Characterization of Volatile and Semi‐Volatile Compounds in Chinese Rice Wines by Headspace Solid Phase Microextraction Followed by Gas Chromatography‐Mass Spectrometry

The volatile and semi‐volatile compounds of Chinese rice wines were extracted by headspace solid phase microextraction (HS‐SPME) and analyzed by gas chromatography‐mass spectrum (GC‐MS). The original Chinese rice wine samples were diluted with deionized water to a final concentration of 6% (v/v) ethanol and then extracted by HS‐SPME. The samples were pre‐equilibrated at 50°C for 15 min and extracted with stirring at the same temperature for 45 min prior to injection into a GC‐MS. A total of 97 volatile and semi‐volatile compounds were identified from ten Chinese typical rice wine samples, including 13 alcohols, 8 acids, 28 esters, 4 aldehydes and ketones, 17 aromatic compounds, 3 lactones, 6 phenols, 3 sulphides, 9 furans and 6 nitrogen‐containing compounds, of which, 39 compounds were firstly reported in Chinese rice wine. By stepwise linear discrimination analysis, the ten Chinese rice wine samples could be classified into three groups according to the production area, and in particular, the production technologies.     

Characterization of volatile compounds from Daqu‐a traditional Chinese liquor fermentation starter

Daqu is a fermentation starter and substrate complex that is used to initiate the solid fermentations for the production of Chinese liquor. The aroma of Daqu is one of the most important factors that influence the flavour of Chinese liquor. To further study the aroma of Daqu, volatile compounds in ten Daqu samples were extracted by headspace solid‐phase microextraction (HS‐SPME) and analysed by gas chromatography–mass spectrum (GC‐MS). The samples were pre‐equilibrated at 50 °C for 10 min and extracted with stirring at the same temperature for 30 min prior to injection into a GC‐MS. A total of 75 volatile compounds were characterised by GC‐MS, including twelve alcohols, eleven esters, eight acids, nine aromatic compounds, four phenols, two furans, fourteen nitrogen‐containing compounds and fifteen aldehydes and ketones. By a principal component analysis (PCA), the ten Daqu samples could be classified into three groups according to their origins and, in particular, the production technologies.     

HS‐SPME/GC‐MS and chemometrics for volatile composition of Chinese traditional aromatic vinegar in the Zhenjiang region

The main purpose of this study was to determine the volatile composition of Zhenjiang aromatic vinegar, one of the four famous China‐style cereal vinegars, by using headspace solid‐phase microextraction (HS‐SPME)/gas chromatography‐mass spectrum (GC‐MS) and chemometrics. For this purpose, the HS‐SPME sampling method for the volatile compounds of Zhenjiang aromatic vinegar was optimized by a second‐order rotatable central composite experimental design (CCD). A HS extraction of the volatile compounds by incubation on a 65 µm thickness polydimethylsiloxane/divinylbenzene (PDMS/DVB) fibre during 44.2 min at 69.5°C with 1.9 g NaCl add gave the most effective and accurate extraction. By the optimized method, a total of 58 volatile compounds, including 9 alcohols, 13 acids, 16 esters, 5 aldehydes, 4 ketones and 8 heterocycle compounds, were identified from 13 aromatic vinegar samples manufactured in Zhenjiang region. By principal components analysis (PCA), the thirteen vinegar samples were classified into 3 groups, and 10 volatile compounds were chosen as characteristic compounds of Zhenjiang aromatic vinegars. Copyright © 2012 The Institute of Brewing & Distilling     

Characterization of rum using solid-phase microextraction with gas chromatography–mass spectrometry

Headspace solid-phase microextraction was used to extract and analyze volatile compounds in different aged rums. The interference of ethanol was resolved with a dilution of the sample at 12% v/v. The extraction procedure, using a 100 μm PDMS fibre with 35 min at 30 °C, permitted the isolation of a large quantity of volatile compounds. One hundred and eighty-four volatile compounds were identified, including 64 esters, 47 benzenic compounds, 16 terpenoids, 14 alcohols, 10 acetals, 9 aldehydes, 6 phenols, 6 ketones, 6 furans, 3 acids and 3 benzopyrans.     

