银杏葡萄酒香气成分的萃取条件优化及其香气物质的测定
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摘要
香气物质的组成是影响葡萄酒品质的重要因素,作者利用响应面法优化顶空固相微萃取银杏葡萄酒中香气物质的条件,使气相色谱法检测香气物质的结果更精确。在单因素实验基础上,运用Box-Benhnken中心组合试验设计响应面分析。同时采用气质联用技术测定银杏葡萄酒中的挥发性成分组成。结果表明:顶空固相微萃取银杏葡萄酒香气的最佳条件为:萃取温度55℃、萃取时间42 min、取样量6 mL。以此优化条件并结合GC-MS分析测得银杏葡萄酒香气成分31种,其中包括酯类15种、酸3种、醇8种、羰基类化合物4种以及酚类1种,其中酯类物质含量最高且种类最多。经计算香气活性值(OAV),有23种化合物的OAV值大于1,说明大多数检测到的物质都对酒的风味产生贡献作用,尤其是异戊醇、苯乙醇、乙酸乙酯、乙酸异戊酯、己酸乙酯、庚酸乙酯以及乙醛等。
Aroma compositions of wine were one of the important factors which influenced the quality of wine. Optimal conditions were obtained via headspace solid phase microextraction(HS-SPME) to analyze aroma substances in ginkgo wine by response surface method,in order to get more accurate results by chromatography. For optimization of component extracted from ginkgo grape wine by HP-SPME,the extraction conditions were investigated using single factor and response surface methodology based on Box-Benhnken design principles. The extraction temperature,extraction time and sample volume were used as main factors when the total peak area of chromatogram was taken as response value in this study. Meanwhile,HS-SPME and gas chromatography coupled with mass spectrometry(GC-MS) were used for the qualitative determination of volatile compounds in Ginkgo wine samples. The results indicated that the optimal extraction was achieved under the following conditions:extraction temperature 55 ℃,extraction time42 min and sample volume 6 mL. Under the above conditions,31 different compounds were identified in Ginkgo grape wine samples,including 15 esters,3 fatty acids,8 higher alcohols,4 carbonyl compounds and 1 phenol compounds. Among those,esters had the highest levels,and the calculation of OAV allowed the determination of the volatile compounds the presented the greater contribution to ginkgo grape wine aroma. There were 23 volatile compounds with OAV >1 among those compounds which were detected in gingko wine. The results indicated that most compounds were showed the contribution to wine aroma,especially isopentyl alcohol,phenethyl alcohol,ethyl acetate,isoamyl acetate,ethyl hexanoate,ethyl acetate and acetaldehyde.
Aroma compositions of wine were one of the important factors which influenced the quality of wine. Optimal conditions were obtained via headspace solid phase microextraction(HS-SPME) to analyze aroma substances in ginkgo wine by response surface method,in order to get more accurate results by chromatography. For optimization of component extracted from ginkgo grape wine by HP-SPME,the extraction conditions were investigated using single factor and response surface methodology based on Box-Benhnken design principles. The extraction temperature,extraction time and sample volume were used as main factors when the total peak area of chromatogram was taken as response value in this study. Meanwhile,HS-SPME and gas chromatography coupled with mass spectrometry(GC-MS) were used for the qualitative determination of volatile compounds in Ginkgo wine samples. The results indicated that the optimal extraction was achieved under the following conditions:extraction temperature 55 ℃,extraction time42 min and sample volume 6 mL. Under the above conditions,31 different compounds were identified in Ginkgo grape wine samples,including 15 esters,3 fatty acids,8 higher alcohols,4 carbonyl compounds and 1 phenol compounds. Among those,esters had the highest levels,and the calculation of OAV allowed the determination of the volatile compounds the presented the greater contribution to ginkgo grape wine aroma. There were 23 volatile compounds with OAV >1 among those compounds which were detected in gingko wine. The results indicated that most compounds were showed the contribution to wine aroma,especially isopentyl alcohol,phenethyl alcohol,ethyl acetate,isoamyl acetate,ethyl hexanoate,ethyl acetate and acetaldehyde.
