Changes in Volatile Compounds of Chinese Luzhou‐Flavor Liquor during the Fermentation and Distillation Process

The aim of this study was to investigate the dynamic of volatile compounds in the Zaopei during the fermentation and distillation process by headspace solid‐phase microextraction‐gas chromatography mass spectrometry (HS‐SPME‐GCMS). Physicochemical properties analysis of Zaopei (fermented grains [FG], fermented grains mixed with sorghum [FGS], streamed grains [SG], and streamed grains mixed with Daqu [SGD]) showed distinct changes. A total number of 66 volatile compounds in the Zaopei were identified, in which butanoic acid, hexanoic acid, ethyl hexanoate, ethyl lactate, ethyl octanoate, hexyl hexanoate, ethyl hydrocinnamate, ethyl oleate, ethyl hexadecanoate, and ethyl linoleate were considered to be the dominant compounds due to their high concentrations. FG had the highest volatile compounds (112.43 mg/kg), which significantly decreased by 17.05% in the FGS, 67.12% in the SG, and 73.75% in the SGD. Furthermore, about 61.49% of volatile compounds of FGS were evaporated into raw liquor, whereas head, heart, and tail liquor accounted for 29.84%, 39.49%, and 30.67%, respectively. Each volatile class generally presented a decreasing trend, except for furans. Especially, the percentage of esters was 55.51% to 67.41% in the Zaopei, and reached 92.60% to 97.67% in the raw liquor. Principal component analysis based ordination of volatile compounds data segregated FGS and SGD samples. In addition, radar diagrams of the odor activity values suggested that intense flavor of fruit was weakened most from FG to SGD.     

汾酒酒醅发酵过程中香气成分的变化规律

采用气相色谱(GC)和气相色谱- 质谱(GC-MS)分析方法,跟踪考查汾酒发酵过程酒醅中各类香气成分的动态变化规律及其相互关系。结果表明：酒醅中大多数香气成分的含量在正常发酵期内随发酵进行呈上升趋势,发酵前期增长较快,发酵中后期增长趋于缓慢;但某些香气成分的含量及量比关系与白酒产品相比却存在一定的差异;汾酒夏季生产没有必要延长发酵期,适当缩短发酵时间可能更好。通过控制发酵条件或利用现代生物技术增乙降乳,进一步探明白酒蒸馏机理改善蒸馏条件,是提高白酒质量的重要措施。     

Effects of different distillation patterns on main compounds of Chinese Luzhou‐flavour raw liquors

This study aimed to investigate the effects of different distillation patterns on main compounds of Chinese Luzhou‐flavour liquor. Results showed that more volatiles of raw liquor might originate from fresh grains for a newly constructed pit. A modest (p  = 0.05) increase in the total amount of volatiles was found in the heart liquor from fermented grains added to fresh grains and rice hulls to distillate (AG pattern), reaching a maximum value of 1012.22 mg/L. The percentage of esters in the AG pattern ranged from 81.22 to >95.03% compared with samples from fermented grains only added to rice hulls to distillate (NG pattern). Acids in the heart liquor obtained by the AG pattern were higher than those for NG, but the corresponding proportion was opposite. Alcohols were detected at ~1.62% in NG pattern but were 1.42% in AG. Cyanide and ethyl carbamate content in the head liquor were far higher than those in the heart and tail liquor. In particular, cyanide content dramatically increased after adding fresh grains during the distillation process. Copyright © 2017 The Institute of Brewing & Distilling     

