The lack of reproducibility of different distillation techniques and its impact on pear spirit composition

We analysed the impact of operation variability on the composition of pear spirits obtained with a Charentais alembic and a packed distillation column. Lack of reproducibility significantly affected the spirits’ compositions, with batch distillation columns more difficult to operate reproducibly vs. traditional alembics. The composition of column distilled spirits differed more in esters, such as ethyl octanoate, ethyl decanoate and ethyl palmitate. In turn, alembic spirit compositions differed more in acetaldehyde and acetal. Moreover, column distilled spirits contained four times more esters, 20% more higher alcohols, 40% less acetaldehyde and 10% less methanol than alembic spirits. Spirits distilled with a rectification column were more concentrated in ethanol than alembic distilled spirits, although both distillation systems recovered the same amount of ethanol in the heart fraction.     

Electrospray ionization mass spectrometry fingerprinting of Brazilian cacha?as produced in copper alembic and in stainless-steel column stills

Brazilian cacha?a can be produced in two different ways: distilled in stainless steel column or in copper alembic stills. We evaluated 36 samples of commercial non-aged cacha?as: 18 samples of sweetened cacha?as distilled in stainless steel column, and 18 samples distilled in copper alembic stills. Fingerprints were obtained through electrospray ionization mass spectrometry by recording the intensity of the 15 most abundant ions. Principal component analysis was applied to the data and separated the samples in two groups. However, after sample standardization with sugar (20?g?L^?1), it was not possible to group them by type of distillation. The results showed that the technique applied did not allow differentiation of cacha?as based on the distillation system, but for the presence or absence of sugar in them.     

猕猴桃果酒酿造

以猕猴桃为原料进行发酵酿酒实验,介绍了猕猴桃酒的生产工艺及其关键技术。以新鲜猕猴桃果实为原料,接种6.0%的活性干酵母,加白砂糖100g/L,在25℃下进行发酵,可获得色泽黄绿、果香浓郁、口味协调、酒体厚实的猕猴桃发酵酒,其酒精度为10.5%vol。所得猕猴桃发酵酒经蒸馏后得到无色透明,具有清爽果香味的猕猴桃白酒,其酒精度达到18%vol。然后,通过提取出茉莉花茶中的香味成分,加入到猕猴桃白酒中,使其具有特殊的茉莉花茶香味。     

Spirit Distillation Strategies for Aroma Improvement Using Variable Internal Column Reflux

The production of spirits by distillation of wine, fruit wines, and grape pomace is normally carried out using classic copper Charentais alembic or batch distillation columns. An alternative to these classic systems, however, is a rectification packed column equipped with an internal partial condenser which allows for easy control of the internal reflux by manipulating the flow of cooling water of the partial condenser. This paper outlines an experimental study which explores the ability of variable reflux distillation policies in packed columns to tailor the chemical composition of the distillate. The results showed that a high reflux rate at the beginning of the distillation is a good option to reduce the impact of unpleasant compounds in the heart cut. Using this strategy, 40 % less head compounds were recovered in the heart cut, reducing their sensorial impact by 70 %. In addition, 50 % less acetic acid was recovered in the heart cuts. High reflux rates during the heart cut distillation reduce the concentration of higher alcohols; nevertheless, this strategy must be applied for longer periods than those used in our study to significantly alter the composition of the heart cuts.     

Influence of the fermentation pH on the final quality of Blanquilla pear spirits

Blanquilla pear concentrate was diluted, fermented and distilled to produce the pear spirits. The fermentations were held at the native pH and at an acidified pH of 3.2. Two sets of experiments were performed using a different fermentation yeast and a different distillation equipment. The heart fractions from each distillation (which form the pear spirits) were analysed by gas chromatography. The results showed, in both experimental sets, that reducing the fermentation pH significantly increased the concentration of most of the higher alcohols and decreased the concentration of ethyl acetate in the spirits. Moreover, pear distillates obtained in the first experimental set showed significantly higher concentrations of most of the long‐chain ethyl esters (C₆–C₁₂) compared to those obtained in the second experimental set.     

