Analysis of early lipid oxidation in smoked, comminuted pork or poultry sausages with spices

Dynamic headspace/gas chromatography-mass spectrometry (GC-MS), front-face fluorescence spectroscopy, and a gas-sensor array technique (electronic nose) have previously detected lipid oxidation in pork back fat or mechanically recovered poultry meat earlier than or at the same time as a sensory panel. The present study was focused on measurement of early lipid oxidation in a more complicated product (freeze-stored, smoked sausages with spices). During the storage time, formation of components contributing to rancid odor and flavor (e.g., hexanal and 1-penten-3-ol) could be monitored with dynamic headspace/GC-MS. The GC-MS data also showed a decrease in 2-furancarboxaldehyde, which could indicate loss of Maillard type components often associated with acidic or meat odor and flavor. The fluorescence spectra were difficult to interpret, probably due to the simultaneous influence from increasing levels of lipid oxidation products and loss of fluorescent Maillard or spice components. The gas-sensor array responses were dominated by signals from, e.g., spice and smoke compounds.     

Volatile constituents of wild citrus Mangshanyegan (Citrus nobilis Lauriro) peel oil

Volatiles of a wild mandarin, Mangshanyegan (Citrus nobilis Lauriro), were characterized by GC-MS, and their aroma active compounds were identified by aroma extract dilution analysis (AEDA) and gas chromatography-olfactometry (GC-O). The volatile profile of Mangshanyegan was compared with those of other four citrus species, Kaopan pummelo (Citrus grandis), Eureka lemon (Citrus limon), Huangyanbendizao tangerine (Citrus reticulata), and Seike navel orange (Citrus sinensis). Monoterpene hydrocarbons predominated in Mangshanyegan, in particular d-limonene and β-myrcene, which accounted for 85.75 and 10.89% of total volatiles, respectively. Among the 12 compounds with flavor dilution factors (FD) = 27, 8 oxygenated compounds, including (Z)- and (E)-linalool oxides, were present only in Mangshanyegan. The combined results of GC-O, quantitative analysis, odor activity values (OAVs), and omission tests revealed that β-myrcene and (Z)- and (E)-linalool oxides were the characteristic aroma compounds of Mangshanyegan, contributing to the balsamic and floral notes of its aroma.     

基于电子鼻的鱼露香气品质识别

为了识别鱼露的品质,并为缩短发酵周期的工艺优选提供理论依据.利用电子鼻对7种鱼露样品的挥发性气味进行了分析,并与项空-气质联用( GC-MS)和感官分析结果进行比较.结果表明:鱼露香气成分复杂,工艺改良对气味影响很大,电子鼻18个金属传感器能很好地将不同样品的气味进行识别.以传统发酵原汁鱼露为标样,电子鼻分析结果表明,加曲改良工艺的4号样品与标样香气最为接近,相似系数达87.8％,该结果与GC-MS数据和感官分析结果一致,可为鱼露速酿工艺的优选提供参考.     

Characteristic odor components of kumquat (Fortunella japonica Swingle) peel oil

This study was conducted to determine the composition of kumquat (Fortunella japonica Swingle) cold-pressed peel oil and to determine which volatile components are primarily responsible for the aroma of this oil. Eighty-two compounds were identified in the oil by GC and GC-MS. The major compounds were limonene (93.73%), myrcene (1.84%), and ethyl acetate (1.13%). Flavor dilution (FD) factors and relative flavor activities (RFA) of volatile constituents were evaluated by aroma extract dilution analysis with gas chromatography-olfactometry (GC-O). Camphene, terpinen-4-ol, citronellyl formate, and citronellyl acetate showed high FD factors (>/=5) and RFA (>20). Citronellyl formate and citronellyl acetate were regarded as the characteristic odor components of the kumquat peel oil from the results of FD factor, RFA, and GC-sniffing. Citronellyl acetate is considered to be the odor component most similar to kumquat by organoleptic evaluation with GC-O.     