古井贡酒酒醅挥发性香气成分的GC-MS与GC-O分析

应用溶剂辅助风味蒸发法结合气相色谱-质谱联用技术、气相色谱-嗅闻技术对古井贡酒酒醅中的挥发性香气成分进行分析。经计算保留指数并结合标准品比对,共定性出148 种挥发性香气成分,其中有21 种香气强度较高的化合物。应用内标法并结合相关阈值对这21 种嗅闻强度高、持续时间长的重要风味组分进行定量分析及香气活度值（odor activity value,OAV）分析,比较它们对酒醅整体香气的贡献程度,其中香气贡献度最高的4 种物质分别为己酸乙酯（OAV=2 817）、辛酸乙酯（OAV=534）、丁酸乙酯（OAV=519）、乙酸-3-甲基丁酯（OAV=137）,酒醅中其他较重要的香气化合物为癸酸乙酯、丁酸、乳酸乙酯、苯乙酸乙酯、苯丙酸乙酯、乙酸苯乙酯、己酸、2,3-丁二醇、乙酸、丙酸和苯乙醇。     

浓香型白酒蒸馏过程中挥发性风味物质的变化规律

建立直接进样结合气相色谱-质谱法(Gas Chromatography-Mass Spectrometry,GC-MS),分别对100年、300年窖龄窖池的酒醅在蒸馏过程中挥发性物质变化规律进行研究,准确定性浓香型白酒中70种典型挥发性化合物,包括酯类39种,醇类14种,酸类6种、烷烃类3种,醛酮类5种,其他3种;其中46种化合物属于两个不同窖龄窖池酿造白酒中的共有成分。同时,在蒸馏过程中,丙二醇、2,3-丁二醇、乙酸、苯乙酸乙酯、十四酸乙酯、棕榈酸乙酯、油酸乙酯和亚油酸乙酯均呈上升的趋势;辛酸乙酯、丁酸己酯、己酸丁酯、庚酸乙酯、乙酸己酯、丁酸丁酯、戊酸乙酯、乙酸异戊酯、正丁醇、戊醇、2-甲基丁醇呈下降的趋势;己酸、丁酸、己醇、辛醇均增加。本研究初步阐释了不同窖龄馏分酒中风味物质的含量差异,发掘了不同馏分酒蒸馏过程中风味物质含量与流酒时间之间的关系,为酒企科学蒸馏、质量摘酒和分级贮存提供了科学数据。     

不同品种小麦发酵面团及馒头挥发性物质的差异分析

目的 研究分析小麦品种对面制品挥发性物质的影响。方法 采用顶空固相微萃取-气相色谱-质谱法,对5个品种小麦粉的发酵面团及馒头挥发性物质进行分析,结合相对气味活度值、主成分分析确定样品的关键特征挥发性物质。结果 5个品种小麦的发酵面团及馒头共检测到106种化合物,其中有以醇类、醛类为主的32种共同物质;发酵面团和馒头分别测得75和95种化合物,各自主要挥发性物质具有明显差异;由蒸制引起的醇类、部分酯类的大量损失和醛类、杂环类的显著增加可能会导致两组样品风味出现差异的关键原因;己酸乙酯等3种物质是发酵面团关键特征挥发性物质;反-2-壬烯醛等3种物质是馒头关键特征挥发物质;异戊醇等16种差异性标志物可能是引起5个品种小麦发酵面团和馒头挥发性物质差异的主要物质。结论 通过对挥发性物质的分析,结合香气评价方法及多元统计分析方法阐明了5个品种小麦发酵面团及馒头挥发性物质的差异性,为细分原料加工适应性提供了参考。     

