Effect of enzyme activity and frozen storage on jalapeño pepper volatiles by selected ion flow tube-mass spectrometry

Abstract: Samples of unblanched (fresh), stannous chloride-treated, or blanched jalapeño peppers were measured for real-time generation of lipoxygenase-derived volatiles during 10 min after tissue disruption. Volatiles were also measured before and after 1.5, 2.5, 3, 6, and 9 mo of frozen storage at −15 °C. The concentration of all lipoxygenase-derived compounds was significantly higher in unblanched jalapeño peppers compared to enzyme inhibited peppers. The maximum concentration of (Z)-3-hexenal, (E)-2-hexenal, and hexanal was detected at about 1.2, 1.5, and 1.5 min after tissue disruption, respectively. A decrease in (Z)-3-hexenal and an increase in dimethyl sulfide and methylbutanal occurred in blanched compared to stannous chloride-treated peppers due to heat. Frozen storage resulted in no major changes in the lipoxygenase-derived volatiles of whole and pureed blanched peppers after 9 mo. However, in whole unblanched peppers a gradual decrease of (Z)-3-hexenal, (E)-2-hexenal, hexanal, hexenol, and hexanol was observed over time; whereas in pureed unblanched peppers these compounds increased, reached maximum concentration, and then decreased. Similarly, the minor volatiles 2-pentenal, 1-penten-3-one, (E)-2-heptenal, (E)-2-octenal, and (E)-2-nonenal showed an initial increase followed by a decline in both whole and pureed unblanched peppers. Tissue disruption increased generation and degradation rates during frozen storage. The compounds (E,Z)-2,6-nonadienal, n-propyl aldehyde, 2-isobutyl-3-methoxypyrazine, and a mixture of terpenes decreased in unblanched and blanched frozen samples, while nonanal and methylbutanal increased only in unblanched samples. Practical Application: Data obtained in this study contribute to the understanding of the dynamics of lipoxygenase-derived volatile formation upon tissue disruption of jalapeño pepper. In addition, it contributes to generate knowledge on the effect of processing techniques, namely blanching and frozen storage, on the volatile profile of these peppers. This knowledge has applications in the manufacturing, product development, and quality control areas of the food industry as useful information to help in the designing and monitoring of processes aimed to obtain products with specific aroma characteristics. For instance, maximum levels of “fresh” and “green” aroma compounds are achieved rapidly during the first few minutes after pepper tissue is disrupted. The inhibition of enzyme activity shortly after this may help to maximize concentration of these aroma notes in the product. Frozen storage produces enzymatic and chemical changes in the volatile profile of unblanched peppers. The aroma profile of blanched peppers is more stable under frozen conditions, with a lower total volatile concentration.     

鲜黄芪和干黄芪挥发性化学成分比较分析

采用同时蒸馏-萃取法提取,用气相-色谱质谱联用法结合计算机谱图检索,对鲜黄芪和干黄芪挥发性化学成分进行分析鉴定。结果表明：鲜黄芪和干黄芪挥发性成分的得率分别为0.64%、0.43%,鲜黄芪和干黄芪共鉴定出挥发性成分76种;二者的共有成分为正己醇、(E)-2-己烯-1-醇、正己醛、己-2-烯醛等11个化合物;鲜黄芪中鉴定出43种挥发性成分,主成分是正己醇、邻二甲苯、(E)-2-己烯-1-醇、(E)-2-己烯醛、正己醛;干黄芪中鉴定出44种香气成分,主成分是正己醛、正己醇、己-2-烯醛。干黄芪挥发性成分与新鲜黄芪挥发性成分相比较组成和相对含量存在着较大差异。     

Comparison of Tomatillo and Tomato Volatile Compounds in the Headspace by Selected Ion Flow Tube Mass Spectrometry (SIFT-MS)

ABSTRACT: The concentration of 31 volatiles were measured in the headspace of tomatillos using selected ion flow tube-mass spectrometry (SIFT-MS), and were compared with those in vine-ripened tomato, roma tomato, cherry tomato, and grape tomato. None of the volatiles were higher in the headspace of tomatillos than of tomatoes. Compounds (E)-2-octenal, (E)-2-pentenal, 2-isobutylthiazole, 6-methyl-5-hepten-2-one, and phenylacetaldehyde were significantly lower in tomatillo than in the tomato varieties in the headspace. After blending, volatiles in the headspace increased, and then decreased after reaching a maximum concentration, due to further degradation or depletion. Compounds (E)-2-pentenal and 1-penten-3-one reached a maximum concentration later than (E)-2-hexenal, (Z)-3-hexenal, and hexanal for tomatillo and tomatoes. The slope of the ratio of (E)-2-hexenal and (Z)-3-hexenal was not significantly different for any of the samples, implying that the activity of cis/trans isomerase was not different between tomatillos and tomatoes.     