FRUIT BRANDY PRODUCTION BY BATCH COLUMN DISTILLATION WITH REFLUX

The relationship between the operating parameters of batch fruit spirits column stills with reflux and the congener (trace compounds that provide flavors and aromas) concentrations in resulting fruit spirits has not been widely studied. Congener concentrations were determined in three different collection fractions, or “cuts,” during batch distillation. Acetaldehyde and ethyl acetate were found in higher concentrations in the head cut, first overhead fraction, of the distillation and have lower boiling points relative to ethanol. 1‐Propanol and isoamyl alcohol (isopentanol) were present in higher concentrations in the tail cut, third or final fraction, of the distillation and have boiling points that are higher than ethanol. Methanol has a unique concentration profile as it has higher concentrations in both the head and tail cuts, but a lower concentration in the heart cut, the middle fraction which is the desired product of the distillation. Methanol was of particular interest because the distillate must adhere to governmental regulations that limit its concentration in the product. Operating‐condition parameters that were studied include the number of trays used in the distillation as well as the use of a “catalytic converter,” a high surface, copper‐packing material thought to catalyze formation of cyanide‐containing compounds allowing them to be separated from the distillate. The effect of the number of trays used in a distillation on the concentration of ethanol and the congeners, methanol, acetaldehyde, ethyl acetate, 1‐propanol and isoamyl alcohol in the final distilled spirits product is presented. An additional result of acetaldehyde production at the copper surface of the catalytic converter was also discovered in the analysis of the data.     

不同酿酒酵母对山葡萄北国蓝蒸馏酒挥发性物质的影响

以市场上常见的8种活性干酵母作为山葡萄北国蓝的发酵剂,通过比较发酵速率、定性定量分析蒸馏酒中香气成分,并结合主成分分析（PCA）,综合得出适合酿造山葡萄北国蓝蒸馏酒的酿酒酵母。结果表明,在发酵过程中,发酵速率最快的是酵母ADT,酵母CEC01次之;发酵完成后,酵母菌MST的发酵原酒酒精度最高,为（9.80±0.11）%vol,发酵最彻底,产酒能力优于其他酵母（P＜0.05）,其次是酵母CEC01,为（9.79±0.01）%vol;酵母菌CEC01发酵的山葡萄蒸馏酒中挥发性物质含量最高,为16 394.24 μg/L,其次是酵母VF（16 163.22 μg/L）、ADT（15 576.32 μg/L）;主成分分析综合得分最高的是酵母CEC01,其次是酵母ADT。由此可得,酵母CEC01、ADT发酵能力强,产酒率高,且蒸馏酒的酒香浓郁、品质较好,适合酿造山葡萄蒸馏酒。     

Aroma compounds in barrel aged apple distillates from two different distillation techniques

The major fermentation and maturation related congeners in apple distillates from two different distillation techniques (alembic and column), matured in oak for 18 months, were measured by GC‐MS and HPLC. Together with a higher ethanol content, column distillates had higher ethyl acetate, methanol and n‐propanol levels compared with alembic distillates. A higher content of acetaldehyde was characteristic of the alembic distillates. The concentrations of i‐butanol, n‐butanol, amyl alcohols and n‐hexanol were not affected by the distillation technique used. Increasing the ageing time of distillates in oak resulted in an increase in the contents of acetaldehyde, ethyl acetate and amyl alcohols while the content of methanol decreased during ageing. Throughout ageing, there were no significant changes in the concentrations of n‐propanol, i‐butanol, n‐butanol and n‐hexanol. Among the maturation related compounds, gallic acid, ellagic acid, vanillin and syringaldehyde were determined in apple distillates with ellagic acid being the most abundant. The contents of gallic acid and ellagic acid increased during ageing whereas vanillin and syringaldehyde slightly increased throughout the 18 months of maturation. © 2019 The Institute of Brewing & Distilling     

不同发酵时间猕猴桃米酒品质变化的研究

以猕猴桃、糯米为原料制备猕猴桃米酒,采用密度瓶法、pH计、电子鼻、电子舌、色度仪等对不同发酵时间的猕猴桃米酒的酒精度、pH值、滋味、气味、色度等品质指标进行检测,并对结果进行主成分分析（PCA）。结果表明,主成分得分排名靠前的3个猕猴桃米酒样品发酵时间分别为78 h、66 h与30 h,其中,发酵30 h的米酒样品中,猕猴桃特有成分萜烯类物质含量最高,同时pH值最低,而苦味、涩味、后味指标均偏低。因此,发酵时间30 h有助于提升猕猴桃米酒的风味。     

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。     

Brazilian cachaça: “Single shot” typification of fresh alembic and industrial samples via electrospray ionization mass spectrometry fingerprinting

