Microsoft Word ，陈保-二校

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1 8 6 Vol. 8 No Journal of Food Safety and Quality Jun., 陈保 1*, 满红平 1, 姜东华 1, 罗正刚 1, 高晓丽 2, 李忠华 2 (1., ; 2., ) 摘要 : 目的方法, (headspace-solid-phase microextraction, HS-SPME) - (gas chromatography-mass spectrometry, GC-MS), 结果,,,, ; ()(I Ⅱ Ⅲ Ⅳ), β-()1,2,3-1,2,4-, 结论,,, 关键词 : ; ; ; ; - Changes of aroma components during Pu er tea fermentation process by headspace-solid-phase microextraction and gas chromatography-mass spectrometry CHEN Bao 1*, MAN Hong-Ping 1, JIANG Dong-Hua 1, LUO Zheng-Gang 1, GAO Xiao-Li 2, LI Zhong-Hua 2 (1. National Center for Pu er Tea Product Quality Supervision and Inspection, Pu er , China; 2. Yunnan Cha Zu Tea Limited Company, Pu er , China) ABSTRACT: Objective To analyze the changes of aroma components during Pu er tea fermentation process. Methods The changes of aroma components during pile-fermentation of Pu er tea were studied by fully automated headspace-solid-phase microextraction (HS-SPME), and were identified by gas chromatography mass spectrometry (GC-MS). Results With the changes of fermentation process, the content of alcohol compounds showed fluctuant trend, the content of ketone, ester and hydrocarbons were decreased, phenols and methoxybenzene were increased, and aldehydes and acids had little change. The content of linalool oxides(i, Ⅱ, Ⅲ, Ⅳ) was highest, benzyl alcohol and β-phenethyl alcohol were the lowest in the end of pile (seventh pile), the content of 1,2,3-trimethoxybenzene and 1,2,4-trimethoxybenzene were the highest at the later pile (sixth pile), then decreased at the seventh pile. Conclusion The variation of aroma components is significant in the pile-fermentation process, which provides some technological supports for improving fermentation process and stabilizing quality. 基金项目 : (2012yzjk03) Fund: Supported by the Science and Technology Plan of Yunnan Provincial Bureau of Quality and Technical Supervision (2012yzjk03) * 通讯作者 :,,, chenbao8493@163.com *Corresponding author: CHEN Bao, Master, Engineer, National Center for Pu er Tea Product Quality Supervision and Inspection, Yongping Road, Simao Zone, Pu er , China. chenbao8493@163.com

2 KEY WORDS: Pu'er tea; pile-fermentation; aroma components; headspace-solid-phase microextraction; gas chromatography-mass spectrometry 1 引言, ()() [1] (), [2],,,, [3-5],,,, [6-13], [14-16], [17],, [18,19] ;, [20] [21,22], (headspace-solid-phase microextraction, HS-SPME)- (gas chromatography-mass spectrometry, GC-MS),, 2 材料和方法 2.1 材料与设备试验材料 : 2014 (), 8.78 t,, (30±1)%,,, 7 :, 7 d 1, ( 10 cm, 50 cm) ( 10 cm, 30 cm) ( 10 cm, 5 cm) 500 g, ( 1:1:1 ), 设备 7890A/7000B - ( Agilent ); ( CTC ); 65 µm PDMS/DVB(Polydimethlsiloxane/Divinylbenzene)( Supelco ) 2.2 试验方法香气提取条件, PDMS/DVB GC h, 2 g 20 ml,,, GC-MS 条件 GC : HP-MS (30 m 0.25 mm, 0.25 µm); 220 ;, 99.99%, 1.2 ml/min; : 50, 1 min, 3 /min 120, 3 min, 5 /min 260, 10 min; MS : EI, 70 ev, 230, 280, 45~450 m/z 2.3 数据处理 GC-MS, NIST11.L,,,, ( ) 3 结果与分析 3.1 普洱茶渥堆过程中香气成分分析, 8, 1 71, 23 ( ), 16 ( 6 7 ), 2, 6, 4, 11, 4, 3, 2 65, 7, 88.26%, 10 : (13.13%) (6.16%) β- (4.77%)(4.09%) Ⅱ(4.05%) α- (3.39%) Ⅳ(3.02%) α- (2.67%) (2.41%) I(2.34%);, β-, α-,,

