普洱熟茶香气成分的顶空固相微萃取条件优化
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摘要
目的优化普洱熟茶香气成分顶空固相微萃取(headspace solid-phase microextraction,HS-SPME)-气质联用的萃取条件。方法利用Box-Benhnken的中心组合实验设计原理,以香气物质的质谱图峰面积为考察指标,对水/茶比、萃取温度、萃取时间进行3因素3水平响应面分析。结果萃取时间、萃取温度、萃取时间-萃取温度、水茶比的二次项和萃取温度的二次项对普洱茶中香气成分提取有显著影响(P<0.05),而其他几项影响不显著。利用Design-Expert 8.0软件,对数据分析后,得到最优条件为水/茶比为9.76、萃取时间2.47 h、萃取温度76.64℃。结论在优化的条件下,香气物质峰面积可达到理论上的最大值是5.48×10~8。
Objective To optimize the extraction conditions of aroma components of ripe Pu-er tea by headspace solid-phase microextraction(HS-SPME)-gas chromatography-mass(GC-MS). Methods Based on Box-Benhnken's central composite experimental design principle, 3 factors and 3 levels of response surface analysis were carried out of the ratio of water to tea, extraction temperature and extraction time with the peak area of aroma substances as the index. Results The extraction time, extraction temperature, extraction time-extraction temperature, the second term of water-tea ratio and extraction temperature had significant effects on the extraction of aroma components in Pu-er tea(P<0.05), while the other factors had no significant effects. After data analysis using Design-expert 8.0 software, the optimal conditions were obtained as follows: water/tea ratio was 9.76, extraction time was 2.47 h, and extraction temperature was 76.64 ℃. Conclusion Under optimized conditions, the peak area of aroma substances can reach the theoretical maximum value of 5.48×10~8.
Objective To optimize the extraction conditions of aroma components of ripe Pu-er tea by headspace solid-phase microextraction(HS-SPME)-gas chromatography-mass(GC-MS). Methods Based on Box-Benhnken's central composite experimental design principle, 3 factors and 3 levels of response surface analysis were carried out of the ratio of water to tea, extraction temperature and extraction time with the peak area of aroma substances as the index. Results The extraction time, extraction temperature, extraction time-extraction temperature, the second term of water-tea ratio and extraction temperature had significant effects on the extraction of aroma components in Pu-er tea(P<0.05), while the other factors had no significant effects. After data analysis using Design-expert 8.0 software, the optimal conditions were obtained as follows: water/tea ratio was 9.76, extraction time was 2.47 h, and extraction temperature was 76.64 ℃. Conclusion Under optimized conditions, the peak area of aroma substances can reach the theoretical maximum value of 5.48×10~8.
引文
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[14]刘晓慧,张丽霞,王日为,等.顶空固相微萃取-气相色谱-质谱联用法分析黄茶香气成分[J].食品科学,2010,31(16):239-243.Liu XH,Zhang LX,Wang RW,et al.Analysis of volatile components of yellow tea by HS-SPME/GC-MS[J].Food Sci,2010,31(16):239-243.
[15]张文杰,刘聪,严亮,等.HS-SPME结合GC-MS分析普洱茶花及茶花粉香气成分[J].食品工业科技,2017,38(16):257-262.Zhang WJ,Liu C,Yan L,et al.Analysis of aroma components in pu-erh tea flower and flower powder by headspace solid-phase microextraction coupled with GC-MS[J].Sci Technol Food Ind,2017,38(16):257-262.
[16]Liu DH,Shi J,Posada LR,et al.Separating tocotrienols from palm oil by molecular distillation[J].Food Rev Inter,2008,24(4):376-391.
[17]Camara JS,Marques JC,Perestrelo RM,et al.Comparative study of the whisky aroma profile based on headspace solid phase microextraction using different fibre coatings[J].J Chromatogr A,2007,1150(1-2):198-207.
[2]张超,卢艳,李冀新,等.茶叶香气成分以及香气形成的机理研究进展[J].福建茶叶,2005,(3):17-19.Zhang C,Lu Y,Li JX,et al.Research progress on aroma components and formation mechanism of tea aroma[J].Tea Fujian,2005,(3):17-19.
[3]吕世懂,孟庆雄,徐咏全,等.普洱茶香气分析方法及香气活性物质研究进展[J].食品科学,2014,35(11):292-298.Lv SD,Meng QX,Xu YQ,et al.Recent progress in aroma analysis methods and aroma active compounds in Pu-erh tea[J].Food Sci,2014,35(11):292-298.
