2种芝麻香型白酒中香气活性成分分析

应用液液萃取法结合气相色谱-质谱-嗅闻联用仪分析2 种芝麻香型白酒（BTQ、YH）中香气活性成分。经保留指数、香气特征并结合标准品比对,BTQ和YH分别定性出挥发性化合物75 种和68 种;结合气相色谱-质谱-嗅闻联用通过芳香萃取物稀释分析分别嗅闻出香气活性化合物48 种和46 种,BTQ中香气稀释（flavor dilution,FD）因子值最大的是3-甲硫基丙醛（FD=6 561）;YH中FD最大的是苯乙醇、3-甲基-1-丁醇、丁酸乙酯、戊酸乙酯（FD=2 187）。通过多种方法联用,对嗅闻到的51 种香气活性成分和28 种非嗅闻活性成分进行定量分析,并结合相关阈值进行香气活性值（odor activity value,OAV）分析,比较它们对整体香气的贡献程度,发现BTQ中有40 种化合物OAV不小于1,YH中有36 种化合物OAV不小于1,2 种酒中香气贡献度最高的是己酸乙酯、3-甲基丁醛、丁酸乙酯、3-甲基丁酸乙酯。结合FD因子及OAV,对这2 种芝麻香型白酒香气有重要贡献的化合物有己酸乙酯、丁酸乙酯和3-甲基丁醛。     

Release of aroma compounds from dry-fermented sausages as affected by antioxidant and saliva addition

The effect of the addition of an antioxidant and saliva on the release of aroma compounds from dry fermented sausages was studied by extracting the headspace at different times using solid phase micro-extraction technique. The compounds were analysed by gas chromatography using a FID detector and identified by mass spectrometry. The addition of butylated hydroxytoluene to dry fermented sausages produced a significant reduction of the release of most of the volatile compounds indicating an oxidation process during sampling. The addition of water and saliva to the dry fermented sausages produced a higher release of pentanal, hexanal and octanal, whilst pentane, 1-octanol, pentanoic acid, and propanal showed a lower rate of release. Moreover, phenylethyl alcohol, 2-butanone, 2,3-pentanedione and 2-nonanone, derived from bacterial metabolism, presented a lower release rate when water and saliva were added. The rate of release of the compounds from dry fermented sausages was not related with the compound hydrophobicity value. Further research is needed to elucidate the effect of fermented sausage matrix on the partitioning of the compounds and its effect on aroma perception.     

Headspace solid‐phase micro extraction coupled to comprehensive two‐dimensional with time‐of‐flight mass spectrometry applied to the evaluation of Nebbiolo‐based wine volatile aroma during ageing

This study presents the application of a headspace solid‐phase microextraction (HS‐SPME) method on the analysis of Nebbiolo‐based wine volatiles by comprehensive two‐dimensional gas chromatography (GC×GC) and time‐of‐flight mass spectrometry (TOF‐MS). The aroma patterns were established for different samples of Nebbiolo‐based wines, aged in oak wood barrels for 18 months at constant temperature. The methodology allowed for the simultaneous analysis of over 130 different volatile compounds detected in the headspace. The odour activity values (OAVs) were assessed to identify potentially important odorants of Nebbiolo‐based wine during ageing. The highest OAVs were obtained for several compounds such as ethyl octanoate, ethyl hexanoate, isoamyl acetate, β‐damascenone, ethyl cinnamate, ethyl 3‐methylbutanate and acetaldehyde. Ethyl butanoate, octanoic acid, ethyl dihydrocinnamate and γ‐nonalactone were also at concentrations higher than their corresponding threshold. Also vanillin, (E)‐whisky lactone, (Z)‐whisky lactone, guaiacol and 4‐ethyl guaiacol seem to be important odorants after oak wood ageing period.     