Copper pot stills (alembics) and industrial stainless steel columns are the most common distillation devices used in Brazil to produce sugarcane spirit (cachaça). The use of both apparatus originates two distinctive products, the so-called (a) alembic (the most valuable) and (b) industrial cachaças, respectively, with subtle but characteristic chemical compositions and sensorial properties. Herein, we demonstrate that the use of direct infusion electrospray ionization mass spectrometry in the negative mode, ESI(−)–MS, is able to provide fast “single shot” fingerprinting discrimination between these two types of spirits. Representative samples of both spirits show ESI(−)–MS with regular sets of diagnostic ions of m/z 279, 255, 199, 171, 143 (alembic) and of m/z 377, 341 (industrial). Principal component analysis (PCA) of the ESI(−)–MS data consistently split the 34 alembic and the 14 industrial samples into two well-defined groups. Sugar addition to the alembic samples was also easily detected.     

在线质谱法快速检测酒中5种常见乙酯

采用在线质谱法,在无需样品预处理的条件下,建立快速检测酒中乙酸乙酯、丁酸乙酯、乳酸乙酯、戊酸乙酯、己酸乙酯5 种常见乙酯的方法。5 种乙酯在0.5～20 mg/L内线性关系良好（R2＞0.99）,2 个加标水平（0.5、5 mg/L）的回收率为81.1%～99.7%,相对标准偏差为4.7%～9.4%,检出限为24～312 μg/L。对市场上消费的蒸馏酒（中国白酒、白兰地、金酒及威士忌）进行检测分析,同种类蒸馏酒检出的主要成分及其比例基本一致,中国白酒、威士忌和白兰地均不同程度地检出乙酯。同时,结合主成分分析可对不同品种的蒸馏酒进行较好的区分。     

Inoculated fermentation of orange juice (Citrus sinensis L.) for production of a citric fruit spirit

The yeast Saccharomyces cerevisiae UFLA CA1174 was evaluated for its potential to produce an orange spirit, as a possible alternative to reduce waste and increase income to citrus farmers. The sugar concentration of the orange juice was adjusted to 16ºBrix and the pH to 4.5. The orange juice was inoculated at approximately 7 log CFU/mL, and the fermentation was performed at room temperature until ºBrix stabilization. The yeast used showed high values for the conversion factors of the substrates into ethanol (Y_p/s 0.50 g/g), the volumetric productivity of ethanol (Q_p 1.78 g/L/h), the biomass productivity (P_x 58.47 g/g) and the fermentation efficiency (E_f 97.83%). The sugars were converted quickly, and a high ethanol concentration (58.13 g/L) was achieved after 24 h of fermentation. The orange wine was distilled in a copper alembic, and the head, heart and tail fractions were collected. The orange spirit produced (heart fraction) had high concentrations of acetaldehyde, ethyl acetate, isoamyl alcohol and 2‐phenylethanol. The results showed that orange juice could be a good substrate for fermentation and distillation, and the sensory analysis performed revealed that the produced beverage had good acceptance by the tasters. Copyright © 2013 The Institute of Brewing & Distilling     

Characterisation of wines and distilled spirits from melon (Cucumis melo L.)

Melon fermentation and distillation was studied with a view to produce melon spirits. Three different substrates were obtained from melon (Cucumis melo L.). Sugar concentration was around 60–70 g L^?1 and the pH between 4.6 and 5.2. The substrates were clarified and then fermented at one of two pH levels at 20 °C. A commercial Saccharomyces cerevisiae starter culture was used to obtain melon wines with an alcohol concentration of 3.8–5.8% (v/v). The melon wines were distilled in a distillation column to yield distillates with an alcohol content of 33–60% (v/v). The major volatiles in the melon wines and in the distillates were analysed by gas chromatography (GC). The results demonstrated that melon could be a good substrate of fermentation and distillation but also yielded significant differences in the volatiles analysed in the different melon wines and distillates obtained from the different substrates in the different conditions of the experiment. Fermentation pH greatly affected the methanol, acetaldehyde, and butanol contents and thus the final quality of the spirits produced.     

