HS-SPME-GC-MS/O联用分析酱油中的香气活性化合物

通过顶空-固相微萃取(HS-SPME)和气相色谱-质谱/嗅闻技术(GC-MS/O)联用,研究酱油的香气组成。GC-MS共分离鉴定出酱油中挥发性化合物109种,其中醇类物质含量最高,占总挥发性化合物的75.82%,其次是醛类、酯类、酸类和呋喃(酮)类等。采用GC-MS/O鉴定出39种为香气活性物质,其中,3-甲基丁醛,2-甲基丁醛,2-甲基丙醛,3-甲硫基丙醛,乙醇,4-羟基-2-乙基-5-甲基-3(2H)-呋喃酮(HEMF),苯乙醛,1-辛烯-3-醇,2-甲基丙酸乙酯,2-甲基丁醇,3-甲基丁醇,二甲基三硫,4-羟基-2,5-二甲基-3(2H)-呋喃酮(HDMF),乙酸和愈创木酚是OAV值大于20且香气强度评分大于2的关键香气活性物质,它们为酱油整体香味贡献麦芽香,烤土豆香味,醇香,焦糖香,花香味,蘑菇香味,果香味,洋葱味,烟熏味等,综合组成了酱油独特的发酵豆制品风味。     

面粉对发酵酱油品质的影响研究

在工业化生产条件下,以面粉和小麦粉混合发酵酱油(FWSS)和纯小麦粉发酵酱油(WSS)为研究对象,通过测定其理化指标、氨基酸组成以及挥发性化合物组成,结合感官评价结果分析两类酱油风味品质差异的形成原因。结果显示：除总酸外,其他理化指标均无显著性差异;FWSS酱油中大部分氨基酸含量均高于WSS酱油,差异较大的为谷氨酸含量(FWSS=21.11%,WSS=20.35%)。挥发性化合物测定结果显示FWSS酱油挥发性化合物相对含量较高,其中酱油中常见的香气活性物质4-羟基-5-乙基-2-甲基-3(2H)-呋喃酮(HEMF,焦糖香),4-乙基愈创木酚(4-EG,烟熏香)含量差异较为明显,与感官评价结果中FWSS酱油其烟熏香味、焦糖香味更加丰富的结果一致。表明在工业生产中,加入40%的面粉替代小麦粉发酵酱油(FWSS),可明显降低酱油中总酸含量(FWSS的总酸含量为1.15 g/100 g,WSS的总酸含量为1.24 g/100 g),提高酱油的香气饱满度和滋味特征。本研究可为高盐稀态酱油的风味品质提升提供理论指导。     

采用GC-O-MS结合香气活力值分析兰陵美酒香气活性组分特征

采用感官为导向的风味化学分析方法对兰陵美酒的香气活性组分特征进行解析。首先采用描述性感官分析技术构建了兰陵美酒香气轮廓图,结果显示兰陵美酒具有花果香、醇香、焦糖和酱香等突出的香气特征。进一步采用顶空固相微萃取(headspace solid phase microextraction,HS-SPME)和液液萃取(liquid-liquid extraction,LLE)前处理方法结合气相色谱-嗅闻-质谱联用仪(gas chromatography-olfactometry-mass spectrometry,GC-OMS)在兰陵美酒中共解析出酯类、醇类、有机酸类、酚类、醛酮类等50种香气活性化合物。基于香气活性组分的精确定量和香气活力值(odor activity value,OAV)分析发现乙酸乙酯、丁酸乙酯、戊酸乙酯、己酸乙酯、辛酸乙酯、异戊醇、苯乙醇、苯甲醛、苯乙醛、香兰素、γ-壬内酯和4-乙烯基愈创木酚等香气化合物是构成兰陵美酒香气特征的关键香气化合物。     

