9个菠萝蜜品系香气成分及特征香气分析
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摘要
【目的】分析不同品系菠萝蜜果实的香气成分和特征香气。【方法】以9个菠萝蜜品系为试材,采用顶空固相微萃取-气相色谱-质谱联用技术分析菠萝蜜果实的香气成分。【结果】9个菠萝蜜品系共检测出挥发性成分130种,其中含有71种酯、16种醇、19种醛、8种酮、3种酸、6种烃类和7种其他物质。9个品系都是以酯类物质为主,醇类物质次之,酸类物质最少;采用聚类分析将‘海大2号’‘20号’‘四季’‘28号’‘45号’‘红肉327’‘305’和‘湿苞’8个品系聚为一类,‘92号’单独为一类;9个菠萝蜜品系的特征香气成分存在一定差异。【结论】菠萝蜜果实的香气成分以酯类为主,醛类次之;不同品系的香气成分不同,各品系间的亲缘关系也不相同;特征香气存在差异,经过OAV值法分析,异戊醇是9个品系都含有的特征香气物质。
【Objective】This study analyzed the aroma components in nine jackfruit varieties and classified the varieties based on aroma components using principal component analysis and cluster analysis.The characteristic aromatic components detected in jackfruits were quantified using the odour activity value(OAV), ratio of concentration of the volatile compound to its odour threshold. Aroma components with the aroma value greater than or equal to 1 were regarded as characteristic aroma.【Methods】The aroma components in the nine jackfruit varieties were analyzed by headspace solid-phase microextraction-gas chromatography-mass spectrometry(SPME-GC-MS). The flesh tissue was homogenized with beater in liquid nitrogen. Flesh(0.2 g) was weighed in 20 mL jaws and added with 5 mL of saturated sodium chloride solution to extract aroma ingredients for 40 min. Aroma ingredients were detected by SHIMADZU QP2010-Plus gas chromatography-mass spectrometer with an automatic injection. A 65μm PDMS/DVB solid phase microextraction extraction head was aged at 250 ℃ for 1 hour in the gas chromatographic inlet before injection. The chromatography was equipped with a DB-5 capillary column(30 m × 0.25 mm × 0.25 μm) and the column temperature was raised following the procedure: initial 40 ℃ for 1 min, an increase to 100 ℃ at 3.5 ℃·min~(-1), and to 180 ℃, and a further increase at 5 ℃·min~(-1) to 250 ℃, which was maintained for 3 min. The inlet temperature was kept at 250 ℃. There was no shunt. The carrier gas was helium at a flow rate of 1.0 mL · min~(-1). Desorption of the extractor at the inlet was allowed for 2 min. The mass spectrometry conditions included an electron impact ion source(EI),an ion source temperature of 230 ℃, an interface temperature of 280 ℃, a detector voltage 350 V, an electron energy 70 e V and a scanning quality range of 35-335 amu. The external standards were methylisovalerate, butyl isovalerate, ethyl isovalerate, butyl acetate, isoamyl acetate, n-propyl acetate, butyl butyrate, benzaldehyde, n-hexanal, isovaleraldehyde, active amyl alcohol, 1-pentanol, isoamyl alcohol, nbutanol, isobutyl isovalerate and isoamyl isovalerate, which were of HPLC purity grade and purchased from Sigma. Sodium chloride(AR) was provided by Sinopharm Chemical Reagent.