加热温度对牡蛎挥发性风味成分的影响

为探讨牡蛎挥发性风味与加工温度的关系,运用电子鼻和顶空固相微萃取气质联用技术（HS-SPME-GC-MS）对不同温度加热牡蛎的挥发性成分进行分析。结果表明,电子鼻能够灵敏地检测到牡蛎在加热过程中气味的变化,新鲜牡蛎在加热到1000C和1500C时气味发生明显变化。通过GC-MS从新鲜牡蛎、100℃加热牡蛎和150℃加热牡蛎中分别检出47、59和56种挥发性物质,己醛、反-2-,顺-6-壬二烯醛、庚醛、辛醛等醛类物质对新鲜牡蛎的风味影响较大,使其具有腥味、蘑菇及黄瓜的风味;经过100℃加热后,牡蛎的腥味减弱,肉香浓郁,醛类和杂环化合物是其主要的挥发性风味物质;150℃加热牡蛎的主要挥发性物质是烃类,杂环化合物对其烘烤风味的形成具有重要作用。     

电子鼻结合HS-SPME-GC-MS分析辐照对甲鱼预制菜挥发性风味成分的影响

为了探究辐照对甲鱼预制菜挥发性风味成分的影响,采用0、4.7、7.1、9.9 kGy剂量⁶⁰Co-γ射线辐照处理甲鱼预制菜,通过感官评定并利用电子鼻结合顶空固相微萃取-气相色谱-质谱联用技术(HS-SPME-GC-MS)分析辐照前后挥发性风味成分的变化。结果表明,5 kGy以内剂量辐照对甲鱼预制菜的感官品质无明显影响,高于5 kGy会影响其气味和滋味,进而可能产生异味。辐照对甲鱼预制菜特征气味引起的差异主要表现在传感器响应值较高的芳香成分和有机硫化物、氮氧化合物、甲烷、醇类和醛酮类物质,利用主成分分析(PCA)和线性判别分析(LDA)能够有效区分经不同剂量辐照处理的甲鱼预制菜。4.7 kGy组与对照组气味差异较小,7.1、9.9 kGy组与对照组差异相对较大。不同剂量辐照后甲鱼预制菜挥发性成分的种类增加,醛类、酸类相对含量降低,烃类、芳香族类、酮类、酯类相对含量升高,醇类、含氮含硫及杂环类相对含量先降低后升高。相对气味活度值(ROAV)分析结果表明,壬醛、癸醛、辛醛、己醛、庚醛、1-辛烯-3-醇和2-戊基呋喃是甲鱼预制菜的关键风味成分,苯甲醛、苯乙醛、(E,E)-2, 4-癸二烯醛对其风味具有重要修饰作用。辐照后辛醛、己醛、1-辛烯-3-醇对甲鱼预制菜总体风味的贡献率降低,庚醛、2-戊基呋喃的贡献率先降低后增加,苯乙醛的贡献率增加并成为关键风味成分。因此,建议采用不超过5 kGy剂量的⁶⁰Co-γ射线辐照处理甲鱼预制菜,在杀菌的同时最大限度保持其原有风味。本研究结果为辐照技术在甲鱼预制菜杀菌保鲜中的应用提供了科学依据。     

Key odorants of Oscypek, a traditional Polish ewe's milk cheese

The unique flavor of Oscypek, a Polish ewe's milk smoked cheese, is described as slightly sour, piquant, salted, and smoked. In this paper with the application of gas chromatography-olfactometry (GC-O) and combination of aroma extract dilution analysis (AEDA) 20 potent odorants of this cheese have been identified within the flavor dilution factor (FD) range of 4-2048. Among them, 2-methoxyphenol, 2-methoxy-4-methylphenol, 4-methylphenol, and butanoic acid showed the highest FD factors. Quantification results based on labeled standard addition followed by calculation of odor activity values (OAV) of 13 compounds with the highest FD factors revealed that 11 compounds were present at concentrations above their odor threshold values and therefore mostly contribute to the overall aroma of smoked ewe's milk cheese. Six of those compounds were represented by phenolic derivatives, with the highest OAV for 2-methoxyphenol (1280). Analysis of key odorants of an unsmoked cheese sample showed that the smoking process had a fundamental influence on Oscypek aroma formation.     