气相色谱-嗅闻/质谱联用分析酵母菌发酵酱油中香气物质

酱油香气物质的形成与酵母菌的代谢息息相关,本文旨在研究酵母菌对发酵酱油中香气物质形成与含量的影响。采用固相微萃取(SPME)结合气相色谱-嗅闻-质谱(GC-O/MS)联用技术分别对不加酵母菌、加AY酵母菌以及加入T酵母菌发酵制得酱油中的香气物质进行检测分析。结果显示:加入酵母菌的酱油中形成的各类香气物质更加丰富,其中AY型鲁氏酵母菌能够产生更多种类的酯类(11种)及醇类(12种)物质;T型鲁氏酵母菌有助于醛类(7种)物质的形成。且AY型鲁氏酵母菌在酱油酿造过程中产生的酯类(155.19 μg/L)、呋喃酮类(68.53 μg/L)、醛类(86.46 μg/L)等物质的含量更高,T型鲁氏酵母菌的产醇类(1260.64 μg/L)物质能力则更加优越。通过对酱油样品中OAV的计算,发现,AY酵母菌酿造酱油中的4-羟基-2-甲基-5-乙基-3(2H)-呋喃酮(HEMF),2/3-甲基丁醛、及苯乙醛的OAV高于其他样品的OAV值,T型鲁氏酵母菌的1-辛烯-3-醇及3-甲硫基丙醛的OAV值高于其他样品的OAV值。将OAV值与PCA结合分析,可以看出,AY型鲁氏酵母菌发酵酱油的香气优势明显,并且T型鲁氏酵母菌发酵酱油以熟土豆气味为主,并伴有蘑菇香气;AY型鲁氏酵母菌发酵酱油以甜香香气为主,并伴有麦芽香气。综上,AY型鲁氏酵母菌的整体产香优于T型鲁氏酵母菌的产香效果。     

SDE和HS-SPME法与GC-MS/O联用分析阳江豆豉的香气活性化合物

采用同时蒸馏萃取法(SDE)和顶空-固相微萃取法(HS-SPME)结合气相色谱-质谱/嗅闻检测技术(GC-MS/O)深入研究阳江豆豉的香气成分,共鉴定出挥发性化合物174种。SDE法对高分子量、低挥发性物质,如呋喃酮、吡喃酮等,有良好的萃取效果;而HS-SPME法能萃取更多的高挥发性化合物,如小分子的酸和酯类。通过GC-O技术在两种方法的萃取物中共嗅闻到46个香气活性区域。其中9种共有化合物(2/3-甲基丁醛、2/3-甲基丁酸、3-甲硫基丙醛、苯乙醛、愈创木酚、3-羟基-2-甲基-4H-吡喃-4-酮和苯乙醇),以及香气强度较高(评分大于2.5分)的单方法检出化合物:SDE法4种(3-羟基-4,5-二甲基-2(5H)-呋喃酮、2-乙酰基-1-吡咯啉、2-丙烯基-3-甲基吡嗪和4-羟基-2,5-二甲基-3(2H)-呋喃酮)、SPME法1种(1-辛烯-3-醇),是阳江豆豉中的关键香气活性物质,对麦芽香、酸奶酪香、烤土豆香、花香、烟熏香、焦糖香和烤香等有贡献。     

β-葡萄糖苷酶和α-L-鼠李糖苷酶对速溶绿茶粉水溶液香气的影响

速溶茶粉是重要的茶叶深加工产品,酶工程技术是改良速溶茶粉及其加工产品风味的重要途径。为了解β-葡萄糖苷酶和α-L-鼠李糖苷酶对速溶绿茶粉水溶液香气的影响,运用感官检验、气相色谱-质谱联用(GC-MS)、香气强度值(OAV)方法对酶处理前后的速溶绿茶粉水溶液进行分析。感官评价和GC-MS分析发现,速溶绿茶粉水溶液主要呈焦糖香和甜香;β-葡萄糖苷酶处理后花香、甜香和青草香显著增强,焦糖香降低,顺式-3-己烯醇、香叶醇、己醇、水杨酸甲酯和苯甲醛这些重要的挥发性化合物的含量显著增加;α-L-鼠李糖苷酶处理后速溶绿茶粉水溶液中焦糖香显著降低;两种酶结合处理后青草香和甜香进一步增强,顺式-3-己烯醇和水杨酸甲酯的含量进一步增加。OAV分析发现,速溶绿茶粉水溶液主要香气贡献成分为3-甲基丁醛、2-甲基丁醛、2-乙基呋喃、柠檬烯和壬醛;β-葡萄糖苷酶处理后主要香气贡献成分为顺式-3-己烯醇、水杨酸甲酯、香叶醇和癸醛;α-L-鼠李糖苷酶对速溶绿茶粉水溶液各成分的OAV值没有显著影响;两种酶联合处理可进一步增强顺式-3-己烯醇的OAV值。以上研究表明β-葡萄糖苷酶可显著改变速溶绿茶粉水溶液的香气,且α-L-鼠李糖苷酶与β-葡萄糖苷酶对增强速溶绿茶粉水溶液的青草香具有协同增效作用,为改良速溶茶粉加工食品的风味提供了技术参考。     