引文
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[14] ZHOU Shan,ZHAO Liwen,MA Tengjiao,et al. Fundamental theory of SPME technology and its application progress[J].Modern Scientific Instruments,2006(2):86-90.(in Chinese)
[15] PU Biao,ZHANG Yao,LIU Yun,et al. Optimization of aroma components extraction from loquat wine by HS-SPME[J].Biochemistry Engineering,2001,37(6):114-119.(in Chinese)
[16] CUEVAS-GLORY L F,PINO J A,SANTIAGO L S,et al. A review of volatile analytical methods for determining the botanical origin of honey[J]. Food Chemistry,2007,103(3):1032-1043.
[17] BOX G E P,STUART H J,GORDON H W. Statistics for experiments:an introduction to design,data analysis,and model building[M]. 1978.
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[19] SHI Jiayi,ZHANG Mengda,JU Xingrong. Optimization of SPME conditions for volatile compounds research in Indica Rice by response surface method[J]. Journal of the Chinese Cereals and Oils Association,2015,30(12):120-125.(in Chinese)
[20] MURALIDHAR R V,CHIRUMAMILA R R. A response surface approach for the comparison of lipase production by Candida cylindracea using two different carbon sources[J]. Biochemical Engineering Journal,20019(1):17-23.
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[22] GURBUZ O,ROUSEFFJ M,ROUSEFF R L. Comparison of aroma volatiles in commercial Merlot and Cabernet Sauvignon wines using gas chromatography-olfactometry and gas chromatography-mass spectrometry[J]. Journal of Agricultural and Food Chemistry,2006,54(11):3990-3996.
[23] AND W F,QIAN M C. Characterization of aroma compounds of Chinese “Wuliangye” and “Jiannanchun” liquors by aroma extract dilution analysis[J]. Journal of Agricultural and Food Chemistry,2006,54(7):2695-2704.
[24] NIU Y W,ZHANG X M,XIAO Z B,et al. Characterization of odor-active compounds of various cherry wines by gas chromatography-mass spectrometry,gas chromatography-olfactometry and their correlation with sensory attributes[J]. Journal of Chromatography B,2011,879(23):2287-2293.
[25] FUHRMANN E,GROSCH W. Character impact odorants of the apple cultivars Elstar and Cox Orange[J]. Food/Nahrung,2002,46(3):187-193.
[26] CHOI H S. Character impact odorants of Citrus Hallabong[(C. unshiu Marcov×C. sinensis Osbeck)×C. reticulata Blanco]cold-pressed peel oil[J]. Journal of Agricultural and Food Chemistry,2003,51(9):2687-2692.
[27] PEINADO R A,MORENO J A,MUNOZ D,et al. Gas chromatographic quantification of major volatile compounds and polyols in wine by direct injection[J]. Journal of Agricultural and Food Chemistry,2004,52(21):6389-6393.
[28] GARCIA-CARPINTERO E G,SANCHEZ-PALOMO E. Volatile and sensory characterization of red wines from cv. Moravia Agria minority grape variety cultivated in La Mancha region over five consecutive vintages[J]. Food Research International,2011,44(5):1549-1560.
[29] GUTH H. Quantitation and sensory studies of character impact odorants of different white wine varieties[J]. Journal of Agricultural and Food Chemistry,1997,45(8):3027-3032.
[30] PERESTRELO R,FERNANDES A. Analytical characterization of the aroma of Tinta Negra Mole red wine:Identification of the main odorants compounds[J]. Analytica Chimica Acta,2006,563(1):154-164.
[31] QUIJANO C E,SALAMANCA G,PINO J A. Aroma volatile constituents of Colombian varieties of mango(Mangifera indica L.)[J]. Flavour and Fragrance Journal,2007,22(5):401-406.
[32] LI H,TAO Y S,KANG W H,et al. Wine aroma analytical investigation progress on GC[J]. Journal of Food Science and Biotechnology,2006(1):20-20.
[33] NOGUEROL-PATO R,GONZALEZ-RODRIGUEZ R M. Influence of tebuconazole residues on the aroma composition of Mencía red wines[J]. Food Chemistry,2011,124(4):1525-1532.
[34] CHISHOLM M G,WILSON M A,GASKEY G M,Characterization of aroma volatiles in key lime essential oils(Citrus aurantifolia Swingle)[J]. Flavour and Fragrance Journal,2003,18(2):106-115.