Flavoromics approach to identifying the key aroma compounds in traditional Chinese milk fan

To determine the key aroma compounds in Chinese milk fan cheese, samples from 6 of the most popular handmade milk fan workshops in Yunnan province of China were analyzed by gas chromatography-mass spectrometry (GC-MS), gas chromatography-olfactometry (GC-O), sensory evaluation, aroma recombination and omission experiments. Seventy-one aroma compounds were identified by GC-MS, and 31 odor-active compounds were detected by GC-O. The relationships between the 31 odor-active compounds and 10 sensory evaluation properties were explored by partial least squares discriminant analysis. The results identified 23 initial key aroma compounds, which were used to simulate the aroma profile of milk fan in aroma recombination experiments. Aroma omission experiments identified propanoic acid, butanoic acid, octanoic acid, octanal, nonanal, 2-nonanone, and ethyl hexanoate as the key aroma compounds. Propanoic acid and butanoic acid contributed to cheese and rancid aromas, octanal and nonanal to the fat aroma, octanoic acid and 2-nonanone to the cheese aroma, and ethyl hexanoate to the fruity aroma of milk fan.     

不同等级金华火腿风味特点研究

随机取5条不同等级金华火腿的股二头肌为样品,利用固相微萃取(SPME)和GC/MS系统进行风味成分研究。结果发现,四级火腿中共检测到116种成分,在1～4级火腿中分别检出84、84、83和92种成分。这些成分可归类为烷烯烃、芳香烃、醇、醛、酮、酸、酯、萜烯类、含氧杂环化合物、含氮杂环化合物、含硫化合物、酰胺类物质和胺类物质。主成分分析显示,第一主成分主要由丁酸、3-甲基丁酸、苯酚、丙酸和丁酸乙酯组成,解释了不同等级金华火腿风味变化总方差的71.6%。第二主成分主要由:已醛、戊醛、2-甲基丁醛、3-甲基丁醛、1-辛烯-3-醇、丙酮和2,3-丁二醇组成,解释了不同等级火腿风味变化总方差的20.5%。根据风味成分产生途径,可以认为微生物是影响产品级别的第一要素。     

Distribution of volatile compounds in lean and subcutaneous fat tissues during processing of dry fermented sausages

The distribution of volatile compound among lean and fat tissues during processing of dry fermented sausages manufactured with either nitrite or nitrate was studied. Twelve volatile compounds were quantified by multiple headspace solid-phase microextraction (multiple HS-SPME) in combination with gas chromatography and mass selective detector (GC–MS) in the lean and fat tissues. The lean tissue contained the highest amount of volatile compounds derived from the lipid oxidation process (heptanal, octanal, nonanal, 1-octen-3-ol, 2-pentanone and 2-heptanone), amino acid degradation reactions (2 and 3-methylbutanal) and esterase activity (ethyl 3-methylbutanoate and ethyl hexanoate). However, the compounds pentanal and hexanal showed similar concentration in both tissues. Few differences were observed in the concentration of volatile compounds due to curing agents throughout the ripening stages although they disappeared after vacuum storage. In conclusion, the main tissue contributing to the flavour development in sausages is the intramuscular fat and the protein fraction. However, the fat tissue contributes to flavour perception due to the solubilization of volatile compounds in it.     

南极磷虾头胸部和腹部挥发性风味成分对比

采用顶空固相微萃取-气相色谱-质谱联用技术分析南极磷虾头胸部、腹部和整虾的挥发性风味成分,结合感觉阈值,利用相对气味活度法评价挥发性风味成分对总体风味的影响程度。结果表明,南极磷虾头胸部的主体风味成分为（E,Z）-2,6-壬二烯醛、3-甲基丁醛、3-甲硫基丙醛、壬醛、苯乙醛、D-柠檬烯、（Z）-4-庚烯醛、二甲基硫醚、辛醛、苯甲醛;南极磷虾腹部主体风味成分为二甲基三硫醚、癸醛、壬醛、3-甲基丁醛、辛醛、二甲基硫醚、D-柠檬烯、（Z）-4-庚烯醛;整虾的主体风味成分则包括二甲基三硫醚、癸醛、（E,Z）-2,6-壬二烯醛、3-甲基丁醛、壬醛、3-甲硫基丙醛、辛醛等物质。     

Effects of environmental factors on leucine catabolism by Carnobacterium piscicola