顶空固相微萃取-气相色谱-质谱联用分析辣椒油中的风味物质

不同条件煎制制备北京红辣椒油,对其进行感官评价并结合顶空-固相微萃取（HS-SPME）和气相色谱-质谱联用（GC-MS）技术研究辣椒油的风味物质组成。结果表明：不同煎制程度显著地影响辣椒油风味,130 ℃油温下煎制10 min的辣椒油（LJY-4）风味最佳。不同煎制程度显著地影响辣椒油所含风味化合物的种类和峰面积比,尤其是酮类、呋喃类、萜烯类及烯醛类等化合物的峰面积比。LJY-4除具有辣椒粉的特征风味化合物外,还富含酮、呋喃等焦甜型风味化合物,其中活性值（OAV）大于20的化合物有9种,分别为2,3-戊二酮、(E,E)-2,4-壬二烯醛、3-甲基丁醛、2-甲基丁醛、2-甲基丙醛、二甲基硫、4-羟基-2,5-二甲基-3(2H)呋喃酮（HDMF）、乙酸和1-辛烯-3-醇,它们为辣椒油贡献了焦甜香、酯香、麦芽香、果香和豆香等,组成了辣椒油独特的风味品质。     

HS-SPME-GC-MS结合感官评价分析金种子馥合香白酒的风味成分

为明确金种子馥合香白酒的特征性风味成分及其呈香贡献、感官特征等,为馥合香白酒的质量分级、储存与勾调等提供参考依据。采用顶空固相微萃取(headspace solid phase microextraction,HS-SPME)和GC-MS分析等方法,结合香气活性值(odor activity value,OAV)分析与感官评价,对馥合香原酒特征性风味成分进行剖析,并比较不同质量等级馥合香原酒的风味差异。结果表明,特级酒中检测到酯类42种、醇类7种、酸类5种、醛类2种、呋喃类1种、含硫化合物1种、烷烃类2种;优级酒中检测到酯类33种、醇类7种、酸类4种、醛类2种、呋喃类2种。OAV分析表明,特级酒与优级酒中至少含有18种物质的OAV≥1,对馥合香白酒的香气有主要贡献;感官评价表明,特级酒与优级酒在"酯香、焦香、窖香"等方面均表现突出。棕榈酸乙酯的相对含量较高是馥合香白酒区别于其他白酒的重要特征,二甲基三硫、糠醛、3-糠醛、3-呋喃甲醇、苯乙醇等特殊风味物质对酒体呈"馥香"特征具有重要作用。     

兼香型年份酒中香味物质的分析

通过单因素试验优化顶空固相微萃取（HS-SPME）条件,并结合气相色谱-质谱（GC-MS）技术研究兼香型年份酒中香味物质成分含量及差异。结果表明,最佳HS-SPME萃取条件为酒样酒精度14%vol,萃取温度40 ℃,萃取时间30 min,解吸时间5 min。GC-MS法共鉴定出67种挥发性风味物质,包括50种酯类,3种醇类,5种酸类,1种芳香族化合物,1种含硫化合物,2种呋喃类,3种酮类和2种醛类。酯类、醇类、酸类和呋喃类总含量随贮藏年份增长呈现上升趋势,醛类和酮类总含量变化规律不明显。经香气活度值（OAV）分析,确定出22种（OAV＞1）成分对白酒香味有贡献,其中有9种（OAV＞10）为重要香气成分,酯类为白酒香气的主要贡献物质。     

脂质对凡纳滨对虾热风干制品香气特性的影响

为研究脂质对凡纳滨对虾热风干制品香气特性的影响,通过有机试剂去除虾体中的甘油三酯或磷脂,采用气相色谱-质谱联用技术和感官评价分析脂质对虾干制品香气特性的影响,以气味活性值(odor activity value,OAV)为指标,筛选香气活性化合物,同时采用偏最小二乘回归法(partial least squares regression,PLSR)分析挥发性化合物与感官属性之间的相关性。结果表明:去除甘油三酯对虾干制品整体香气影响较小,烤香味、肉香味和腥味的感官评分稍有减弱,而去除磷脂对主要香气特征有很大影响,烤香味、肉香味、腥味、焦糖香和甜香味的感官评分均大幅度降低;虾干制品中鉴定出16种香气活性化合物,吡嗪类、胺类、杂环类、醛类是其主要成分,其中3-乙基-2,5-二甲基吡嗪、2,5-二甲基吡嗪、三甲胺、3-(甲硫基)丙醛是贡献最大的4种物质;去除甘油三酯和磷脂后,吡嗪类、胺类、杂环类、醛类的OAV值显著下降,而去除磷脂后下降幅度更大,且在去磷脂虾干制品中2-戊基呋喃和3-(甲硫基)丙醛未检出;PLSR结果表明,18种香气活性化合物与感官属性具有较好的相关性。综上所述,脂质对虾干制品整体香气有较大影响,而磷脂对香气特性的作用远大于甘油三酯。该研究为虾类特征香气的形成机制研究提供了理论参考。     