3 6, : ,, α-,,, 57, 87.93%, 10 : (26.44%) β- (5.68%)(4.37%) α- (2.97%) Ⅱ(2.82%) Ⅳ(2.80%) β- (2.33%)(2.32%) I(2.08%) 1,2,4- (2.02%); β-,, 1,2,4-,,, 53, 84.44%, 10 : (24.99%) Ⅱ(6.82%) Ⅳ(5.10%) α- (4.24%) I(4.17%) α- (3.56%) 1,2,4- (2.84%) Ⅲ(2.45%)(2.33%) 1,2,3- (2.12%); α-, 1,2,4-1,2,3-,, Table 1 表 1 普洱茶渥堆发酵过程中香气成分分析结果 Results of aroma components during Pu er tea fermentation process (%) 1 I Ⅱ Ⅲ Ⅳ α α ,7, β , ,4,

4 续表 1 (%) α α γ ,6, α β , , , , ,3, β α β , δ

5 6, : 续表 1 (%) , ,2, ,2, N Fig. 1 1 Changes of aroma components during Pu'er tea fermentation process 3.2 普洱茶渥堆发酵过程中香气成分组成变化 1,,,,,,, 36.78%, 27.4%, 28.31%, (28.68%);,, 8.04%, 54.9%;,, 6.02%, 62.2%;,, 65.6%; 3.21% 2 ;, 8.67%, 15.7 ; 3.3 普洱茶渥堆发酵过程中主要香气成分的变化 2 3, (I Ⅱ Ⅲ Ⅳ) α-,,,, 0.87%, 78.7%;

6 (I Ⅱ Ⅲ Ⅳ), 4.17% 6.82% 5.10% 4.75%, 78.2% 68.4% %; α-, 4.75%, 40.1%,,,,,, [23,24] ; α-, [25,26] 3, β-,,,, 2.61%, 5.87, ; β-, 9.28%, 6.80,, 0.42%, 65.7%, β- 6,,,, α-,, 2 Fig. 2 Changes of linalool oxides 4 Fig. 4 Changes of ketone compounds 3 Fig. 3 Changes of alcohols compounds 5 Fig. 5 Changes of methoxybenzene compounds

7 6, : [10],,, α-,, 1.42%,, 3.56%, 1.51,,,,,,, [8],,, 2.33%, 62.2% 4, α- β-,,, α-β-, 0.22% 0.37% 1.47%, 77.3% 80.7% 69.2%,, β- [24] 5, 1,2,3-1,2,4-, 1,2,3-,, 3.57%; 1,2,4-, 4.50%, 7.65, [27] ; (), [24],, [10] 4 结论与讨论,,,,, ;, (I Ⅱ Ⅲ Ⅳ) α- ; β- ; α- β- ; ; α-, ; 1,2,3-1,2,4-,,,,,, β-,, [18],,,, 18.54%, 65.5%, [20], 4,, 4 15%~30% 1,2,3-1,2,4-,,,, [28],,,,,,,, 1,2,3-1,2,4- 参考文献 [1] GB/T [S]. GB/T Product of geographical indication-pu er tea [S]. [2] Lu HP, Zhang YJ, Lin Z, et al. Processing and chemical constituents of Pu-erh tea: a review [J]. Food Res Int, 2013, 53(2): [3] Hou Y, Shao WF, Xiao R, et al. Pu-erh tea aqueous extracts lower atherosclerotic risk factors in a rat hyperlipidemia model [J]. Exp Gerontol, 2009, 44(6/7): [4] Kuo KL, Weng MS, Chiang CT, et al. Comparative studies on the hypolipidemic and growth suppressive effects of oolong, black, Pu-erh, and green tea leaves in rats [J]. J Agric Food Chem, 2005, 53(2): [5] Lee LK, Foo KY. Recent advances on the beneficial use and health implications of Pu-erh tea [J]. Food Res Int, 2013, 53(2): [6],. [J]., 2011, 10: Cao YN, Liu TX. Analysis of aroma composition in Pu-erh raw and ripe teas with different storage time [J]. Food Ind, 2011, 10: [7],,,. [J]., 2010, 26(9): Ren HT, Zhou B, Xia KG, et al. Analysis and comparison of the aroma components of Pu-er raw tea in different grades [J]. Mod Food Sci Technol, 2010, 26(9): [8],,. [J]., 2014, 27(1): Zhang X, Liu L, Tong HR. Analysis of volatile components of Pu-erh tea [J]. Southwest China J Agric Sci, 2014, 27(1): [9],,,. [J]., 2016, 42(12): Tian XJ, Wang J, Deng YJ, et al. Characteristic aroma components analysis of raw Pu er tea at different storage time [J]. Food Ferment Ind, 2016, 42(12):