[4]Xu YQ,Wang C,Li CW,et al.Characterization of aroma-active compounds of pu-erh tea by headspace solid-phase microextraction(HS-SPME)and simultaneous distillation-extraction(SDE)coupled with GC-olfactometry and GC-MS[J].Food Anal Method,2016,9(5):1188-1198.
[5]洪涛,黄遵锡,李俊俊,等.普洱熟茶和生茶香气成分的提取和测定分析[J].茶叶科学,2010,30(5):336-342.Hong T,Huang ZX,Li JJ,et al.Extraction and analysis on the aromatic components of Pu-erh ripe tea and raw tea[J].J Tea Sci,2010,30(5):336-342.
[6]Lv HP,Zhong QS,Lin Z,et al.Aroma characterisation of Pu-erh tea using headspace-solid phase microextraction combined with GC/MS and GC-olfactometry[J].Food Chem,2012,130(4):1074-1081.
[7]黄长修,王宏涛,蓝洪桥,等.超临界CO2萃取铁观音茶叶香气成分[J].化学工程,2010,38(12):1-4.Huang CX,Wang HT,Lan HQ,et al.Extraction of arom acomponents from Tieguanyin tea by using supercritical CO2[J].Chem Eng,2010,38(12):1-4.
[8]王道平,甘秀海,梁志远,等.固相微萃取法与同时蒸馏萃取法提取茶叶香气成分[J].西南农业学报,2013,26(1):131-135.Wang DP,Gan XM,Liang ZY,et al.Analysis on aroma compositions of tea by SPME and SDE[J].J Southwest Agric Sci,2013,26(1):131-135.
[9]黄世永,杜丽平,李建勋,等.HS-SPME-GC-MS分析普洱茶中木香类特征香气成分[J].饮料工业,2015,18(5):24-29.Huang SY,Du LP,Li JX,et al.Analysis of wood aroma characteristic compounds in Pu-erh tea by HS-SPME-GC-MS[J].Beverage Ind,2015,18(5):24-29.
[10]李艳清,付大友,王蓉.茶叶香气成分测定方法研究进展[J].茶叶科学技术,2009,(1):8-10.Li YQ,Fu DY,Wang R.Advances in the determination of aroma components in tea[J].J Tea Sci Technol,2009,(1):8-10.
[11]Wu Y,Lv S,Lian M,et al.Study of characteristic aroma components of baked Wujiatai green tea by HS-SPME/GC-MS combined with principal component analysis[J].CyTA-J Food,2016,14:1-10.
[12]吕海鹏,钟秋生,林智.陈香普洱茶的香气成分研究[J].茶叶科学,2009,29(3):219-224.Lv HP,Zhong QS,Lin Z.Study on the aroma components in Pu-erh tea with stale flavor[J].J Tea Sci,2009,29(3):219-224.
[13]李倩,蒲彪.响应面法优化花椒香气成分的HS-SPME萃取条件的研究[J].食品工业科技,2012,(2):334-337.Li Q,Pu B.Optimization of component HS-SPME extraction from Zanthoxylum bumgeanum Maxim by response surface methodology[J].Sci Technol Food Ind,2012,(2):334-337.
[14]刘晓慧,张丽霞,王日为,等.顶空固相微萃取-气相色谱-质谱联用法分析黄茶香气成分[J].食品科学,2010,31(16):239-243.Liu XH,Zhang LX,Wang RW,et al.Analysis of volatile components of yellow tea by HS-SPME/GC-MS[J].Food Sci,2010,31(16):239-243.
[15]张文杰,刘聪,严亮,等.HS-SPME结合GC-MS分析普洱茶花及茶花粉香气成分[J].食品工业科技,2017,38(16):257-262.Zhang WJ,Liu C,Yan L,et al.Analysis of aroma components in pu-erh tea flower and flower powder by headspace solid-phase microextraction coupled with GC-MS[J].Sci Technol Food Ind,2017,38(16):257-262.
[16]Liu DH,Shi J,Posada LR,et al.Separating tocotrienols from palm oil by molecular distillation[J].Food Rev Inter,2008,24(4):376-391.
[17]Camara JS,Marques JC,Perestrelo RM,et al.Comparative study of the whisky aroma profile based on headspace solid phase microextraction using different fibre coatings[J].J Chromatogr A,2007,1150(1-2):198-207.