Comparison on aroma compounds in Chinese soy sauce and strong aroma type liquors by gas chromatography–olfactometry,chemical quantitative and odor activity values analysis

In order to elucidate the differences on aroma compounds in Chinese liquors with different aroma styles and the reasons, aroma compounds of Xijiu in soy sauce aroma and strong aroma type were investigated in the research. By gas chromatography–olfactometry (GC–O), aroma compounds in Chinese liquor were chosen for quantitative and odor activity value (OAV) analysis. Ethyl hexanoate, butanoic acid, 3-methylbutanoic acid, hexanoic acid and dimethyl trisulfide were considered to be the most powerful odorants in both liquor samples (aroma intensity ≥3.5) by GC–O. As important aroma compounds (OAV ≥10) in the liquors, ethyl propanoate, ethyl 2-methylpropanoate and 1-propanol were considered with much higher OAVs in soy sauce aroma type liquor, while OAVs of ethyl pentanoate, ethyl hexanoate, ethyl heptanoate, ethyl octanoate, ethyl lactate, hexyl acetate, butyl hexanoate, hexyl hexanoate and hexanoic acid were far lower in strong aroma type liquor. The OAV of ethyl hexanoate in strong aroma type liquor exceeded 50,000, which explained the reason why strong aroma liquor was considered with prominent fruity aroma. The odor differences between the liquors were mainly caused by the manufacturing practices.     

Reducing the Influence of the Thermally Induced Reactions on the Determination of Aroma-Active Compounds in Soy Sauce Using SDE and GC-MS/O

A method based on simultaneous distillation extraction (SDE) coupled with gas chromatography–mass spectrometry/olfactometry (GC-MS/O) was developed for the analysis of volatile profiles in soy sauce. Its optimum operating conditions were as follows: 100 mL soy sauce plus 100 mL saturated brine; 2 h extraction using 50 mL dichloromethane. Eighty-eight volatile compounds were identified. Of these, 26 aroma-active compounds were detected by GC-O including 3-(methylthio)propanal, 2-methoxy-4-vinylphenol, 2-methoxyphenol, 2-methylbutanoic acid, 2,3-butanedione, phenylacetaldehyde, 2-ethyl-6-methylpyrazine, 3-methylbutanal, 2-methylbutanal, 3-methyl-1-butanol, and 2-methyl-1-butanol (which occurred at a high odor intensity in both high-salt liquid-state fermentation soy sauce (HLFSS) and low-salt solid-state fermentation soy sauce (LSFSS). SDE analysis of the odorless soy sauce indicated 12 volatiles (mainly Strecker aldehydes and α-dicarbonyl compounds). Thus, the proportions of these compounds (1.94–54.07 %) shown in previous GC-MS results could result from thermal degradation of non-volatile compounds in soy sauce. Especially, the contribution of 3-methylbutanal, 2-methylbutanal, phenylacetaldehyde, 3-(methylthio)propanal, and 2,3-butanedione to the aroma of soy sauce could be overestimated by conventional SDE-GC-O. With a full consideration of such limitations, this study will improve the application of SDE on aroma analysis of complex food matrix.     

清香型志都五谷酒关键香气成分分析

通过液液萃取和顶空固相微萃取技术,结合气相色谱-质谱-嗅闻联用仪分析一种清香型志都五谷酒香气活性成分.通过香气提取稀释分析法共得到40种香气物质,且香气稀释(flavor dilution,FD)因子最大的为异丁酸、月桂酸乙酯、愈创木酚和2-苯乙醇(FD＞4 096),通过质谱、保留指数、香气特征和标准品比对共定性出3...     

