刘青青^1，5，吕杨俊^2，4，曹晓念^1，3，5，潘俊娴^2，4，冯华芳^1，5，蒋玉兰^2，4，兰 余^1，5，张士康^2，4，朱跃进^2，4*，沈才洪^1，3，5*

（1.泸州老窖股份有限公司，四川泸州 646000；

2.中华全国供销合作总社杭州茶叶研究院，浙江杭州 310016；

3.国家固态酿造工程技术中心，四川泸州 646000；

4.浙江省茶资源跨界应用技术重点实验室，浙江杭州 310016；

5.国家级沈才洪酿酒师技能大师工作室，四川泸州 646000）

摘要：采用50/30 μm DVB/CAR/PDMS萃取头，在四种萃取温度（45、50、60、70 ℃）下萃取40 min，以不分流或分流两种模式，分流模式下包括1∶1、3∶1、5∶1、10∶1四种分流比，分别对茶酒挥发性物质进行萃取，通过气相色谱-质谱检测，建立适用于茶酒挥发性物质萃取分析的检测方法。结果表明，分流模式较适用于茶酒挥发性物质检测，分流比3∶1 时检出的茶酒挥发性物质总数最多，且更利于茶酒中低丰度的茶叶挥发性物质检出。萃取温度为50 ℃时，检测出茶酒挥发性物质总数最多；因此，检测茶酒中挥发性物质的适宜条件为：50/30 μm DVB/CAR/PDMS萃取头，萃取温度50 ℃，萃取时间40 min，分流模式，分流比3∶1。在该条件下，茶酒中共检出70种挥发性物质，其中以己酸乙酯、丁酸乙酯、辛酸乙酯、庚酸乙酯、乙酸乙酯、己酸己酯、戊酸乙酯、己酸等为主，并检出芳樟醇、α-松油醇等茶叶挥发性物质。同时经四大酯、三大酸标准溶液检测验证，该条件具有较好的重复性和准确性，该方法的建立可为茶酒挥发性物质的分析提供参考。

关键词：茶酒；挥发性物质；顶空固相微萃取-气相色谱-质谱联用技术

中图分类号：TS207.3 文献标识码：A 文章编号：1674-506X（2022）02-0137-0009

Study on Detection Method of Volatile Compounds in Tea Liquor Based on HS-SPME-GC-MS

LIU Qingqing^1，5，LV Yangjun^2，4，CAO Xiaonian^1，3，5，PAN Junxian^2，4，FENG Huafang^1，5，JIANG Yulan^2，4，LAN yu^1，5，ZHANG Shikang^2，4，ZHU Yuejin^2，4*，SHEN Caihong^1，3，5*

（1.Luzhou Laojiao Co., Ltd., Luzhou Sichuan 646000, China;

2.Hangzhou Tea Research Institute, CHINA COOP, Hangzhou Zhejiang 310016, China;

3.National Engineering Technology Research Center of Solid-state Brewing, Luzhou Sichuan 646000, China;

4.Zhejiang Key Laboratory of Transboundary Applied Technology for Tea Resources, Hangzhou Zhejiang 310016, China;

5.National SHEN Caihong Wine-making Skills Master Studio, Luzhou Sichuan 646000, China）

Abstract：In order to establish a suitable method for extraction and analysis of volatile compounds in tea liquor. The volatile compounds in tea liquor were extracted by using a 50/30 μm divinylbenzene/carboxen/polydimethylsiloxane (DVB/CAR/PDMS) extraction head, with 4 extraction temperatures of 45 ℃, 50 ℃, 60 ℃ and 70 ℃ for 40min and detected by gas chromatography-mass spectrometry (GC-MS) using two kinds of split mode, no split mode and split mode, and four different split ratios 1∶1, 3∶1, 5∶1 and 10∶1 were used in split mode. The results showed that the split injection mode was more suitable for the detection of volatile compounds in tea liquor, and when the split ratio was 3∶1, the total number of volatile compounds in tea liquor was the most, and it was more conducive to the detection of low abundance volatile compounds of tea in tea liquor. When the extraction temperature was 50 ℃, the total number of volatile compounds in tea liquor was the most. Therefore, the appropriate conditions for extraction and analysis of volatile substances in tea liquor were 50/30 μm DVB/CAR/PDMS extraction head, extraction temperature 50 ℃ for 40 min, split injection and split ratio 3∶1. Under this conditions, 70 kinds of volatile compounds were detected in tea liquor. The main volatile compounds were ethyl hexanoate, ethyl butyrate, ethyl octanoate, ethyl heptanoate, ethyl acetate, hexyl hexanoate, ethyl valerate, hexanoic acid and other. The volatile components of tea including linalool and α-terpineol were detected. The method was verified by the standard solution of three major acids and four major esters, which showed good repeatability and accuracy. The establishment of this method can provide reference for the detection of volatile compounds in tea liquor.

Keywords：tea liquor; volatile compounds; HS-SPME-GC-MS

doi：10.3969/j.issn.1674-506X.2022.02-021

收稿日期：2021-05-17

基金项目：酒城英才专项“泸州老窖养生酒技术产业创新团队”

作者简介：刘青青（1990-），女，硕士，工程师。研究方向：露酒、白酒品评及风味研究。

*通信作者：朱跃进（1957-），女，研究员，研究方向：茶叶加工及跨界开发；沈才洪（1966-），男，正高级工程师，博士生导师，首批国家非物质文化遗产传承人。研究方向：发酵工程。

引用格式：刘青青,吕杨俊,曹晓念,等.基于HS-SPME-GC-MS的茶酒挥发性物质检测方法研究[J].食品与发酵科技,2022,58(2):137-144,155.