8 [10],,,. [J]., 2007, 34(2): Zhang LZ, Wang DL, Chen WX, et al. Determination of volatiles of Pu er tea stored for different lengths time [J]. Acta Hortic Sin, 2007, 34(2): [11],,,. [J]., 2015, 36(10): : Xie JL, Zhang W, Chen XQ, et al. Analysis of changes in aroma constituents during storage of ripe Pu er tea [J]. J Food Sci, 2015, 36(10): [12],. [J]., 2015,31(4): Liu TX, Tan MZ. The effect of different drying temperatures on the transformation of polyphenols and volatile aroma components in Pu-erh tea [J]. Mod Food Sci Technol, 2015, 31(4): [13] Zhu Y, Luo Y, Wang P, et al. Simultaneous determination of free amino acids in Pu-erh tea and their changes during fermentation [J]. Food Chem, 2016, 194: [14],,,. [J]., 2015, 31(12): Lv HP, Zhang Y, Yang T, et al. Key aroma constituents affecting the quality of ripened Pu-erh tea [J]. Mod Food Sci Technol, 2015, 31(12): [15],. [J]., 2012, 5: Cao YN, Liu TX. Analysis of lerpenes and methoxybenzene components in aroma composition of Pu-erh raw tea and ripe tea [J]. Sci Technol Food Ind, 2012, 5: [16],,,. [J]., 2014, 34(1): Chen CM, Chen Z, Shi H, et al. Analysis on characteristic flavor components of aged Pu-erh tea [J]. J Tea Sci, 2014, 34(1): [17],,,. [J]., 2014, 34(1): Lv HP, Zhong QS, Shi J, et al. Study on fingerprint on volatile constituents of Pu-erh tea [J]. J Tea Sci, 2014, 34(1): [18],,,. [J]., 2009, 29(2): Lv HP, Zhong QS, Wang L, et al. Study on the change of aroma constituents during Pu-erh tea process [J]. J Tea Sci, 2009, 29(2): [19],,. [J]., 2009, 30(10): Lv CY, Shan ZG, Liu QJ. Analysis of changes in aroma components of Pu-erh tea during post-fermentation process [J]. J Food Sci, 2009, 30(10): [20],,,. Ren HT, Zhou B, Xia KG, et al. Compare analysis of fermentation degree on the aromatic components of Pu-erh tea [J]. Food Res Dev, 2011, 32(11): [21],,,. [J]., 2015,6(4): Chen B, Liu XY, Pu HJ, et al. Study on variation of main chemical components during Pu er tea fermentation process of different raw materials [J]. J Food Saf Qual, 2015, 6(4): [22],,,. [J]., 2016, 37(4): Chen B, Pu HJ, Dao SQ, et al. Study on variation of metal elements during Pu er tea fermentation [J]. Sci Technol Food Ind, 2016, 37(4): [23],,,. [J]., 2014, 35( 11): Lv SD, Meng QX, Xu YQ, et al. Recent progress in aroma analysis methods and aroma active compounds in Pu-erh tea [J]. J Food Sci, 2014, 35( 11): [24] Du L, Li J, Li W, et al. Characterization of volatile com-pounds of Pu-erh tea using solid-phase micro extraction and simultaneous distillation-extraction coupled with gas chromatography-mass spectrometry [J]. Food Res Int, 2014, 57: [25],,,. /GC-MS [J]., 2013, 34(8) : Lv SD, Jiang DH, Yang F, et al. Analysis of aroma components between Pu-erh ripe tea and anhua dark tea by headspace solid-phase micro extraction and GC-MS [J]. Chin J Trop Crops, 2013, 34(8): [26] Lv HP, Zhong QS, Lin Z, et al. Aroma characterisation of Pu-erh tea using headspace-solid phase micro extraction combined with GC/MS and GC-olfactometry [J]. Food Chem, 2012, 130(4): [27] Xu X, Yan M, Zhu Y. Influence of fungal fermentation on the development of volatile compounds in the Puer tea manufacturing process [J]. Eng Life Sci, 2005, 5( 4): [28],,,. [J]., 2010, 36(4): Gu XG, Zhang ZZ, Ning JM, et al. Analysis of free aroma components and change of aroma components during the pile-fermation process of Pu-erh tea [J]. Food Ferment Ind, 2010, 36(4): 作者简介 ( 责任编辑 : 杨翠娜 ) 陈保, 硕士, 工程师, 主要研究方向为茶叶分析测试 chenbao8493@163.com [J]., 2011, 32(11):

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Microsoft Word ， 陈 保-二校

Microsoft Word ，陈保-二校