同时蒸馏萃取结合GC-MS分析酿酒五粮原料蒸煮香气成分

采用同时蒸馏萃取结合气相色谱-质谱分别对浓香型白酒生产使用的五粮（高粱、小麦、玉米、糯米、大米）以及按生产比例制备的混合粮食样品的蒸煮香气中挥发性成分进行分析。结果表明,5种单粮中共鉴定出153种化合物;高粱、小麦、玉米、糯米、大米中分别鉴定出108、93、93、66、66种化合物,其中鉴定出较多数量的醛类、醇类、酮类、芳香类、酯类等化合物。采用双柱定性,在混合粮食样品中共鉴定出140种化合物。采用气相色谱-嗅闻-质谱联用法在混合粮食样品中共鉴定出29种香气活性化合物,结合香气提取稀释分析和香气活性值评价不同化合物对粮食蒸煮整体风味的影响。经计算,苄硫醇、(E,E)-2,4-癸二烯醛、(E)-2-壬烯醛、壬醛、己醛、辛醛、(E)-2-辛烯醛、(E,Z)-2,6-壬二烯醛、正庚醇、(E)-2-癸烯醛、(E,E)-2,4-壬二烯醛、苯乙醛、4-乙基愈创木酚、己酸乙酯、香叶基丙酮、辛酸乙酯、香草醛17种化合物的香气活性值不低于1,被认为是对粮香有贡献的重要风味化合物,其中苄硫醇和(E,Z)-2,6-壬二烯醛首次在蒸煮粮食香气中被鉴定。     

Evolution of aroma compounds of murtilla fruits (Ugni molinae Turcz) during storage

BACKGROUND: ‘Murtilla’, ‘mutilla’ or ‘murta’ (Ugni molinae Turcz) is a native Chilean species that produces a small berry fruit with a special aroma, whose volatile compounds have not yet been identified. The fruit may be consumed raw and also as jams, juice, canned products, confections and liquor. RESULTS: At the beginning and end of the storage, 24 volatile compounds were identified in murtilla fruit aroma and the concentration of these compounds in murtilla fruit ranged from 1.2 to 250.5 µg kg^?1 fresh weight. Methyl 2‐methyl butanoate, ethyl butanoate, ethyl 2‐methyl butanoate, methyl hexanoate, ethyl hexanoate, methyl benzoate and ethyl benzoate were the major components, all of which have been reported as potent odors in other aromatic fruits. Based on estimated odor activity value, the most potent compound in the murtilla fruit aroma were ethyl hexanoate and 4‐methoxy‐2,5‐dimethyl‐furan‐3‐one. The statistical analysis showed that the storage produced a distinct effect on the same volatile compounds released from the murtilla ecotypes. CONCLUSION: The volatile compounds identified in murtilla fruit aroma, which may be described as fruity, sweet and floral, have been found in other aromatic fruits. Concerning the aroma, the murtilla fruit from ecotype 19‐1 was shown to be the best in cooled storage. Copyright © 2007 Society of Chemical Industry     

甑桶醅层高度及结构设计对蒸馏效率及酒质的影响研究

探索浓香型白酒甑桶醅层高度及结构的设计对蒸馏效率及酒质的影响。研究表明,单位质量糟醅的蒸馏效率随醅层高度的增加逐渐升高。醅层高度相同时,小直径的甑桶蒸馏效率高于大直径甑桶;甑桶的高径比较大时有利于强化蒸馏,符合增己降乳的原则,可有效提高蒸馏效率与酒质。     

Odour‐active compounds in pineapple (Ananas comosus [L.] Merril cv. Red Spanish)

Application of solid‐phase microextraction, simultaneous distillation–extraction and liquid–liquid extraction combined with GC‐FID, GC‐MS, aroma extract dilution analysis, and odour activity value was used to analyse volatile compounds from pineapple (Ananas comosus [L.] Merril cv. Red Spanish) and to estimate the most odour‐active compounds. The analyses led to the identification of ninety‐four compounds, seventy‐two of them were positively identified. Twenty odorants were considered as odour‐active compounds, from which ethyl 2‐methylbutanoate, 2,5‐dimethyl‐4‐hydroxy‐3(2H)‐furanone, 1‐(E,Z,Z)‐3,5,8‐undecatetraene, ethyl 3‐(methylthio)propanoate, 1‐(E,Z)‐3,5‐undecatriene, ethyl hexanoate and methyl hexanoate were the most odour contributors and contribute to the typical pineapple aroma, while the others are responsible for fruity and sweet odour notes.     