The metabolites from leucine degradation are involved in dry fermented sausage aroma. The catabolism of leucine by a strain of Carnobacterium piscicola was studied directly in the growth medium with 3H-labelled leucine to investigate the effect of five parameters: phase of growth, pH, oxygen, glucose and alpha-ketoisocaproic acid. Resting cells (RC) were also incubated with 3H-labelled leucine. The radioactive metabolites from leucine catabolism were analysed by high performance liquid chromatography (HPLC). At pH 5.4 and 7.2, the main metabolites detected were 3-methyl butanal, 3-methyl butanol and alpha-ketoisocaproic acid. At pH 6.5, the leucine catabolism was maximum and was characterised by a high production of 3-methyl butanoic acid. Leucine catabolism was most important during the exponential phase of growth. The addition of alpha-ketoisocaproic acid at 1%, glucose at levels of 0.5% to 2% and shaking of the growth medium increased leucine catabolism.     

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...     

Biochemical activities of Micrococcaceae and their effects on the aromatic profiles and odours of a dry sausage model

Micrococcaceae are used as starter cultures in fermented meat, it is therefore important to determine their biochemical activities and especially their aroma producing potential. With this aim, 19 strains of Micrococcaceae were studied in a dry-sausage model. Odours of the samples were assessed by a trained panel. Volatile compounds were analysed by dynamic headspace gas chromatography–mass spectrometry. Strains belonging to the speciesStaphylococcus warneriorStaphyloccocus saprophyticusthat were both lipolytic and unable to reduce nitrate, developed putrid, nauseous or bread odours. These samples were characterized by high desorption of aldehydes (heptanal, hexanal, octanal), 3-hydroxy butan-2-one and 2, 3-butanedione. The highest dry-cured odour was developed with the inoculation of strains ofStaphylococcus carnosusandStaphylococcus xylosuswhich had low lipolytic and proteolytic activities and did not produce acetoin but effectively reduced nitrate. Their inoculation in the sausage model was associated with the greatest desorbtion of 3-methyl butanal, methylketones and ethyl esters and the lowest desorption of alkanes and 3-hydroxy butan-2-one and 2, 3-butanedione.     

Effect of fat content on aroma generation during processing of dry fermented sausages

Dry fermented sausages with different fat contents were produced (10%, 20% and 30%). The effect of fat content and ripening time on sensory characteristics, lipolysis, lipid oxidation and volatile compounds generation was studied. Also, the key aroma components were identified using gas chromatography (GC) and olfactometry. High fat sausages showed the highest lipolysis and lipid oxidation, determined by free fatty acid content and thiobarbituric acid reactive substances (TBARS), respectively. A total of 95 volatile compounds were identified using SPME, GC and mass spectrometry (MS). Fat reduction decreased the generation of lipid derived volatile compounds during processing while those generated from bacterial metabolism increased, although only at the first stages of processing. The consumers preference in aroma and overall quality of high and medium fat sausages was related to the aroma compounds hexanal, 2-nonenal, 2,4-nonadienal, ethyl butanoate and 1-octen-3-ol which contributed green, medicinal, tallowy, fruity and mushroom notes.     

Static Headspace and Aroma Extract Dilution Analysis of Parmigiano Reggiano Cheese

ABSTRACT The aroma compounds in Parmigiano Reggiano cheese were studied with Aroma Extract Dilution Analysis (AEDA). Both static headspace and solvent extraction, high-vacuum distillation techniques were used to isolate aroma compounds. Thirty-six odor-active compounds had high flavor dilution values. Static headspace gas chromatography/olfactometry (GC/O) analysis found that acetaldehyde, 2-methylpropanal, 2-methylbutanal, 3-methylbutanal, ethyl butanoaic, and ethyl hexanoate had low detection volumes, while high-vacuum distillation revealed that acetic, butanoic, hexanoic, octanoic, and decanoic acids, and ethyl butanoate, ethyl hexanoate, dimethyl trisulfide, methional, and phenylacetaldehyde had high flavor dilution values. In addition, some pyrazines appear to be important to the aroma of this cheese.     