Comparison of Two Extraction Techniques,Solid‐Phase Microextraction Versus Continuous Liquid–Liquid Extraction/Solvent‐Assisted Flavor Evaporation,for the Analysis of Flavor Compounds in Gueuze Lambic Beer

Lambic is a beer style that undergoes spontaneous fermentation and is traditionally produced in the Payottenland region of Belgium, a valley on the Senne River west of Brussels. This region appears to have the perfect combination of airborne microorganisms required for lambic's spontaneous fermentation. Gueuze lambic is a substyle of lambic that is made by mixing young (approximately 1 year) and old (approximately 2 to 3 years) lambics with subsequent bottle conditioning. We compared 2 extraction techniques, solid‐phase microextraction (SPME) and continuous liquid–liquid extraction/solvent‐assisted flavor evaporation (CCLE/SAFE), for the isolation of volatile compounds in commercially produced gueuze lambic beer. Fifty‐four volatile compounds were identified and could be divided into acids (14), alcohols (12), aldehydes (3), esters (20), phenols (3), and miscellaneous (2). SPME extracted a total of 40 volatile compounds, whereas CLLE/SAFE extracted 36 volatile compounds. CLLE/SAFE extracted a greater number of acids than SPME, whereas SPME was able to isolate a greater number of esters. Neither extraction technique proved to be clearly superior and both extraction methods can be utilized for the isolation of volatile compounds found in gueuze lambic beer.     

Volatile Compounds in Fermented and Acid-hydrolyzed Soy Sauces

ABSTRACT: Volatile compounds in fermented and acid-hydrolyzed soy sauces were isolated and analyzed using solvent extraction and solid-phase microextraction. Quantitatively, alcohols and esters were dominant in the volatiles of fermented soy sauce, whereas heterocyclic compounds, including pyrazines and furans, and acids were relatively abundant in the acid-hydrolyzed soy sauce. The odor-active compounds were also evaluated. The major odor-active compounds of fermented soy sauce were acetic acid, furfuryl alcohol, 2-methoxyphenol, benzeneethanol, benzoic acid, butyric acid, 2-ethyl-4-hydroxy-5-methyl-3(2H) furanone, and 2-methylbutanal, whereas acetic acid, 2-methoxyphenol, formic acid, benzoic acid, 2,5-dimethylpyrazine, 2,6-dimethylpyrazine, butyric acid, 2,6-dimethoxyphenol, 3-hydroxy-2-methyl-4H-pyran-4-one, 2-acetyl-5-methylfuran, 2,5-dimethyl-3-ethylpyrazine, and 2-methylbutanal constituted the major odor-active compounds of acid-hydrolyzed soy sauce.     

中式酱油和日式酱油香气物质的对比研究

采用直接溶剂萃取法对中式酱油和日式酱油的挥发性香气物质进行提取、浓缩,并利用气相色谱.质谱联用仪(GC-MS)对其进行鉴定.研究结果表明,中式酱油中鉴定出94种风味物质,日式酱油中鉴定出125种风味物质.中式酱油的主要挥发性物质为酯类(35.97%)、醇类(17.79%)、酸类(16.05%)和醛酮类(8.67%),而日式酱油的主要挥发性物质为酯类(52.98%)、酸类(24.01%)、醇类(9.31%)和醛酮类(6.02%),挥发性香气物质的种类及其相对含量的差异是造成2种酱油香气差别的主要原因.     

红曲霉菌混合制曲高盐稀态发酵过程挥发性物质的变化

为研究添加红曲复合制曲酿造酱油高盐稀态发酵过程中风味物质变化,通过顶空固相微萃取-气相色谱-质谱联用（HS-SPME-GC-MS）对稀醪中的挥发性风味物质进行分析,确定稀醪的固相微萃取最佳条件为:75 μm CAR/PDMS萃取头,添加2.5 g氯化钠、萃取温度50 ℃、萃取时间30 min。在该条件下,对不同酱油的挥发性物质种类数量及其占比进行分析,发现红曲酱油相比于其他酱油具有更高的酯类物质占比和丰度,并对稀醪发酵10、30、50、70、80、120、160 d样品检测得到醇类（14种）、酸类（7种）、酮类（9种）、酯类（15种）、酚类（6种）、醛类（3种）、吡嗪类（3种）、吡咯类（1种）、烯类（1种）、呋喃类（2种）和其他（4种）,共65种物质。对比发现,红曲酱油挥发性物质中酯类的含量与种类最为丰富,是构成红曲酱油风味的的主要物质。经热图分析发现,稀醪发酵0~120 d是醛酮类、吡嗪、吡咯类物质含量的生成时期;醇类物质是在整个发酵期间均有某种物质显著增加,稀醪发酵80~180 d是酚类、酸类、酯类的显著增加时期;其中酯类香气物质的增加说明了红曲酵母的添加显著加强了酱油的酯类风味,改善了酱油风味。     