不同来源浓香型酒醅的挥发性成分差异分析

为研究不同来源浓香型酒醅的挥发性成分差异，采用顶空-气相色谱质谱联用（HS-GC-MS）法对酒醅挥发性成分进行测定，结合主坐标分析、t检验方法比较不同来源出窖/入窖酒醅挥发性成分的差异，以及入窖酒醅挥发性成分差异对出窖酒醅挥发性成分的影响。结果表明，不同来源的出窖酒醅中共检出41种挥发性成分，其多样性、香气成分类别上具有相似性；不同来源入窖酒醅中共检出27种挥发性成分，其多样性和香气成分类别上都存在差异。入窖酒醅S_2在乙醇、乳酸乙酯和乙酸含量显著高于入窖酒醅S_4（P＜0.05），其他相对含量＞1%挥发性成分显著低于S_4（P＜0.05）。差异性分析结果表明，不同来源的入窖酒醅挥发性成分的差异不会对出窖酒醅的挥发性成分产生显著影响。     

白酒组分与质量的关系

对白酒中的微量成分复杂的成因进行了分析。浓香型白酒的香气成分主要来自于：（1）粮食原料的香气成分；（2）酒曲的曲香成分；（3）糟酷中的原料、辅料与发酵微生物的代谢物构成的糟香成分；（4）窖泥微生物产生的复杂代谢产物，经蒸馏过程带入酒中成分，为浓香型酒特有的呈香呈味物质的体现。酸、酯、醇、醛是主要物质基础，还有其他复杂成分协同的作用产生窖香成分；（5）陈味成分。是有别于窖香，比窖香更好的一种特有香味成分。（陶然）     

Analysis of Volatile Flavor Components in Steamed Rangia Clam by Dynamic Headspace Sampling and Simultaneous Distillation and Extraction

The volatile flavor components of steamed rangia clam (Rangia cuneata) were extracted by dynamic headspace sampling (DHS) and simultaneous distillation/extraction (SDE) techniques, and analyzed by gas chromatography/mass spectrometry (GC/MS) and GC-coupled aroma perception. Twenty-two heterocyclic aroma compounds were identified. Volatile flavor compounds in other chemical classes, such as aldehydes, alcohols, ketones, and terpenes, also were identified. The unique clam aromas were contributed by a combination of S-, and N- containing compounds and ketones. In general, sampling methods (DHS and SDE) complemented each other in compounds detected in the sample. However, SDE gave more information on characteristic steamed clam flavors.     

Analysis of characteristic aroma of fungal fermented Fuzhuan brick‐tea by gas chromatography/mass spectrophotometry

Fuzhuan brick‐tea is a popular fermented Chinese dark tea because of its typical fungal aroma. Fungal growth during the production process is the key step in achieving the unique colour, aroma and taste of Fuzhuan brick‐tea. To further understand the generation of the characteristic aroma, changes in the main volatile compounds of Fuzhuan brick‐tea during the fungal growth stage were studied by gas chromatography/mass spectrophotometry. The results showed that the content of volatile compounds, especially aldehyde compounds with stale aroma such as (E)‐2‐pentenal, (E)‐2‐hexenal, 1‐penten‐3‐ol, (E, E)‐2,4‐heptadienal and (E, Z)‐2,4‐heptadienal, increased significantly in fermented tea samples. The concentration of terpene alcohols with flower aroma also increased notably during the fermentation process. The compounds with stale and flower aromas in combination with some volatile components of the raw material contributed to the characteristic ‘fungal/flower’ aroma of Fuzhuan brick‐tea. Microbial metabolism during the fermentation process probably played the key role in the generation of characteristic aromatic compounds of Fuzhuan brick‐tea. Copyright © 2007 Society of Chemical Industry     

贾湖原香型白酒主要风味物质馏出规律初探

为研究贾湖原香型白酒馏酒规律,将蒸馏发酵50 d贾湖原香型白酒酒醅得到的基酒,采用气相色谱（GC）法分析不同馏酒时间原酒的骨架成分。结果表明,贾湖原香型基酒中的酸类、乙缩醛、醇类、酯类等主要风味骨架成分随蒸馏时间差异明显,酸类物质随着蒸馏时间延长含量逐渐增大;除β-苯乙醇外,醇类随着蒸馏时间延长,含量逐渐减少;除乳酸乙酯、壬酸乙酯外,酯类随着蒸馏时间延长含量逐渐减少。结果表明7～35 min蒸馏时间的白酒品质最好。     

