SDE-GC-MS法重现性及普洱茶发酵香气变化研究
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摘要
【目的】为研究同时蒸馏萃取法提取普洱茶香气物质的重现性。【方法】以2次普洱茶发酵的原料(晒青毛茶)和出堆样为材料,SDE各提取3次,应用气相色谱质谱联用仪检测。【结果】各样品中鉴定出64～82个化合物,物质鉴定重复率为50.78%～71.30%;同一样品3次重复检测物质峰面积的精密度(RSD)为0.76%～70.91%。原料以醇类物质(53.3%和50.0%)为主,发酵后1,2,3-三甲氧基苯、3,4,5-三甲氧基苯等杂氧化合物增加,出堆样以杂氧化合物(44. 0%和41.5%)为主。【结论】SDE-GC-MS法研究茶叶香气需增加重复次数或改进方法。
【Objective】The aroma substances in Pu-erh tea were studied by Simultaneous-dist extraction(SDE) previously, however, the reproducibility of these methods were not studied. 【Method】 In this work, two raw materials and two Pu-erh tea fermented samples were extracted three times by Simultaneous-dist extraction method(SDE), and detected by Gas Chromatography-mass Spectrometry(GC-MS), respectively. 【Result】The 64-82 compounds were detected, and the repetition rate of substance identification were 50.78 %-71.30 %. The reproducibility(RSD) of peak areas detected in the same samples for three times was 0.76 %-70.91 %. The main aroma substances in raw materials(R1 and R2) were alcohol with relative contents of 53.3 % and 50.0 %, respectively. After fermentation, relative levels of heterocyclic compounds, such as 1, 2, 3-trimethoxy benzene and 3, 4, 5-trimethoxy benzene were increased. And main aroma substances in fermented samples(P1 and P2) were heterocyclic compounds with relative contents of 44.0 % and 41.5 %, respectively. 【Conclusion】It need to develop more repeats analyses or improve the extraction method in the study of aroma substances of Pu-erh tea using SDE-GC-MS method.
【Objective】The aroma substances in Pu-erh tea were studied by Simultaneous-dist extraction(SDE) previously, however, the reproducibility of these methods were not studied. 【Method】 In this work, two raw materials and two Pu-erh tea fermented samples were extracted three times by Simultaneous-dist extraction method(SDE), and detected by Gas Chromatography-mass Spectrometry(GC-MS), respectively. 【Result】The 64-82 compounds were detected, and the repetition rate of substance identification were 50.78 %-71.30 %. The reproducibility(RSD) of peak areas detected in the same samples for three times was 0.76 %-70.91 %. The main aroma substances in raw materials(R1 and R2) were alcohol with relative contents of 53.3 % and 50.0 %, respectively. After fermentation, relative levels of heterocyclic compounds, such as 1, 2, 3-trimethoxy benzene and 3, 4, 5-trimethoxy benzene were increased. And main aroma substances in fermented samples(P1 and P2) were heterocyclic compounds with relative contents of 44.0 % and 41.5 %, respectively. 【Conclusion】It need to develop more repeats analyses or improve the extraction method in the study of aroma substances of Pu-erh tea using SDE-GC-MS method.
引文
[1]曹艳妮,刘通讯.不同储存时间普洱生茶和熟茶香气成分分析[J].食品工业,2011(10):64-67.
[2]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.
[3]吕才有,单治国,刘勤晋.普洱茶后发酵中的香气成分变化分析[J].食品科学,2009(10):252-256.
[4]叶静,王文光,李军,等.四种曲霉属真菌发酵对普洱茶香气成分的影响(英文)[J].Journal of Chinese Pharmaceutical Sciences,2016(4):284-290.
[5]施梦南,龚淑英.茶叶香气研究进展[J].茶叶,2012,38(1):19-23.
[6]曹艳妮,刘通讯.普洱生茶和熟茶香气中萜烯类和甲氧基苯类成分分析[J].食品工业科技,2012(5):128-130.
[7]赵苗苗,杨如兵,吕才有.基于电子鼻及GC-MS技术对临沧晒青毛茶香气成分的对比研究[J].中国农学通报,2018,34(2):113-122.
[8]Xu X,Yan M,Zhu Y.Influence of Fungal Fermentation on the Development of Volatile Compounds in the Puer Tea Manufacturing Process[J].Engineering in Life Sciences,2005,5(4):382-386.