Changes in Volatile Compounds of Chinese Rice Wine Wheat Qu During Fermentation and Storage

In order to understand the optimum time of using wheat Qu for Chinese rice wine brewing on the basis of the contents of volatile compounds, changes in volatile compounds of Chinese rice wine wheat Qu during fermentation and storage were studied by headspace solid phase microextraction (HS‐SPME) combined with gas chromatography‐mass spectrum (GC‐MS). It was shown that the concentrations of most groups of volatiles, including alcohols, aldehydes, aromatic compounds, phenols, sulphides, furans, and nitrogen‐containing compounds, increased progressively from the first day to the fourth day of fermentation, and then decreased gradually. A minority group of volatile compounds such as acids and ketones peaked after one day of fermentation, esters increased slowly from the first day to the eighth day of fermentation. Lactones and esters rose slowly from the first day to the fifteenth day of fermentation respectively, and decreased afterwards, whereas the evolution of terpenes was somewhat erratic. These results suggested that changes in the concentrations of most groups of volatile compounds during fermentation and storage were uniform. This made it possible to determine the optimum level of fermentation and storage for Chinese rice wine wheat Qu on the basis of the contents of volatile compounds.     

HS-SPME-GC-MS analysis of volatile aromatic compounds in alcohol related beverages made with mulberry fruits

Wine aroma is one of the most important parameters responsible for its quality, and hence for consumer acceptance. In order to obtain an appropriate technique to study volatile aroma compounds in mulberry wines, headspace-solid phase microextraction (HS-SPME) comb 40°C for 30 min with a 50/30 μm divinylbenzenecarboxen-polydimethylsiloxane (DVB-CAR-PDMS) fiber. Approximately 80 volatile compounds have been quantified in the mulberry wine, pertaining at several chemical groups, mainly higher alcohols, fatty acids, esters, and some volatile phenols whose concentration range from few to 138.36 mg/L. This work describes a novel methodology for the analysis of mulberry wines by HS-SPME coupled to GC-MS. HS-SPME using a 50/30 μm DVB-CAR-PDMS fiber is provided the higher extraction efficiency (p<0.05) for the volatiles including the most esters, higher alcohols, and fatty acids than by the other fibers.     

2种不同工艺酱油原油的挥发性成分的分析

通过用SPME萃取结合GC-MS分析了2种不同工艺酱油原油的挥发性成分,用面积归一化法测定其组分的相对含量,2种酱油中共鉴定出117种(7大类)挥发性风味化合物,天然晒露的酱油共有62种,低盐保温发酵原油有84种,所鉴定的风味化合物包括15种醇,10种酚,18种酸,19种酯,21种醛酮化合物,27种杂环化合物和7种含硫化合物。其中O-愈创木酚、乙酸、3-甲基丁酸、2-甲基丁酸、2-甲基丁醛、苯甲醛、苯乙醛和三甲基吡嗪为2种酱油中都存在的主体物质。尽管酱油中多数香气成分含量极微,但是多种香气成分的存在极大地丰富了酱油的风味。     

