食品科学 ›› 2020, Vol. 41 ›› Issue (18): 218-225.doi: 10.7506/spkx1002-6630-20190804-048

• 成分分析 • 上一篇    下一篇

气相色谱-静电场轨道阱高分辨质谱法辅助鉴定酱油未知的气味活性化合物

冯云子,周婷,蔡宇,陈子杰,赵谋明   

  1. (1.华南理工大学食品科学与工程学院,广东?广州 510641;2.赛默飞世尔科技(中国)有限公司,上海 201206)
  • 出版日期:2020-09-25 发布日期:2020-09-18
  • 基金资助:
    “十三五”国家重点研发计划重点专项(2018YFD0400405);国家自然科学基金青年科学基金项目(31701591); 中央高校基本科研业务费专项(x2skD2190910);广东省自然科学基金项目(A2017030310027)

Identification of Unknown Aroma-active Compounds of Soy Sauce by Gas Chromatography-Orbitrap-Mass Spectrometry

FENG Yunzi, ZHOU Ting, CAI Yu, CHEN Zijie, ZHAO Mouming   

  1. (1. School of Food Science and Engineering, South China University of Technology, Guangzhou 510641, China;2. Thermo Fisher Scientific (China) Co. Ltd., Shanghai 201206, China)
  • Online:2020-09-25 Published:2020-09-18

摘要: 以高盐稀态酱油为测试样品,采用气相色谱-静电场轨道阱高分辨质谱(gas chromatography-orbitrap-mass spectrometry,GC-Orbitrap-MS)法、辅助气相色谱-单四极杆质谱-嗅闻(gas chromatography-quadruple-mass spectrometry-olfactometry,GC-Q-MS-O)联用法鉴定“未知”气味活性化合物。GC-Q-MS和GC-Orbitrap-MS分别鉴定出91?种和166?种挥发性化合物,Orbitrap-MS检出总峰面积为单四极杆质谱的31?倍。GC-Q-MS-O结果分析中有4?处较强的香气活性区域“果香”、“果香”、“清香,草香”、“花果香”,无鉴定结果。利用高分辨Orbitrap-MS技术,通过高质量精度的质谱数据推算化合物碎片及其天然同位素组成,辅助以NIST谱库比对、保留指数及香气特征等信息,全面定性4?个未知香气活性物质为异丁酸乙酯、丁酸乙酯、3-己烯-2-酮和异佛尔酮。结果表明,GC-Orbitrap-MS辅助分析GC-Q-MS-O数据,能够有效地鉴定出含量低于单四极杆质谱检出限,或因与其他物质重叠而无法准确定性的未知气味活性化合物,对于风味化学领域香气活性物质的深度挖掘具有重要意义。

关键词: 气相色谱-质谱-嗅闻;气相色谱-静电场轨道阱质谱;酱油;气味活性化合物

Abstract: Gas chromatography-orbitrap-mass spectrometry (GC-Orbitrap-MS) combined with gas chromatography-quadruple-mass spectrometry-olfactometry (GC-Q-MS-O) was used to identify the ‘unknown’ aroma active compounds of soy sauce in this study. GC-Q-MS and GC-Orbitrap-MS identified 91 and 166 volatile compounds, respectively. The total peak area detected by Orbitrap-MS was 31 times as large as that detected by Q-MS. Four intense aroma-active areas with ‘fruity’, ‘fruity’, ‘grassy’ and ‘flowery and fruity’ notes were not identified in GC-Q-MS-O. In order to identify the 4 unknown compounds, the compound fragments and natural isotopic compositions were estimated by GC-Orbitrap-MS based on the high-precision mass spectral data. In addition, by comparing the mass spectra with the NIST mass spectral library as well as considering the retention index and aroma characteristics, they were identified as ethyl isobutyrate, ethyl butyrate, 3-hexen-2-one and 3,5,5-trimethyl-2-cyclohexenone (isophorone). This study showed that GC-Orbitrap-MS combined with GC-Q-MS-O could effectively reveal the ‘unknown’ aroma-active compounds whose contents were below the detection limit of quadrupole MS, or which could not be determined due to overlapping with other volatiles, which would be of important significance for the identification of aroma-active compounds in the field of flavor chemistry.

Key words: gas chromatography-mass spectrometry-olfactometry; gas chromatography-orbitrap-mass spectrometry; soy sauce; aroma-active compounds

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