食品科学 ›› 2026, Vol. 47 ›› Issue (13): 228-235.doi: 10.7506/spkx1002-6630-20251205-060

• 成分分析 • 上一篇    下一篇

酒醅中高级脂肪酸及其乙酯类化合物高灵敏检测

高蕾,卢云浩,包晓明,涂荣坤,张晓娟,王松涛,迟原龙,许正宏   

  1. (1.四川大学轻工科学与工程学院,四川 成都 610000;2.岛津企业管理(中国)有限公司,四川 成都 610000;3.泸州老窖股份有限公司,四川 泸州 646000;4.江南大学生物工程学院,江苏 无锡 214000;5.国家固态酿造工程技术研究中心,四川 泸州 646000)
  • 出版日期:2026-07-15 发布日期:2026-07-17
  • 基金资助:
    四川大学-泸州老窖文化与科技创新研究中心科研合作项目(KY202401); 四川省科技计划资助项目(2026NSFSC0157);中央高校基本科研业务费专项资金资助项目(YJ202368)

High-Sensitivity Detection of Long-Chain Fatty Acids and Long-Chain Fatty Acid Ethyl Esters in Fermented Grains (Jiupei)

GAO Lei, LU Yunhao, BAO Xiaoming, TU Rongkun, ZHANG Xiaojuan, WANG Songtao, CHI Yuanlong, XU Zhenghong   

  1. (1. College of Biomass Science and Engineering, Sichuan University, Chengdu 610000, China; 2. Shimadzu (China) Co. Ltd., Chengdu 610000, China; 3. Luzhou Laojiao Co. Ltd., Luzhou 646000, China; 4. School of Biotechnology, Jiangnan University, Wuxi 214000, China; 5. National Engineering Research Center of Solid-State Brewing, Luzhou 646000, China)
  • Online:2026-07-15 Published:2026-07-17

摘要: 高级脂肪酸及其乙酯类化合物是影响白酒风味品质与稳定性的关键物质,然而酒醅基质复杂,干扰严重,导致目标化合物难以准确定量。以正庚烷为提取溶剂,经超声辅助提取60 min,衍生化处理30 min,基于气相色谱-串联质谱法,在多反应监测模式下采用内标-外标相结合的定量策略建立酒醅中高级脂肪酸及其乙酯类化合物含量的靶向检测方法。结果表明,18 种目标化合物在测定质量浓度范围内线性关系良好(R2>0.99),检出限为0.33~533.60 μg/L,定量限为1.11~1 778.66 μg/L,平均加标回收率为81.22%~113.67%,相对标准偏差为3.22%~12.55%,表明该方法灵敏度高、准确度与精密度良好。基于该方法对多轮次酒醅进行分析发现,油酸乙酯、亚油酸乙酯和棕榈酸乙酯在发酵过程中持续积累,且在第4轮次后加速积累,至第7轮次时3 种乙酯类化合物含量分别达245.39、729.79、161.65 mg/100 g。该检测方法前处理操作简单、准确度高,可为复杂发酵体系中痕量乙酯类化合物的高效检测提供可靠工具。

关键词: 酒醅;高级脂肪酸;高级脂肪酸乙酯;多反应监测模式;气相色谱-串联色谱法

Abstract: Long-chain fatty acids (LCFAs) and long-chain fatty acid ethyl esters (LCFAEEs) are key substances that influence the flavor quality and stability of Baijiu. However, the complex matrix of fermented grains introduces significant interferences, making the accurate quantification of target compounds challenging. In this study, a gas chromatography-tandem mass spectrometry method was established for the targeted detection of LCFAs and LCFAEEs in fermented grains. Samples were extracted using n-heptane ultrasonically for 60 min, followed by derivatization treatment for 30 min. The mass spectrometer was operated in multiple reaction monitoring (MRM) mode. Quantification of the analytes was performed using both internal and external standards. The results showed that the calibration curves for the 18 target compounds exhibited good linearity within the tested concentration ranges (R2 > 0.99), with detection limits ranging from 0.33 to 533.60 μg/L and quantification limits from 1.11 to 1 778.66 μg/L. The average recoveries for spiked sample ranged from 81.22% to 113.67%, with relative standard deviations between 3.22% and 12.55%, indicating high sensitivity, accuracy, and precision of the method. Analysis of fermented grains from various fermentation rounds using this method revealed that ethyl oleate, ethyl linoleate, and ethyl palmitate accumulated continuously during the fermentation process, with accelerated accumulation after the 4th round. By the 7th round, the contents of these three ethyl esters reached up to 245.39, 729.79, and 161.65 mg/100 g, respectively. The proposed method features simple pretreatment procedures and high accuracy, providing a reliable tool for the efficient detection of trace ethyl esters in complex fermentation systems.

Key words: jiupei; long-chain fatty acids; long-chain fatty acid ethyl esters; multiple reaction monitoring mode; gas chromatography-tandem mass spectrometry

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