不同发酵时间的郫县豆瓣酱挥发性成分分析

为研究不同发酵时间对郫县豆瓣酱挥发性成分的影响,采用顶空固相微萃取(HS-SPME)结合气质联用技术(GC-MS),对两种原料生椒醅与阴瓣子,以及3 种不同发酵时间的郫县豆瓣酱中的挥发性成分进行分析鉴定。从两种原料中共分离鉴定出66 种挥发性化合物,其中醇5 种、酯24 种、酸2 种、醛5 种、烃23 种、酚4 种、呋喃化合物1 种、含氮化合物2 种;从3 种发酵豆瓣中共分离鉴定出88 种挥发性化合物,其中醇7 种、酯20 种、酸3 种、醛9 种、烃35 种、酚6 种、酮4 种、含氮化合物3 种。其相同的成分是苯甲醛、苯乙醛、(Z)-3,7- 二甲基-1,3,6- 辛三烯、3,7- 二甲基-1,6- 辛二烯-3- 醇、2,6,6- 三甲基-2- 环己烯-1,4- 二酮、4- 乙基愈创木酚、十四烷、十七烷、十六酸乙酯等。     

米曲霉发酵高盐稀态酱油过程中典型挥发性风味物质的形成

米曲霉是发酵酱油的主要菌种,为了更加具体了解米曲霉发酵酱油过程中典型挥发性风味物质的形成,该研究利用气相色谱-质谱联用（GC-MS）仪对沪酿3.042米曲霉单菌种发酵高盐稀态酱油在不同发酵阶段的酱醪进行挥发性风味物质检测,并与12种市售高盐稀态酱油的挥发性风味物质进行对比验证。结果表明,酱醪发酵0～6个月的过程中,醇酚类、酸类物质、酯类物质、含氮化合物含量逐渐增加,挥发性风味物质之间组成比例更加协调,典型的挥发性风味物质包括乙醇、乙酸、3-甲基丁酸、苯乙酸乙酯、十六酸乙酯、2,5-二甲基吡嗪、2,3,5-三甲基吡嗪、苯甲醛、苯乙醛,与市售酱油中典型的挥发性风味物质相同,这些物质保证了酱油风味的相似性。     

Olfactometric characterization of aroma active compounds in fermented fish paste in comparison with fish sauce,fermented soy paste and sauce products

Aroma active compounds in commercial fermented fish meat paste product (fish miso), fermented soy paste (soy miso), fish sauce and soy sauces were characterized by using a dynamic headspace method for volatile isolation and GC olfactometry for odor perception. A total of 123 volatile compounds consisting mainly of aldehydes, alcohols, esters, ketones, furans, sulfur and nitrogen-containing compounds, aromatics and acids were consistently identified. A major 16 odor-active compounds were distinguished to contribute as key aroma compounds for the miso and sauce products. Olfactometric and sensory findings clearly differentiated miso products with caramelic, fruity aroma notes, whereas fish sauce products were characterized by ammoniacal, fishy, nutty and cheesy odor note. Soy sauce products, however, were dominated by nutty and cheese aroma. Use of koji for fish miso production was found effective to enhance sweet aroma to the product with a reduction of nutty, meaty and rancid nuance. Principal component analysis employed for statistical interpretations clearly elucidated the relationship among different types of fermented products.     

耐盐乳酸菌和酵母菌强化技术对高盐稀态发酵酱醪品质的影响

分别将耐盐乳酸菌Tetragenococcus halophilus CGMCC 3792、耐盐酵母菌Zygosaccharomyces rouxii CGM-CC 3791和Candida versatilis CGMCC 3790菌悬液接入酱醪中,利用顶空-固相微萃取偶联气质联用技术(HS-SPME/GC-MS)检测了发酵125 d酱醪中挥发性组分的变化。研究结果表明,T.halophilus CGMCC 3792强化的酱醪中酸类、醇类、酮类、呋喃类、吡嗪类和其他组分的相对含量降低,酯类、醛类和酚类组分的相对含量增加,其中苯乙醇、乙酸乙酯、辛酸乙酯、癸酸乙酯和4-乙基愈创木酚等的相对含量显著增加,而Z.rouxii CGMCC 3791、C.versatilis CGMCC 3790共培养强化的酱醪中醇类、酯类、醛类和其他组分的相对含量增加,酸类、酚类、呋喃类和吡嗪类组分的相对含量降低,其中苯乙醇、长链脂肪酸乙酯(月桂酸乙酯、棕榈酸乙酯、亚油酸乙酯等)的相对含量显著增加。此外,本研究中T.halophilus CGMCC 3792强化的酱醪中4-乙基愈创木酚的相对含量大幅增加,且在整个发酵过程中其含量也单调增加,对于T.halophilus CGMCC 3792是否具有分泌4-乙基愈创木酚的能力以及是否冷温工艺赋予该菌株合成4-乙基愈创木酚的能力需进一步探究。     