Comparison of odor-active compounds from six distinctly different rice flavor types

Using a dynamic headspace system with Tenax trap, GC-MS, GC-olfactometry (GC-O), and multivariate analysis, the aroma chemistry of six distinctly different rice flavor types (basmati, jasmine, two Korean japonica cultivars, black rice, and a nonaromatic rice) was analyzed. A total of 36 odorants from cooked samples were characterized by trained assessors. Twenty-five odorants had an intermediate or greater intensity (odor intensity >or= 3) and were considered to be major odor-active compounds. Their odor thresholds in air were determined using GC-O. 2-Acetyl-1-pyrroline (2-AP) had the lowest odor threshold (0.02 ng/L) followed by 11 aldehydes (ranging from 0.09 to 3.1 ng/L), guaiacol (1.5 ng/L), and 1-octen-3-ol (2.7 ng/L). On the basis of odor thresholds and odor activity values (OAVs), the importance of each major odor-active compound was assessed. OAVs for 2-AP, hexanal, ( E)-2-nonenal, octanal, heptanal, and nonanal comprised >97% of the relative proportion of OAVs from each rice flavor type, even though the relative proportion varied among samples. Thirteen odor-active compounds [2-AP, hexanal, ( E)-2-nonenal, octanal, heptanal, nonanal, 1-octen-3-ol, ( E)-2-octenal, ( E, E)-2,4-nonadienal, 2-heptanone, ( E, E)-2,4-decadienal, decanal, and guaiacol] among the six flavor types were the primary compounds explaining the differences in aroma. Multivariate analysis demonstrated that the individual rice flavor types could be separated and characterized using these compounds, which may be of potential use in rice-breeding programs focusing on flavor.     

Odor-active compounds in cooked rice cultivars from Camargue (France) analyzed by GC-O and GC-MS

Volatile compounds of cooked rice from scented (Aychade, Fidji) and nonscented (Ruille) cultivars grown in the Camargue area in France were compared to that of a marketed Asian scented one (Thai) by gas chromatography-olfactometry (GC-O) and gas chromatography-mass spectrometry (GC-MS). GC-O analyses of the organic extracts resulted in the perception of 40 odorous compounds. Only two compounds, oct-1-en-3-one and 2-acetyl-1-pyrroline, were almost always perceived. Hierarchical cluster analysis showed that most of the difference between rice odors was linked to quantitative differences with only 11 compounds being specific to some of the rice. Sixty compounds were identified and quantified by GC-MS, including a few new odor-active components. Principal component analysis enabled us to differentiate scented cultivars from a nonscented one, and scented rice cultivars from Camargue from a Thai sample. Calculated odor-active values evidenced that the Thai sample odor differed from that of scented Camargue cultivars because of the degradation of lipids and of cinnamic acid compounds.     

Characterization of volatile compounds contributing to naturally occurring fruity fermented flavor in peanuts

Published research has indicated that ethyl 2-methylpropanoate, ethyl 2-methybutanaote, ethyl 3-methylbutanoate, hexanoic acid, butanoic acid, and 3-methylbutanoic acid are responsible for fruity fermented (FF) off-flavor; however, these compounds were identified in samples that were artificially created by curing immature peanuts at a constant high temperature. The objective of this study was to characterize the volatile compounds contributing to naturally occurring FF off-flavor. Volatile compounds of naturally occurring FF and no-FF samples were characterized using solvent-assisted flavor evaporation (SAFE), solid phase microextraction (SPME), gas chromatography-olfactometry (GC-O), and gas chromatography-mass spectrometry (GC-MS). Aroma extract dilution analysis (AEDA) identified 12 potent aroma active compounds, none of which were the previously identified esters, with no consistent differences among the aroma active compounds in no-FF and FF samples. Hexanoic acid alone was identified in the naturally occurring FF sample using the SAFE GC-MS methodology, whereas two of the three previously identified esters were identified in natural and artificially created samples. The same two esters were confirmed by SPME GC-MS in natural and artificially created samples. This study demonstrated the need for caution in the direct application of data from artificially created samples until those compounds are verified in natural samples. However, these results suggest that a laboratory method using SPME-GC techniques could be developed and correlated on an ester concentration versus FF intensity basis to provide an alternative to sensory analysis for detection of FF off-flavor in peanut lots.     