【Results】There were 130 volatile components in the nine jackfruit varieties, including 71 esters, 16 alcohols, 19 aldehydes, 8 ketones, 3 acids, 6 hydrocarbons and 7 other substances. The nine varieties were dominated by ester-based substances, followed by alcohol substances, acid substances and so on. The major aroma components in the nine varieties included 12 components, namely isoamyl isovalerate, isopentyl isooctanoate, propyl isovalerate, amyl valerate, butyl isovalerate, amyl valerate, esters, isobutyl isovalerate,phenylpropionaldehyde, isoamyl alcohol, ethyl isovalerate and isoamyl acetate. The characteristic aroma was different among the nine varieties. The principal component analysis and cluster analysis(intergroup connection) were used to classify the nine cultivars. The case system cluster analysis was carried out based on the Euclidean distance. When the distance was 9, 6 varieties including the‘Haida 2'‘No.20'‘Siji'‘No. 28'‘No. 45'and‘Red flesh 327'were grouped together in a class, which displayed obvious difference with the other three varieties. When the distance was 11, the 9 varieties could be divided into two categories,‘No. 92'alone as a class, and the other eight as the other class. And the distance between‘No. 92'and the other eight varieties was the greatest(25). The main aroma components in‘Haida 2'‘No. 20'‘Siji'‘No. 28'‘No. 45'‘Red flesh 327'‘305'and‘Soft type'were isoamyl isovalerate, amyl isovalerate, butyl isovalerate, ethyl isovalerate, propyl isovalerate and heptanoic acid heptyl ester, without isoamyl octanoate. The main aroma components in‘No. 92'were isovalerate butyl ester and isoamyl octanoate, which was unique in‘No. 92'. The comprehensive scores of the aroma components in the nine jackfruit varieties were in order of‘No. 92'>‘No. 45'>‘305'>‘Soft type'>‘No. 20'>‘Haida 2'>‘No. 28'>‘Red flesh 327'>‘Siji'. There were more than 40 esters in‘305'‘Soft type'‘No. 28'‘No. 45'and‘Siji'. However, in‘Red flesh 327'there were only 30 esters, but alcohol substances, aldehydes, hydrocarbons and other substances were most abundant among the nine varieties. There were isovaleraldehyde, isovalerate, isoamyl alcohol, isovaleric acid and phenylethyl alcohol in‘Haida 2';ethyl 2-methyl butyrate, ethyl isovalerate, isopentyl alcohol and isovaleric acid in‘305'; ethyl 2-methyl butyrate, isoamyl acetate, ethyl isovalerate, isoamyl alcohol and isovaleric acid in‘Soft type'; ethyl isovalerate and isoamyl alcohol in‘No. 28'; isoamyl acetate, ethyl isovalerate and isoamyl alcohol in‘No. 45'; isovaleraldehyde, alcohols and isovaleric acid in‘No. 20'; isovaleraldehyde, isoamyl acetate, isovalerate, isoamyl alcohol and phenylethyl alcohol in‘Red flesh 327'; isoamyl alcohol in‘Siji'; and isovaleraldehyde,(Z)-2-decenal, isoamyl alcohol, phenylethyl alcohol and isovaleric acid in‘No. 92'.【Conclusion】Although the aroma components of the nine varieties of jackfruit were different, the important aroma components of the nine cultivars were esters, which accounted for more than half of the total aroma and formed the major flavor substances in jackfruit. Isoamyl alcohol was the characteristic aroma substance in the nine cultivars according to the results of OAV value analysis. Isooctanoate was a unique aroma ingredient of‘No. 92', which was quite different from the other eight varieties.‘Red flesh 327'had the least amount of esters, but it contained the largest variety of substances including the specific component of 1-chloropentane, which provides a special aroma of this cultivar.