VOLATILE CONSTITUENTS OF ORANGE WINE OBTAINED FROM MORO ORANGES (CITRUS SINENSIS[L.] OSBECK)

The volatile constituents of blood orange wine were determined. Moro variety (Citrus sinensis[L.] Osbeck) was used for the production of wine. The fermentation was performed spontaneously at 20C. Volatile components were extracted with dichloromethane, and analyzed by gas chromatography‐flame ionization detection (GC/FID) and gas chromatography‐mass spectrometry (GC/MS). A total of 64 volatiles, including higher alcohols (20), esters (13), terpenes (11), acids (7), volatile phenols (6), lactones (2), acetal compounds (2), ketone (1), aldehyde (1) and acetoin (1) were identified in wine. The total amount of volatile compounds was 125.0 mg/L. Higher alcohols and esters were the largest groups and made up more than 86% of the volatiles.     

Characterisation of odour‐active compounds in papaya (Carica papaya L.) wine

The volatile compounds of papaya wine were isolated by continuous solvent extraction and analysed by gas chromatography‐flame ionization detector and gas chromatography‐mass spectrometry. A total of 118 volatile constituents were detected, and ninety‐seven were positively identified. The composition of papaya wine included fifty‐three esters, twenty‐two alcohols, nine acids, seven phenols and derivatives, seven sulphur compounds, five lactones, five terpenes, three ketones, two aldehydes and five miscellaneous compounds. The aroma‐active areas in the gas chromatogram were screened by application of the aroma extract dilution analysis and by odour activity values. Six odorants were considered as odour‐active volatiles: ethyl octanoate, (E)‐β‐damascenone, 3‐methylbutyl acetate, benzyl isohtiocyanate; ethyl hexanoate and ethyl butanoate.     

Comparison of simultaneous distillation extraction (SDE) and solid‐phase microextraction (SPME) for the analysis of volatile compounds in dry‐cured ham

Simultaneous distillation extraction (SDE) and solid‐phase microextraction (SPME) using a carboxen/polydimethylsiloxane fibre were compared for their effectiveness in the extraction of volatile compounds from dry‐cured ham samples. A higher number of compounds was detected using SPME owing to the use of a solvent delay time in the GC‐MS analysis of SDE extracts. SPME was more efficient in extracting low molecular weight and high volatility compounds, while SDE was able to extract compounds with low volatilities that were not extracted using SPME. Both techniques satisfactorily extracted most volatiles previously highlighted as odour‐active compounds in dry‐cured ham. However, the ratio between some compounds from lipid oxidation and those from degradation of amino acids was much lower in SDE extracts than with SPME, which could be a consequence of the development of Strecker degradation of amino acids during distillation in SDE owing to the high temperatures used. Similarly, diunsaturated aldehydes detected in SDE extracts were absent using SPME, probably owing to oxidation of polyunsaturated fatty acids in SDE as a consequence of the temperature during extraction. Copyright © 2004 Society of Chemical Industry     

蓝波奶酪挥发性风味成分的分离与鉴定

采用顶空固相微萃取法和同时蒸馏萃取法提取蓝波奶酪中的挥发性风味成分,利用气相色谱-质谱联用技术对挥发性风味成分进行分离鉴定。结果表明,经过气相色谱-质谱联用技术分析,共鉴定出111 种挥发性成分,包括烃类2 种、醛类6 种、酮类12 种、酸类20 种、酯类49 种、醇酚类13 种、含硫含氮及其他杂环化合物9 种。可能对风味造成影响的化合物有：2-庚酮、2-壬酮、丁酸、己酸、辛酸、正癸酸、癸酸乙酯、3-（甲硫基）-1-丙醇、6-庚基四氢-2H-吡喃-2-酮。     

金华火腿挥发性风味的分离与鉴定

<正> 金华火腿是我国最著名的火腿品种,素以经久耐藏,芳香独特而著称。我国其他地方名腿的加工技术也都是由金华引进技术,经演变而成的.因此金华火腿的风味无疑是我国腌制火腿的代表,但对这一传统食品的风味了解极少。