[35] FERREIRA V,AZNAR M,LOPEZ R,et al. Quantitative gas chromatography-olfactometry carried out at different dilutions of an extract. Key differences in the odor profiles of four high-quality Spanish aged red wines[J]. Journal of Agricultural and Food Chemistry,2001,49(10):4818-4824.
[2] DU Wenming,XU Kehan. Nutrition and medicinal value of Ginkgo[J]. Hebei Forestry Science and Technology,2002(3):48-48.(in Chinese)
[3] SUN Pengpeng,WANG Jungao,LIU Mingming,et al. Research on one kind of Ginkgo leaf flavored liquor[J]. Journal of Shandong Polytechnic University,2013,27(2):42-46.(in Chinese)
[4] ZHAO Li,LIU Liping,LIU Jianjun,Study on the fermentation conditions of Ginkgo fruit wine[J]. Liquor-making Science and Technology,2014(6):35-38.(in Chinese)
[5] MALHERBE S,MENICHELLI E,TOIT M D,et al. The relationships between consumer liking,sensory and chemical attributes of Vitis vinifera L. cv. Pinotage wines elaborated with different Oenococcus oeni starter cultures[J]. Journal of the Science of Food and Agriculture,2013,93(11):2829-2840.
[6] WANG X,XIE K L,ZHUANG H N,et al. Volatile flavor compounds,total polyphenolic contents and antioxidant activities of a China gingko wine[J]. Food Chemistry,2015,182:41-46.
[7] ZHENG Xinhua,ZHANG Min,LIU Yaping. Analysis of aroma components by GC-MS and deacidification of plum wine[J]Journal of Food Science and Biotechnology,2014,33(4):432-437.(in Chinese)
[8] SAGRATINI G,MAGGI F,CAPRIOLI G,et al. Comparative study of aroma profile and phenolic content of Montepulciano monovarietal red wines from the Marches and Abruzzo regions of Italy using HS-SPME-GC-MS and HPLC-MS[J]. Food Chemistry,2012,132(3):1592-1599.
[9] WELKE J E,ZANUS M,LAZZAROTTO M,et al. Quantitative analysis of headspace volatile compounds using comprehensive two-dimensional gas chromatography and their contribution to the aroma of Chardonnay wine[J]. Food Research International,2014,59:85-99.
[10]中华人民共和国国家标准,GB/T 15038-2006,葡萄酒、果酒通用分析方法[S].北京:中国标准出版社,2006.
[11] XIAO Z B,YU D,NIU Y W,et al. Characterization of aroma compounds of Chinese famous liquors by gas chromatography-mass spectrometry and flash GC electronic-nose[J]. Journal of Chromatography B,2014,945:92-100.
[12] VAN DEN D H,KRATZ P D. A generalization of the retention index system including linear temperature programmed gas-liquid partition chromatography[J]. Journal of Chromatography A,1963,11:463-471.
[13] ZHANG Yi,GAO Bei,XU Yujuan,et al. Determination of volatile compounds in"Chuliang"longan using headspace solid-phase microextraction and GC-MS[J]. Food Science,2010,31(16):156-160.(in Chinese)
[14] ZHOU Shan,ZHAO Liwen,MA Tengjiao,et al. Fundamental theory of SPME technology and its application progress[J].Modern Scientific Instruments,2006(2):86-90.(in Chinese)
[15] PU Biao,ZHANG Yao,LIU Yun,et al. Optimization of aroma components extraction from loquat wine by HS-SPME[J].Biochemistry Engineering,2001,37(6):114-119.(in Chinese)
[16] CUEVAS-GLORY L F,PINO J A,SANTIAGO L S,et al. A review of volatile analytical methods for determining the botanical origin of honey[J]. Food Chemistry,2007,103(3):1032-1043.
[17] BOX G E P,STUART H J,GORDON H W. Statistics for experiments:an introduction to design,data analysis,and model building[M]. 1978.
[18] SADOUGHI N,SCHMIDTKE L M,ANTALICK G,et al. Gas chromatography-mass spectrometry method optimized using response surface modeling for the quantitation of fungal off-flavors in grapes and wine[J]. Journal of Agricultural and Food Chemistry,2015,63(11):2877-2885.