高盐稀态酿造酱油中香气活性成分在灭菌前后的变化

为了确定高盐稀态酿造酱油中香气活性成分在灭菌前后的变化情况,采用液液萃取结合溶剂辅助风味成分蒸发法提取灭菌前后酱油样品中的挥发性成分,采用气相色谱-嗅觉检测器联用仪对提取物进行分析,从中检测到24?种香气活性物质,经过与标准品的香气特征、质谱、保留指数进行比对,对其结构进行确定。以2-辛醇为内标,采用内标标准曲线的方法对其进行定量;根据定量结果和香气阈值,计算香气活性值。结果表明,导致灭菌前后香气差别的主要原因为3-甲硫基丙醛、麦芽酚、5-乙基-4-羟基-2-甲基-3(2H)-呋喃酮、4-羟基-2,5-二甲基-3(2H)呋喃酮、己醛、香兰素、愈创木酚和4-乙基愈创木酚质量浓度的变化,此结果与香气评价的结果一致。     

基于GC-O、OAV及Feller加和模型对酱香型习酒特征香气成分的分析

通过气相色谱-质谱联用仪、气相色谱硫磷检测器研究3种酱香型习酒(习酒蓝、习酒印象贵州、习酒银质)中的挥发性香气成分,分别鉴定出99、96、98种香气成分,其中各包含12种含硫化合物.基于气相色谱嗅闻仪和香气活性值(odor activity value,OAV)方法,表明己酸乙酯(OAV:1720～1992)、丁酸乙酯...     

应用GC-O和GC-MS分析酱香型习酒中挥发性香气成分

利用液液萃取法(LLE)提取酱香型习酒中的香气化合物,按照酸碱性将萃取组分分离,获得酸性/水溶性、中性、碱性三个组分,通过气相色谱-闻香法(GC-O)结合气相色谱-质谱(GC-MS)分别进行香气成分分析。在具有典型酱香特征的习酒中共检测出72种香气化合物,其中酸性组分29种,中性组分43种,碱性组分22种,14种香气化合物在两种或两种以上组分中均可检测到。研究发现酱香型习酒中主要的香气物质是酯类、醇类、挥发性有机酸、呋喃类、芳香族类、酚类、醛酮类、吡嗪类以及含硫化合物等。香气强度较大的物质有丁酸乙酯、己酸乙酯、1-丙醇、3-甲基丁醇、乙酸、3-甲基丁酸、糠醛、四甲基吡嗪和二甲基三硫,这些物质对酱香型习酒的风味贡献较大。     

Characterization of the differences in the aroma of cherry wines from different price segments using gas chromatography–mass spectrometry,odor activity values,sensory analysis,and aroma reconstitution

The aroma composition, aroma-active compounds, and sensory attributions of cherry wines from three different price segments were investigated. A total of 48 aroma compounds were identified and quantified using headspace solid-phase microextraction (HS-SPME)/gas chromatography–mass spectrometry (GC–MS), among which 23 aroma compounds were further screened out as important odorants based on their odor activity values (OAVs); then, the previously mentioned 23 volatiles were correlated to sensory attributes using partial least-squares regression (PLSR). The result indicates that the differently priced wines were associated with different compounds and aroma attributions. Finally, aroma reconstitution was performed by mixing odor-active aroma compounds (OAVs>1) on the basis of their measured concentrations in the original sample. The result indicated that the aroma profile of the reconstituted sample was similar to that of the original sample.     

Characterization of potent odorants in Thai chempedak fruit (Artocarpus integer Merr.), an exotic fruit of Southeast Asia

Chempedak (Artocarpus integer Merr.) is a native fruit in Malaysia, Indonesia and southern Thailand, and like jackfruit, belongs to the Moraceae family. The characteristic aroma-active components of two chempedak cultivars, Tongtapan and Sainumpung, grown in southern Thailand were analyzed by aroma extract dilution analysis (AEDA) combined with gas chromatography–olfactometry (GC–O) and gas chromatography–mass spectrometry (GC–MS). The predominant odorants [with flavor dilution (FD) factors > 9] in both cultivars were 4-hydroxy-2,5-dimethyl-3(2H)-furanone (burnt sugar, sweet), 3-methylbutanal (dark chocolate), methional (cooked potato-like), and 2-acetyl-1-pyrroline (popcorn, jasmine), while ethyl 3-methylbutanoate (fruity) was predominant only in Tongtapan cultivar. Selected positively identified aroma-active compounds were further quantified using stable isotope dilution assays (SIDA) combined with GC–MS. On the basic of the quantitative data and odor thresholds, odor activity values (OAV) were determined. Aroma recombination models and omission models were constructed for both cultivars based on concentrations of odorants with high OAVs and then validated and characterized by sensory studies. Complete aroma recombination models of both chempedak cultivars were reconstituted and characterized by comparison with authentic chempedak fruits. Omission studies were performed to verify the significance of character-impact odorants in both chempedak cultivars. Based on sensory evaluation, 3-methylbutanal, octanal, and 2-acetyl-1-pyrroline were found to be important odorants in the overall aromas of both cultivars, while ethyl 3-methylbutanoate was an additional key odorant in the aroma of the Tongtapan cultivar.