A fermented meat model system for studies of microbial aroma formation

A fermented meat model system was developed, by which microbial formation of volatiles could be examined. The model was evaluated against dry, fermented sausages with respect to microbial growth, pH and volatile profiles. Fast and slowly acidified sausages and models were produced using the starter cultures Pediococcus pentosaceus and Staphylococcus xylosus. Volatiles were collected and analysed by dynamic headspace sampling and GC-MS. The analysis was primarily focused on volatiles arising from amino acid degradation and a total of 24 compounds, of which 19 were quantified, were used for multivariate data analysis. Growth of lactic acid bacteria was comparable for model and sausages, whereas survival of S. xylosus was better in the model. Multivariate analysis of volatiles showed that differences between fast and slowly acidified samples were identical for model and sausage. For both sausage and model, fast-acidified samples had a high content of ketones, sulphides and methyl-branched acids, whereas slowly acidified samples had the highest content of methyl-branched alcohols, aldehydes, their ethyl esters, phenylacetaldehyde and methional. Furthermore, model repeatability with respect to pH, microbial growth and volatile profiles was similar to sausage production. Based on these findings, the model system was considered valid for studies of aroma formation of meat cultures for fermented sausage.     

果腔顶空法分析厚皮甜瓜"银帝"的挥发性成分

采用果腔顶空法结合气-质联用(GC/MS)技术分析了“银帝”厚皮甜瓜的挥发性风味物质。该法共分离出82种化合物,初步定性60种,其中以酯类为主体,主要包括乙酸乙酯、丙酸-2-丁烯酯、羟氨基甲酸乙酯、丁二酸甲酯乙酯和2-甲基丁酸乙酯等。果腔顶空法无需溶剂、简便、快速,减化了传统风味物质测定方法的样品前处理环节, 使所测挥发性风味成分更接近于天然。     

Analysis of odour‐active compounds of black mangrove (Avicennia germinans L.) honey by solid‐phase microextraction combined with gas chromatography–mass spectrometry and gas chromatography–olfactometry

The volatile compounds of Cuban black mangrove (Avicennia germinans L.) honey were analysed by solid‐phase microextraction (SPME) followed by gas chromatography–mass spectrometry and gas chromatography–olfactometry. A total of 66 compounds were positively identified in this product for the first time. Application of the aroma extract dilution analysis in a novel approach, which consisted of carrying out successively dilutions of the honey sample with a synthetic honey before the SPME, revealed 17 odour‐active areas in the flavour dilution factor range of 32–1024. On the basis of the quantitative data and odour thresholds, odour activity values (OAV; ratio of concentration to odour threshold) were calculated. Sixteen compounds showed OAVs >1, among which dimethyl sulphide, 3‐methyl butanal, 2‐methylbutanal, heptanal, octanal, phenylacetaldehyde, (Z)‐linalool oxide, (E)‐linalool oxide, nonanal, hotrienol, isophorone, lilac aldehyde A, 1‐nonanol, decanal, 4‐vinyl‐2‐methoxyphenol and (E)‐β‐damascenone showed the highest values and should be considered as the most odour‐active compounds, particularly (E)‐β‐damascenone, nonanal and decanal.     

Release of Five Indicator Volatiles from a Model Meat Emulsion to Study Phase Contribution to Meat Aroma

The objective of this work was to develop a model meat emulsion in order to study the release of aroma-related compounds from the lipid and aqueous phases. Hexanal, octanal and nonanal were taken as indicators of lipid oxidation whereas 2-ethyl-3,5-dimethyl pyrazine and 2-methyl pyrazine were Maillard reaction indicators. Four systems were studied: I) a model meat emulsion; II) phosphate buffer; III) phosphate buffer + myofibrillar proteins; and IV) canola oil. Release of indicator compounds from each of the studied systems was analyzed in the headspace. It was concluded that pyrazines mainly contributed to aroma in lipid systems and in protein solutions but not in emulsions and non protein aqueous systems. Hexanal, octanal, and nonanal were minor aroma contributors in lipid media, whereas hexanal and nonanal were released in small amount from protein emulsions. Conversely, octanal can be considered of an important aroma contributor in emulsions; the three aldehydes showed a high release from aqueous systems, with and without protein.     