[19] SHI Jiayi,ZHANG Mengda,JU Xingrong. Optimization of SPME conditions for volatile compounds research in Indica Rice by response surface method[J]. Journal of the Chinese Cereals and Oils Association,2015,30(12):120-125.(in Chinese)
[20] MURALIDHAR R V,CHIRUMAMILA R R. A response surface approach for the comparison of lipase production by Candida cylindracea using two different carbon sources[J]. Biochemical Engineering Journal,20019(1):17-23.
[21] CAPONE S,TUFARIELLO M,FRANCIOSO L,et al. Aroma analysis by GC/MS and electronic nose dedicated to Negroamaro and Primitivo typical Italian Apulian wines[J]. Sensors and Actuators B:Chemical,2013,179:259-269.
[22] GURBUZ O,ROUSEFFJ M,ROUSEFF R L. Comparison of aroma volatiles in commercial Merlot and Cabernet Sauvignon wines using gas chromatography-olfactometry and gas chromatography-mass spectrometry[J]. Journal of Agricultural and Food Chemistry,2006,54(11):3990-3996.
[23] AND W F,QIAN M C. Characterization of aroma compounds of Chinese “Wuliangye” and “Jiannanchun” liquors by aroma extract dilution analysis[J]. Journal of Agricultural and Food Chemistry,2006,54(7):2695-2704.
[24] NIU Y W,ZHANG X M,XIAO Z B,et al. Characterization of odor-active compounds of various cherry wines by gas chromatography-mass spectrometry,gas chromatography-olfactometry and their correlation with sensory attributes[J]. Journal of Chromatography B,2011,879(23):2287-2293.
[25] FUHRMANN E,GROSCH W. Character impact odorants of the apple cultivars Elstar and Cox Orange[J]. Food/Nahrung,2002,46(3):187-193.
[26] CHOI H S. Character impact odorants of Citrus Hallabong[(C. unshiu Marcov×C. sinensis Osbeck)×C. reticulata Blanco]cold-pressed peel oil[J]. Journal of Agricultural and Food Chemistry,2003,51(9):2687-2692.
[27] PEINADO R A,MORENO J A,MUNOZ D,et al. Gas chromatographic quantification of major volatile compounds and polyols in wine by direct injection[J]. Journal of Agricultural and Food Chemistry,2004,52(21):6389-6393.
[28] GARCIA-CARPINTERO E G,SANCHEZ-PALOMO E. Volatile and sensory characterization of red wines from cv. Moravia Agria minority grape variety cultivated in La Mancha region over five consecutive vintages[J]. Food Research International,2011,44(5):1549-1560.
[29] GUTH H. Quantitation and sensory studies of character impact odorants of different white wine varieties[J]. Journal of Agricultural and Food Chemistry,1997,45(8):3027-3032.
[30] PERESTRELO R,FERNANDES A. Analytical characterization of the aroma of Tinta Negra Mole red wine:Identification of the main odorants compounds[J]. Analytica Chimica Acta,2006,563(1):154-164.
[31] QUIJANO C E,SALAMANCA G,PINO J A. Aroma volatile constituents of Colombian varieties of mango(Mangifera indica L.)[J]. Flavour and Fragrance Journal,2007,22(5):401-406.
[32] LI H,TAO Y S,KANG W H,et al. Wine aroma analytical investigation progress on GC[J]. Journal of Food Science and Biotechnology,2006(1):20-20.
[33] NOGUEROL-PATO R,GONZALEZ-RODRIGUEZ R M. Influence of tebuconazole residues on the aroma composition of Mencía red wines[J]. Food Chemistry,2011,124(4):1525-1532.
[34] CHISHOLM M G,WILSON M A,GASKEY G M,Characterization of aroma volatiles in key lime essential oils(Citrus aurantifolia Swingle)[J]. Flavour and Fragrance Journal,2003,18(2):106-115.
[35] FERREIRA V,AZNAR M,LOPEZ R,et al. Quantitative gas chromatography-olfactometry carried out at different dilutions of an extract. Key differences in the odor profiles of four high-quality Spanish aged red wines[J]. Journal of Agricultural and Food Chemistry,2001,49(10):4818-4824.