Identification of the volatile component(s) causing the characteristic foxy odor in various cultivars of Fritillaria imperialis L. (Liliaceae)

To identify the component(s) causing the foxy odor, characteristic for some Fritillaria imperialis cultivars, the headspace of flower bulbs was analyzed using gas chromatography-olfactometry (GC-O) and GC-mass spectrometry (GC-MS). Six Fritillaria species and cultivars were selected as follows: F. imperialis cv. Premier (very strong foxy odor), F. imperialis cv. Lutea (strong foxy odor), F. imperialis ssp. Inodora (no odor), Fritillaria eduardii (weak mousy odor), Fritillaria raddeana (no odor), and an F1 of F. imperialis Lutea x Inodora (weak foxy odor). Volatiles from these flower bulbs were accumulated on Tenax and injected into the GC by thermodesorption. The majority of the volatiles consisted of low molecular weight aliphatic compounds. GC-O revealed that the foxy odor was caused by a single component, identified as 3-methyl-2-butene-1-thiol on the basis of smell in GC-O analyses (two GC columns), mass spectra, and retention times. Chemical identification was substantiated by GC-O and GC-MS of an authentic standard of 3-methyl-2-butene-1-thiol, prepared by organic synthesis.     

Differences in odor-active compounds of trincadeira wines obtained from five different clones

Odorant compounds of five young clonal red wines made from cv. Trincadeira, a native grape variety of Vitis vinifera L. grown in Portugal, were studied using 2001 and 2003 vintages. The study was carried out using gas chromatography-mass spectrometry (GC-MS) for compound identification and the gas chromatography-olfactometry (GC-O) posterior intensity method to detect the potentially most important aroma compounds. Forty-one odorant peaks were detected by GC-O analysis, from which 31 were identified by GC-MS. The odorant compounds with the highest odorant average intensities are 3-methylbutanoic acid, 2-phenylethanol, 2,5-dimethyl-4-hydroxy-3(2H)-furanone, and 4-vinylguaiacol. The GC-O analysis showed odor intensity differences among compounds, which was confirmed by analysis of variance (ANOVA). Principal component analysis (PCA) and hierarchical cluster analysis (HCA) showed that the five clonal wines from the 2001 vintage were more similar than those from the 2003 vintage. Moreover, stepwise linear discriminant analysis (SLDA) demonstrated that the factor vintage has influence on the Trincadeira clonal red wine odorant profile differentiation.     

Characterization of Royal Gala apple aroma using electronic nose technology-potential maturity indicator

Changes in aroma of apple harvested at four different maturities were measured at harvest and after short-term storage using electronic aroma sensors ("electronic nose") and classical headspace/gas chromatography methods. Stored fruits were also evaluated by a trained sensory panel. Compared with headspace/gas chromatography, the electronic nose was found to be more sensitive ( approximately 40 times) in terms of sample size. The sampling procedure for the electronic nose was much less complex. Using discriminant function analysis, both methods classified the apples tested into groups according to harvest date. After storage, the groupings were more diffuse. Results from sensory testing showed partial separation along the first linear discriminant but did not classify the apple into distinct groups. Important differences between treatments were found for "overall flavor", "acid flavor" intensity, "crispness", "cider/fermented aroma", "vegetative aroma", and "canned pear aroma".     