洋河系列绵柔型白酒香气成分研究

利用液液萃取法提取洋河系列绵柔型白酒中的香气化合物,通过气相色谱-闻香法(GC-O)及气相色谱-质谱(GC-MS)技术对其进行鉴定。在具有典型绵柔型特征的海之蓝、天之蓝和梦之蓝三种酒中分别检测出55、57和59种呈香化合物。研究发现洋河系列绵柔型白酒的主要风味物质为己酸乙酯,对其风味有较大贡献的还有己酸、丁酸乙酯、二甲基三硫、三甲基吡嗪、γ-壬内酯。此外,在海之蓝中苯乙醛、3-甲基丁醇、庚酸乙酯、己酸-3-甲基丁酯、丁酸、乙酸对其风味贡献较大;天之蓝中1-辛烯-3-酮、辛酸乙酯、2-乙酰基-5-甲基呋喃、丁酸香气强度较大;梦之蓝中1-辛烯-3-酮、己酸-3-甲基丁酯、2-羟基-3-甲基丁酸乙酯、辛酸乙酯、4-甲基苯酚、庚酸乙酯香气强度较大。     

The influence of Debaryomyces hansenii and Candida utilis on the aroma formation in garlic spiced fermented sausages and model minces

The influence of the yeast starter cultures Debaryomyces hansenii and Candida utilis on fermented meat aroma was studied in model minces and in commercial-type fermented sausages. Volatile compounds from model minces and sausages were collected using diffusive and dynamic headspace sampling respectively and were identified by gas chromatography/mass spectrometry (GC/MS). A triangle test was carried out on the sausages to detect whether the yeast influenced the sausage odour. C. utilis demonstrated high metabolic activity in the model minces, producing several volatile compounds, in particularly esters. C. utilis also seemed to ferment the amino acids valine, isoleucine and leucine into compounds important for the aroma of sausages. D. hansenii on the contrary, had very little effect on the production of volatile compounds in the model minces. In the sausage experiment both yeast cultures died out before the ripening process ended and the sensory analysis showed only a slight difference between the sausages. A fungistatic test of the garlic powder added to the sausages indicated that garlic inhibits the growth of the yeast starter cultures.     

Ability of meat starter cultures to catabolize leucine and evaluation of the degradation products by using an HPLC method

The degradation of leucine generates aroma compounds involved in the typical flavour of dry fermented sausage. The ability of lactic acid bacteria and staphylococci of meat origin to produce aromatic compounds from leucine was studied. Whole cells were incubated with³H-labelled leucine under different conditions. The radioactive metabolites produced were analysed by high performance liquid chromatography. All the strains studied were able to catabolise leucine but catabolic profiles were quantitatively and qualitatively different. The catabolism of leucine by Lactobacillus sakei,Lactobacillus curvatus and Pediococcus acidilactici was very low and required α -ketoglutarate, which indicates that an aminotransferase was involved in the first step of leucine catabolism. Carnobacterium piscicola produced a large amount of 3-methyl butanal, whereas Staphylococcus carnosus mainly produced 3-methyl butanoic acid. Leucine was mainly degraded into α -ketoisocaproic acid by Lactobacillus plantarum and Carnobacterium divergens. Nitrate affected leucine catabolism only in S. carnosus.     

Evaluation of volatile flavour compounds from cashew apple (Anacardium occidentale L) juice by the Osme gas chromatography/olfactometry technique

The headspace volatile components of the juice of cashew apples from a commercial Brazilian dwarf genotype were separated by high‐resolution gas chromatography and identified by GC/MS. Five judges evaluated the GC effluents using the Osme technique in order to determine the importance of each compound to the characteristic cashew aroma. Esters methyl 3‐methyl butanoate, ethyl 3‐methyl butanoate, methyl butanoate, ethyl butanoate, ethyl trans‐2‐butenoate and methyl 3‐methyl pentanoate were important to the sweet, fruity and cashew‐like aroma. Cis‐3‐hexenol, hexanal and 2‐methyl‐2‐pentenal presented different green notes. In spite of the flame ionisation detector being unable to detect sulphur compounds, the olfactometric analysis revealed chromatographic regions where sulphur‐like odours were perceived by the Osme sensory panel. The most intense unpleasant odour was due to 2‐methyl butanoic acid, which was described as very stinky. The sensory panel showed good olfactory sensitivity and reproducibility. Sensory and instrumental data correlation allowed a greater understanding of the role of several volatile compounds in the sensory quality of the juice. Copyright © 2003 Society of Chemical Industry