【Objective】This study analyzed the aroma components in nine jackfruit varieties and classified the varieties based on aroma components using principal component analysis and cluster analysis.The characteristic aromatic components detected in jackfruits were quantified using the odour activity value(OAV), ratio of concentration of the volatile compound to its odour threshold. Aroma components with the aroma value greater than or equal to 1 were regarded as characteristic aroma.【Methods】The aroma components in the nine jackfruit varieties were analyzed by headspace solid-phase microextraction-gas chromatography-mass spectrometry(SPME-GC-MS). The flesh tissue was homogenized with beater in liquid nitrogen. Flesh(0.2 g) was weighed in 20 mL jaws and added with 5 mL of saturated sodium chloride solution to extract aroma ingredients for 40 min. Aroma ingredients were detected by SHIMADZU QP2010-Plus gas chromatography-mass spectrometer with an automatic injection. A 65μm PDMS/DVB solid phase microextraction extraction head was aged at 250 ℃ for 1 hour in the gas chromatographic inlet before injection. The chromatography was equipped with a DB-5 capillary column(30 m × 0.25 mm × 0.25 μm) and the column temperature was raised following the procedure: initial 40 ℃ for 1 min, an increase to 100 ℃ at 3.5 ℃·min~(-1), and to 180 ℃, and a further increase at 5 ℃·min~(-1) to 250 ℃, which was maintained for 3 min. The inlet temperature was kept at 250 ℃. There was no shunt. The carrier gas was helium at a flow rate of 1.0 mL · min~(-1). Desorption of the extractor at the inlet was allowed for 2 min. The mass spectrometry conditions included an electron impact ion source(EI),an ion source temperature of 230 ℃, an interface temperature of 280 ℃, a detector voltage 350 V, an electron energy 70 e V and a scanning quality range of 35-335 amu. The external standards were methylisovalerate, butyl isovalerate, ethyl isovalerate, butyl acetate, isoamyl acetate, n-propyl acetate, butyl butyrate, benzaldehyde, n-hexanal, isovaleraldehyde, active amyl alcohol, 1-pentanol, isoamyl alcohol, nbutanol, isobutyl isovalerate and isoamyl isovalerate, which were of HPLC purity grade and purchased from Sigma. Sodium chloride(AR) was provided by Sinopharm Chemical Reagent.【Results】There were 130 volatile components in the nine jackfruit varieties, including 71 esters, 16 alcohols, 19 aldehydes, 8 ketones, 3 acids, 6 hydrocarbons and 7 other substances. The nine varieties were dominated by ester-based substances, followed by alcohol substances, acid substances and so on. The major aroma components in the nine varieties included 12 components, namely isoamyl isovalerate, isopentyl isooctanoate, propyl isovalerate, amyl valerate, butyl isovalerate, amyl valerate, esters, isobutyl isovalerate,phenylpropionaldehyde, isoamyl alcohol, ethyl isovalerate and isoamyl acetate. The characteristic aroma was different among the nine varieties. The principal component analysis and cluster analysis(intergroup connection) were used to classify the nine cultivars. The case system cluster analysis was carried out based on the Euclidean distance. When the distance was 9, 6 varieties including the‘Haida 2'‘No.20'‘Siji'‘No. 28'‘No. 45'and‘Red flesh 327'were grouped together in a class, which displayed obvious difference with the other three varieties. When the distance was 11, the 9 varieties could be divided into two categories,‘No. 92'alone as a class, and the other eight as the other class. And the distance between‘No. 92'and the other eight varieties was the greatest(25). The main aroma components in‘Haida 2'‘No. 20'‘Siji'‘No. 28'‘No. 45'‘Red flesh 327'‘305'and‘Soft type'were isoamyl isovalerate, amyl isovalerate, butyl isovalerate, ethyl isovalerate, propyl isovalerate and heptanoic acid heptyl ester, without isoamyl octanoate. The main aroma components in‘No. 92'were isovalerate butyl ester and isoamyl octanoate, which was unique in‘No. 92'. The comprehensive scores of the aroma components in the nine jackfruit varieties were in order of‘No. 92'>‘No. 45'>‘305'>‘Soft type'>‘No. 20'>‘Haida 2'>‘No. 28'>‘Red flesh 327'>‘Siji'. There were more than 40 esters in‘305'‘Soft type'‘No. 28'‘No. 45'and‘Siji'. However, in‘Red flesh 327'there were only 30 esters, but alcohol substances, aldehydes, hydrocarbons and other substances were most abundant among the nine varieties. There were isovaleraldehyde, isovalerate, isoamyl alcohol, isovaleric acid and phenylethyl alcohol in‘Haida 2';ethyl 2-methyl butyrate, ethyl isovalerate, isopentyl alcohol and isovaleric acid in‘305'; ethyl 2-methyl butyrate, isoamyl acetate, ethyl isovalerate, isoamyl alcohol and isovaleric acid in‘Soft type'; ethyl isovalerate and isoamyl alcohol in‘No. 28'; isoamyl acetate, ethyl isovalerate and isoamyl alcohol in‘No. 45'; isovaleraldehyde, alcohols and isovaleric acid in‘No. 20'; isovaleraldehyde, isoamyl acetate, isovalerate, isoamyl alcohol and phenylethyl alcohol in‘Red flesh 327'; isoamyl alcohol in‘Siji'; and isovaleraldehyde,(Z)-2-decenal, isoamyl alcohol, phenylethyl alcohol and isovaleric acid in‘No. 92'.【Conclusion】Although the aroma components of the nine varieties of jackfruit were different, the important aroma components of the nine cultivars were esters, which accounted for more than half of the total aroma and formed the major flavor substances in jackfruit. Isoamyl alcohol was the characteristic aroma substance in the nine cultivars according to the results of OAV value analysis. Isooctanoate was a unique aroma ingredient of‘No. 92', which was quite different from the other eight varieties.‘Red flesh 327'had the least amount of esters, but it contained the largest variety of substances including the specific component of 1-chloropentane, which provides a special aroma of this cultivar.