HS-SPME/GC-MS和电子感官技术分析毛霉型豆豉发酵过程中风味品质

为了对毛霉型豆豉发酵过程中风味进行综合评价,本试验采用顶空固相微萃取/气相色谱-质谱法(HS-SPME/GC-MS)结合电子鼻、电子舌对其发酵过程进行研究。结果表明,毛霉型豆豉不同发酵时期的11个样品共鉴定出68种挥发性风味成分,其中包括酯类18种、醛类7种、酸类3种、醇类26种、酮类4种、其他类10种。挥发性风味成分的种类由前发酵的15种上升至豆豉发酵成熟时(35~42 d)的31种,含量由前发酵1.69 μg·g^-1上升至发酵终点44.20 μg·g^-1,呈递增趋势,至发酵成熟期稳定,与电子鼻测定结果一致。电子舌测定结果显示,后发酵35 d时,成品的涩味、苦味及苦味回味降到适宜程度,鲜味和丰富性较高,而此时的挥发性风味成分种类丰富、含量高、香味浓郁、丰富性好,滋味和气味俱佳。因此,HS-SPME/GC-MS结合电子感官技术对毛霉型豆豉产品品质的判别具有可行性,可为生产条件的优化提供理论依据。     

Volatile components and key odorants of fennel (Foeniculum vulgare Mill.) and thyme (Thymus vulgaris L.) oil extracts obtained by simultaneous distillation-extraction and supercritical fluid extraction

Volatile oil extracts of fennel seeds (Foeniculum vulgare Mill.) and thyme leaves (Thymus vulgaris L.) were obtained by simultaneous distillation-extraction (SDE) and supercritical fluid extraction (SFE) and analyzed by gas chromatography-mass spectrometry (GC-MS). In general, fennel oil extracted by SDE and SFE showed similar compositions, with trans-anethole, estragole, and fenchone as the main components. In contrast, thymol and p-cymene, the most abundant compounds in thyme leaves, showed big differences, with generally higher amounts of monoterpenes obtained by SDE. However, in this case, the differences between the extracts were higher. Key odorants of fennel seeds determined by gas chromatography-olfactometry (GC-O) showed similar patterns when applying SDE and SFE. trans-Anethole (anise, licorice), estragole (anise, licorice, sweet), fenchone (mint, camphor, warm), and 1-octen-3-ol (mushroom) were the most intense odor compounds detected in fennel extracts. Thymol and carvacrol, with oregano, thyme, and spicy notes, were identified as key compounds contributing to the aroma of thyme leaves.     

Aroma compounds of fresh milk from New Zealand cows fed different diets

Volatile compounds were extracted from fresh milk produced by New Zealand cows using the newly developed solvent-assisted flavor evaporation (SAFE) technique. The two samples that were used came from cows that had been fed on different diets and represented the considerably different flavors of Northern hemisphere and New Zealand milk. Using gas chromatography-olfactometry (GC-O), 71 aroma compounds were found from the milk extracts, 66 of which were identified. Nearly all of the aroma compounds were common to both extracts, despite the two milk samples having quite different flavors. Only one compound, gamma-12:2 lactone, was significantly odor-active for the extract of milk from cows fed a supplement diet, but was not found for the extract of milk from cows fed a pasture diet. Thus, differences in milk flavor are primarily caused by concentration differences of a common set of flavor compounds, rather than by the occurrence of compounds uniquely associated with a particular feed.     

Gas chromatography-olfactometry (GC-O) and proton transfer reaction-mass spectrometry (PTR-MS) analysis of the flavor profile of grana padano,parmigiano reggiano,and grana trentino cheeses

Gas chromatography-olfactometry (GC-O) and proton transfer reaction-mass spectrometry (PTR-MS) techniques were used to deduce the profile of odor-active and volatile compounds of three grana cheeses: Grana Padano (GP), Parmigiano Reggiano (PR), and Grana Trentino (GT). Samples for GC-O analysis were prepared by dynamic headspace extraction, while a direct analysis of the headspace formed over cheese was performed by PTR-MS. The major contributors to the odor profile were ethyl butanoate, 2-heptanone, and ethyl hexanoate, with fruity notes. A high concentration of mass 45, tentatively identified as acetaldehyde, was found by PTR-MS analysis. Low odor threshold compounds, e.g., methional and 1-octen-3-one, which contributed to the odor profile but were not detected by FID, were detected by PTR-MS. Principal component analysis on both GC-O and PTR-MS data separated the three cheese samples well and showed specific compounds related to each sample.