Odour‐active compounds in mango (Mangifera indica L. cv. Corazón)

Simultaneous distillation–extraction combined with GC‐FID and GC‐MS were used to analyse volatile compounds from mango (Mangifera indica L. cv. Corazón) and to estimate the most odour‐active compounds in the fruit. The analyses led to the identification of 167 components, from which 128 were positively identified. The aroma‐active areas in the gas chromatogram were screened by the application of the aroma extract dilution analysis and by odour activity values. Eighteen odorants were considered as the most odour‐active compounds: (E)‐β‐damascenone, ethyl butanoate, (E,Z)‐nonadienal, ethyl 2‐methylpropanoate, (E)‐2‐nonenal, (E)‐β‐ionone, terpinolene, δ‐3‐carene, β‐caryophyllene, ethyl 2‐methylbutanoate, limonene, myrcene, linalool, γ‐octalactone, nonanal, methyl benzoate, 2,5‐dimethyl‐4‐methoxy‐3(2H)‐furanone and hexanal.     

泸型曲酒"增己降乙"方法的探讨

当基酒中乙酸乙酯组分偏高,会使香气不正、不协调、典型性差,影响酒质。找出了发酵产物中乙酸乙酯偏高的原因,并制定了降低乙酸乙酯的工艺措施：（1）优选原料配比,提高制曲温度;（2）降低窖内材料氧气分压;（3）回醅（酒）发酵;（4）入窖条件遵循“二高一低”,即高酸度、高淀粉、低水分,并采用“原出原入”的方法;（5）科学分馏;（6）黄水回用;（7）加强老窖养护。（陶然）     

利用废啤酒蒸馏回收酒精及风味物质的研究

采用泡罩式蒸馏塔将废啤酒进行蒸馏,制备废啤酒蒸馏酒。利用气相色谱-质谱联用（GC-MS）仪检测废啤酒和其蒸馏酒中的风味物质,并对废啤酒、废啤酒蒸馏酒以及浓香型白酒的风味进行感官品评。结果表明,共检测出16种主要的醇类、酯类和醛类挥发性物质与废啤酒比较。丁酸乙酯、己酸乙酯、乙酸苯乙酯、正丁醛、2-甲基丁醛、己醛、异戊醛、乙醛这8种风味物质在蒸馏酒中消失;2-苯基乙醇、乙酸异戊酯在蒸馏酒中质量浓度减少;正丙醇、异丁醇、异戊醇、乙酸乙酯、辛酸乙酯、糠醛等风味物质则在蒸馏酒中质量浓度增加。废啤酒蒸馏酒的酯香味突出、香气纯净、风味持久性好。将感官品评结果和主成分分析（PCA）结合发现废啤酒蒸馏酒与浓香型白酒有一定的相似性,可作为白酒基酒使用。     

清香型不同次原酒香气成分分析

采用液液萃取方法提取清香型不同米次原酒中的香气物质,通过气相色谱-闻香技术(GC-O)和气相色谱-质谱法(GC-MS)对香气化合物进行分析。在清香型原酒中共发现FD≥25的香气物质50种,定性47种。闻香结果显示,酯类和芳香族化合物是清香型原酒的重要香气物质。大原酒B和二原酒GC-O分析结果比较接近。酯类香气物质对大原酒A的香气贡献相对较大,芳香族、有机酸、硫化物、内酯类及杂环类化合物对大原酒B和二原酒的香气贡献相对较大,酚类化合物仅在大原酒B中FD值较大。正是这些香气物质的种类、浓度的不同使得次原酒的香气有明显差异。     

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.