引文
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[5]RASMUSSEN P.Identification of volatile components of jackfruit by gas chromatography/mass spectrometry with two different columns[J].Analytical Chemistry,1983,55(8):1331-1335.
[6]WONG K C,LIM C L,WONG L L.Volatile flavour constituents of chempedak(Artocarpus polyphema Pers.)fruit and jackfruit(Artocarpus heterophyllus Lam.)from malaysia[J].Flavour&Fragrance Journal,1992,7(6):307-311.
[7]MAIA J G S,ANDRADE E H A,ZOGHBI M D G B.Aroma volatiles from two fruit varieties of jackfruit(Artocarpus heterophyllus Lam.)[J].Food Chemistry,2004,85(2):195-197.
[8]ONG B T,NAZIMAH S A H,OSMAN A,QUEK S Y,VOONY Y,HASHIM D M,CHEW P M,KONG Y W.Chemical and flavour changes in jackfruit(Artocarpus heterophyllus Lam.)cultivar J3 during ripening[J].Postharvest Biology&Technology,2006,40(3):279-286.
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[10]纳智.菠萝蜜中香气成分分析[J].热带亚热带植物学报,2004,12(6):538-540.NA Zhi.Analysis of aroma components in jackfruit[J].Journal of Tropical and Subtropical Botany,2004,12(6):538-540.
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[12]贺书珍,张彦军,徐飞,朱科学,谭乐和,吴刚,付莉莉.菠萝蜜果实成熟过程中香气成分组成及变化规律研究[J].热带作物学报,2015,36(9):1614-1619.HE Shuzhen,ZHANG Yanjun,XU Fei,ZHU Kexue,TAN Lehe,WU Gang,FU Lili.Study on composition and variation of aroma components in fruit ripening process of pineapple fruit[J].Chinese Journal of Tropical Crops,2015,36(9):1614-1619.
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[15]PINO J A,MESA J.Contribution of volatile compounds to mango(Mangifera indica L.)aroma[J].Flavour&Fragrance Journal,2006,21(2):207-213.
[16]孙宝国.食用调香术第二版[M].北京:化学工业出版社,2010:4.SUN Baoguo.Edible flavoring second edition[M].Beijing:Chemical Industry Press,2010:4.
[17]丁吉星,何玉云,梁艳英,崔长伟,王华,李华.新型嘉宝果起泡酒香气成分及特征香气分析[J].食品科学,2014,35(24):145-150.DING Jixing,HE Yuyun,LIANG Yanying,CUI Changwei,WANG Hua,LI Hua.Analysis of aroma components and characteristic aroma of new Jiabao fruit sparkling wine[J].Food Science,2014,35(24):145-150.
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[2]ADELA K.Flavor quality of fruits and vegetables[J].Journal of the Science of Food&Agriculture,2008,88(11):1863-1868.
[3]刘鑫泉.菠萝蜜果实香味物质形成相关酶活性及基因表达分析[D].湛江:广东海洋大学,2016.LIU Xinquan.Study on activity and gene expression of fragrance substance in pineapple fruits[D].Zhanjiang:Guangdong Ocean University,2016.
[4]SWORDS G,BOBBIO P A,HUNTER G L K.Volatile constituents of jackfruit(Arthocarpus heterophyllus)[J].Journal of Food Science,2010,43(2):639-640.
[5]RASMUSSEN P.Identification of volatile components of jackfruit by gas chromatography/mass spectrometry with two different columns[J].Analytical Chemistry,1983,55(8):1331-1335.