[9]Gong Z,Watanabe N,Yagi A,et al.Compositional Change of Tea during Processing[J].Bioscience Biotechnology & Biochemistry,2014,57(10):1745-1746.
[10]李建勋,杜丽平,王超,等.顶空固相微萃取-气相色谱-质谱联用法分析黑茶香气成分[J].食品科学,2014,35(2):191-195.
[11]陈保,徐明发,姜东华,等.不同普洱茶原料渥堆发酵过程中香气成分的变化研究[J].食品安全质量检测学报,2018,9(2):284-293.
[12]张灵枝,王登良,陈维信,等.不同贮藏时间的普洱茶香气成分分析[J].园艺学报,2007,34(2):504-506.
[13]徐咏全,张晨霞,孔雅雯,等.HS-SPME-GC-MS-GC-O分析普洱茶粉中的关键性香气组分[J].食品研究与开发,2017(20):152-159.
[14]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(16):257-262.
[15]Lv H,Zhong Q,Lin Z,et al.Aroma characterisation of Pu-erh tea using headspace-solid phase microextraction combined with GC/MS and GC-olfactometry[J].Food Chemistry,2012,130(4):1074-1081.
[16]谷勋刚,张正竹,宁井铭,等.普洱茶渥堆阶段游离态香气成分分析及含量变化[J].食品与发酵工业,2010(4):161-164.
[17]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.
[18]李建勋,杜丽平,王超,等.顶空固相微萃取-气相色谱-质谱联用法分析黑茶香气成分[J].食品科学,2014,35(2):191-195.
[19]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(11):292-298.
[20]吕海鹏,张悦,杨停,等.影响普洱熟茶香气品质的关键香气成分分析[J].现代食品科技,2015,31(12):394-399.
[2]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.
[3]吕才有,单治国,刘勤晋.普洱茶后发酵中的香气成分变化分析[J].食品科学,2009(10):252-256.
[4]叶静,王文光,李军,等.四种曲霉属真菌发酵对普洱茶香气成分的影响(英文)[J].Journal of Chinese Pharmaceutical Sciences,2016(4):284-290.
[5]施梦南,龚淑英.茶叶香气研究进展[J].茶叶,2012,38(1):19-23.
[6]曹艳妮,刘通讯.普洱生茶和熟茶香气中萜烯类和甲氧基苯类成分分析[J].食品工业科技,2012(5):128-130.
[7]赵苗苗,杨如兵,吕才有.基于电子鼻及GC-MS技术对临沧晒青毛茶香气成分的对比研究[J].中国农学通报,2018,34(2):113-122.
[8]Xu X,Yan M,Zhu Y.Influence of Fungal Fermentation on the Development of Volatile Compounds in the Puer Tea Manufacturing Process[J].Engineering in Life Sciences,2005,5(4):382-386.
[9]Gong Z,Watanabe N,Yagi A,et al.Compositional Change of Tea during Processing[J].Bioscience Biotechnology & Biochemistry,2014,57(10):1745-1746.
[10]李建勋,杜丽平,王超,等.顶空固相微萃取-气相色谱-质谱联用法分析黑茶香气成分[J].食品科学,2014,35(2):191-195.
[11]陈保,徐明发,姜东华,等.不同普洱茶原料渥堆发酵过程中香气成分的变化研究[J].食品安全质量检测学报,2018,9(2):284-293.
[12]张灵枝,王登良,陈维信,等.不同贮藏时间的普洱茶香气成分分析[J].园艺学报,2007,34(2):504-506.
[13]徐咏全,张晨霞,孔雅雯,等.HS-SPME-GC-MS-GC-O分析普洱茶粉中的关键性香气组分[J].食品研究与开发,2017(20):152-159.
[14]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(16):257-262.
[15]Lv H,Zhong Q,Lin Z,et al.Aroma characterisation of Pu-erh tea using headspace-solid phase microextraction combined with GC/MS and GC-olfactometry[J].Food Chemistry,2012,130(4):1074-1081.
[16]谷勋刚,张正竹,宁井铭,等.普洱茶渥堆阶段游离态香气成分分析及含量变化[J].食品与发酵工业,2010(4):161-164.
[17]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.
[18]李建勋,杜丽平,王超,等.顶空固相微萃取-气相色谱-质谱联用法分析黑茶香气成分[J].食品科学,2014,35(2):191-195.
[19]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(11):292-298.
[20]吕海鹏,张悦,杨停,等.影响普洱熟茶香气品质的关键香气成分分析[J].现代食品科技,2015,31(12):394-399.