甲醇内标法测定酒精饮料中乙醇含量的研究

在国产SC－6气相色谱仪上使用FID和GDX－102填充柱,甲醇作内标,用峰高比测定酒精饮料中的乙醇含量。对无水乙醇、两种米酒、1种葡萄酒和1种啤酒分别进行了10次平等测定,其CV依次是0．010、0．021、0．0059和00082。可定量回收添加的乙醇。方法具有简便快速的特点。     

Chemical Typification of the Sugarcane Spirits Produced in São Paulo State

To typify São Paulo State sugarcane spirits, 37 chemical compounds were analyzed in 81 Brazilian sugarcane spirits (cachaça), which were produced in different cities from São Paulo State. Among these samples, 56 were distilled in copper alembics, and the other 25 were distilled in steel columns. Hierarchical cluster analysis and principal component analysis were performed with both chemical data sets. The chemical profiles of the cachaças distilled in the column apparatus formed 4 specific clusters, which correspond to 4 distinct geographic regions of São Paulo State. For the cachaças that were distilled in copper alembics, 2 cachaça clusters were formed; however, no correlation between their respective chemical similarities and geographical origins was observed.     

不同品种葡萄皮渣蒸馏酒挥发性香气成分分析

采用顶空固相微萃取-气相色谱-质谱联用（HS-SPME-GC-MS）技术对3种葡萄（贵人香、雷司令、霞多丽）皮渣蒸馏酒的挥发性香气成分进行检测分析。结果表明,从3种葡萄皮渣蒸馏酒中共检测出114种挥发性香气化合物,包括酯类40种、醇类23种、酸类8种、醛类4种、酮类2种、酚类2种、萜烃类24种、其他类11种,其中酯类、醇类和萜烃类挥发性化合物相对含量较高,且贵人香皮渣蒸馏酒的香气成分种类更为丰富。为进一步研究香气化合物与葡萄皮渣品种的关系,对3种葡萄皮渣蒸馏酒样共有的22种香气成分和8类香气化合物进行主成分分析（PCA）,经综合评价得出贵人香葡萄皮渣蒸馏酒香气品质最佳,雷司令葡萄皮渣蒸馏酒次之,霞多丽葡萄皮渣蒸馏酒最差。     

猕猴桃干型果酒发酵工艺优化

以猕猴桃为原料,研究其干型果酒的发酵工艺条件。通过单因素试验和正交试验,研究活性干酵母接种量、SO2 添加量、发酵温度与发酵时间对猕猴桃干型果酒发酵过程的影响,并对发酵工艺条件进行优化。结果表明,猕猴桃干型果酒发酵工艺最佳条件为活性干酵母接种量0.7g/L、SO2 添加量80mg/L、发酵温度26℃、发酵时间21d,酒体风格较为突出。     

Effect of cooling conditions on separation of volatile compounds in grappa using tray and packed columns without reflux

Marcs were distilled using an industrial batch distillation plant. The performance of a tray column and a packed column without reflux were studied under different conditions of vapour cooling obtained by changing the water flow rates (100–350 L h^?1). The temperature of cooling water was +12 °C. With this kind of plant the cooling conditions normally used for producing grappa in the tray column is a water flow of 200 L h^?1 and 250 L h^?1 in the packed column. Each distillate was collected in fractions and analysed for ethanol, lower volatile alcohols and esters. The results show that the tray column under a water flow rate of 200 L h^?1 has a strong rectification effect on the volatile compounds and it has a significant decrease in separation efficiency at 300 L h^?1. Instead, the packed column is poorly affected by the change of the water flow rates from 150 to 350 L h^?1 and a distillate very rich of volatile compounds can be obtained. It was concluded that in order to maintain the classical method of grappa production, which consists in cutting the initial and the final fractions of distillate, the packed column is the most suitable.     

A laboratory yeast strain suitable for spirit production

Yeast strains of the species Saccharomyces cerevisiae currently in use for the production of consumable alcohols such as beer, wine and spirits are genetically largely undefined. This prevents the use of standard genetic manipulations, such as crossings and tetrad analysis, for strain improvement. Furthermore, it complicates the application of the majority of modern methods developed in yeast molecular biology. Here we used two haploid laboratory strains with suitable auxotrophic markers for the construction of a genetically well defined, prototrophic diploid production strain. This strain was tested for its fermentative and sensory performances in comparison to commercially available yeasts. Three different fruit mashes (cherries, plums and pears) were fermented in a 90 kg scale. These were then subjected to distillation and used for the production of spirits with a final ethanol content of 40% (v/v). Fermentation parameters assayed included growth, sugar utilization, ethanol production and generation of volatile compounds, higher alcohols and glycerol. The spirits were also tested for their sensory performances and the data obtained statistically consolidated. Our results clearly demonstrate that this laboratory strain does not display any disadvantage compared with commercial yeasts in spirit production for any of the parameters tested, yet it offers the potential to apply both classical breeding and modern molecular genetic techniques for adjusting yeast physiology to special production schemes.