[6]WONG K C,LIM C L,WONG L L.Volatile flavour constituents of chempedak(Artocarpus polyphema Pers.)fruit and jackfruit(Artocarpus heterophyllus Lam.)from malaysia[J].Flavour&Fragrance Journal,1992,7(6):307-311.
[7]MAIA J G S,ANDRADE E H A,ZOGHBI M D G B.Aroma volatiles from two fruit varieties of jackfruit(Artocarpus heterophyllus Lam.)[J].Food Chemistry,2004,85(2):195-197.
[8]ONG B T,NAZIMAH S A H,OSMAN A,QUEK S Y,VOONY Y,HASHIM D M,CHEW P M,KONG Y W.Chemical and flavour changes in jackfruit(Artocarpus heterophyllus Lam.)cultivar J3 during ripening[J].Postharvest Biology&Technology,2006,40(3):279-286.
[9]郭飞燕,纪明慧,舒火明,陈静,陈益南.海南菠萝蜜挥发油的提取及成分鉴定[J].食品科学,2010,31(2):168-170.GUO Feiyan,JI Minghui,SHU Huoming,CHEN Jing,CHENYinan.Extraction and composition identification of volatile oil from pineapple in hainan[J].Food Science,2010,31(2):168-170.
[10]纳智.菠萝蜜中香气成分分析[J].热带亚热带植物学报,2004,12(6):538-540.NA Zhi.Analysis of aroma components in jackfruit[J].Journal of Tropical and Subtropical Botany,2004,12(6):538-540.
[11]李洪波,刘胜辉,李映志,毛琪,叶春海.顶空固相微萃取和气相色谱-质谱法测定菠萝蜜果肉中的香气成分[J].热带作物学报,2013,34(4):755-763.LI Hongbo,LIU Shenghui,LI Yingzhi,MAO Qi,YE Chunhai.Determination of aroma components in pineapple flesh by headspace solid phase microextraction and gas chromatographymass spectrometry[J].Chinese Journal of Tropical Crops,2013,34(4):755-763.
[12]贺书珍,张彦军,徐飞,朱科学,谭乐和,吴刚,付莉莉.菠萝蜜果实成熟过程中香气成分组成及变化规律研究[J].热带作物学报,2015,36(9):1614-1619.HE Shuzhen,ZHANG Yanjun,XU Fei,ZHU Kexue,TAN Lehe,WU Gang,FU Lili.Study on composition and variation of aroma components in fruit ripening process of pineapple fruit[J].Chinese Journal of Tropical Crops,2015,36(9):1614-1619.
[13]魏长宾,刘胜辉,陆新华,吴青松,孙光明.6个菠萝品种香气成分及特征香气分析[J].广东农业科学,2015,42(24):111-117.WEI Changbin,LIU Shenghui,LU Xinhua,WU Qingsong,SUN Guangming.Analysis of aroma components and characteristic aroma of six pineapple cultivars[J].Guangdong Agricultural Sciences,2015,42(24):111-117.
[14]HAYATA Y,SAKAMOTO T,MANEERAT C,LI X,KOZUKAH,SAKAMOTO K.Evaluation of aroma compounds contributing to muskmelon flavor in porapak Q extracts by aroma extract dilution analysis[J].Journal of Agricultural&Food Chemistry,2003,51(11):3415-3418.
[15]PINO J A,MESA J.Contribution of volatile compounds to mango(Mangifera indica L.)aroma[J].Flavour&Fragrance Journal,2006,21(2):207-213.
[16]孙宝国.食用调香术第二版[M].北京:化学工业出版社,2010:4.SUN Baoguo.Edible flavoring second edition[M].Beijing:Chemical Industry Press,2010:4.
[17]丁吉星,何玉云,梁艳英,崔长伟,王华,李华.新型嘉宝果起泡酒香气成分及特征香气分析[J].食品科学,2014,35(24):145-150.DING Jixing,HE Yuyun,LIANG Yanying,CUI Changwei,WANG Hua,LI Hua.Analysis of aroma components and characteristic aroma of new Jiabao fruit sparkling wine[J].Food Science,2014,35(24):145-150.
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