the fact that it has the special property of in-source fragmentation, EC was detected under the full scan model. The primary parent ion with m/z 90.05 was used as qualitative ion and its daughter ion with m/z 62.02 as both qualitative and quantitative ions considering that a great noise and low response values were achieved respectively when using the primary parent ion and the secondary daughter ion as quantitative ions. The calibration curve showed good linearity in the range of 12.2–244 μg/L with a correlation coefficient greater than 0.999. The limit of detection (LOD) was 0.95 μg/L. The recoveries of EC from spiked samples were 83.46%–106.79%, with relative standard deviations (RSD) of 0.67%–3.54%. Overall, the method was suitable for the quantitation of EC in Maotai-flavor Baijiu with the advantages of rapidity, low detection limit and high accuracy.

Key words: ethyl carbamate; in-source fragmentation; Q Exactive Focus mass spectrometry; primary daughter ion quantitation; Maotai-flavor Baijiu

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