Effect of enzymes on strawberry volatiles during storage, at different ripeness level, in different cultivars, and during eating

Strawberry samples with enzyme activity and without enzyme activity (stannous chloride added) were measured for real-time formation of lipoxygenase (LOX) derived aroma compounds after 5 min pureeing using selected ion flow tube-mass spectrometry (SIFT-MS). The concentration of (Z)-3-hexenal and (E)-2-hexenal increased immediately after blending and gradually decreased over time, while hexanal concentration increased for at least 5 min in ground strawberries. The formation of hexanal was slower than the formation of (Z)-3-hexenal and (E)-2-hexenal in the headspace of pureed strawberries. The concentration of LOX aldehydes and esters significantly increased during refrigerated storage. Damaging strawberries increased the concentration of LOX aldehydes but did not significantly affect the concentration of esters. The concentrations of many of the esters were strongly correlated to their corresponded acids and/or aldehydes. The concentration of LOX-generated aldehydes decreased during ripening, while fruity esters increased. Different varieties had different aroma profiles and esters were the greatest percentage of the volatiles. The aroma release of some of the LOX-derived aldehydes in the mouthspace in whole strawberries compared to chopped strawberries showed that these volatiles are formed in the mouth during chewing. The persistence of LOX-derived compounds was higher than esters after swallowing. The mouthspace after and before swallowing persistence ratio of esters decreased as the chain length of the acid part of the ester compounds increased in whole strawberries. PRACTICAL APPLICATION: The storage studies showed that the concentrations of fruity and fresh volatiles increased during ripening and storage while damaging only increases the fresh volatiles. The nose, mouth, and headspace information can be used in the flavor industry to improve the formula of natural strawberry flavor by considering human perception during eating.     

GC-O结合OAV鉴定陇南初榨橄榄油关键香气成分

选取甘肃陇南代表性品种莱星和鄂植8号初榨橄榄油及消费口碑良好的特级混合初榨橄榄油为研究对象,通过气相色谱-质谱（gas chromatography-mass spectrometry,GC-MS）检测比较3 种初榨橄榄油的挥发性物质组成,同时采用气相色谱-嗅闻（gas chromatography-olfactometry,GC-O）技术筛选其香气活性物质,最后结合香气活性值（odor activity value,OAV）分析各呈香组成对橄榄油香气轮廓呈现的贡献性,从而鉴定出3 种橄榄油各自的关键香气成分。结果表明：采用GC-MS在莱星、特级混合及鄂植8号初榨橄榄油中各检测出35、30 种及25 种挥发性成分,其中己醇、3-己烯-1-醇、(E)-2-己烯-1-醇和(E)-2-己烯醛的含量丰富。采用GC-O在3 种初榨橄榄油中各筛选出13、15 种和12 种香气活性成分,包含具有青草特征的C6化合物、呈现油脂香气的庚醛和(E,E)-2,4-癸二烯醛以及表现其他气味信息的香气物质。OAV分析发现3 个样品各有12、13 种及11 种关键香气成分（OAV≥1）,以1-辛烯-3-醇、芳樟醇、(E)-2-己烯醛和(E,E)-2,4-癸二烯醛为代表的OAV较高,对初榨橄榄油呈香品质具有重要作用。本研究筛选出3 种初榨橄榄油的关键香气成分,结果可为提升初榨橄榄油风味品质提供理论基础。     

顶空固相微萃取-气相色谱-质谱法分析东北油豆角挥发性成分

采用顶空固相微萃取气相色谱-质谱法对东北油豆角挥发性物质进行检测分析,为优质栽培、品质育种及贮藏加工提供参考。结果表明,油豆角挥发成分包括醛、醇、酮、酸、酯、烃、呋喃及醚等类物质。未加工青荚中鉴定出48 种挥发成分,主要为2-己烯醛（相对含量为40.01%）、己醇（12.64%）、己醛（11.40%）,与3-己烯-1-醇、反-2-己烯醛、反-2-顺-6-壬二烯醛、3-甲基-1-丁醇、2-乙基己醇、反,反-2,4-庚二烯醛、反-2-壬烯醛、β-环柠檬醛、肉豆蔻醛等物质共同作用形成青豆荚气味;可食熟荚中鉴定出26 种挥发成分,主要为1-辛烯-3-醇（48.77%）,与顺-4-庚烯醛、3-甲硫基丙醛,反-2-庚烯醛、辛醛、壬醛、香叶基丙酮等共同作用形成油豆角特异
芳香性质。     

大白菜风味物质的气相色谱-质谱分析

利用顶空固相微萃取和气相色谱- 质谱联用分析技术,对12 个大白菜试材进行连续2 年的风味物质成分分析。共检测鉴定出了腈类、酯类、醛类、酮类、醇类、烃类及杂环类等14 类170 多种化合物。主要的风味物质有45 种,初步认为2- 环己烯-1- 醇、2- 己烯醛、3- 己烯-1- 醇、苯丙腈和苯乙基异硫氰酸酯等5 种成分为大菜的特征性风味物质。     

Comparative study of extra virgin olive oil flavor profile of Koroneiki variety (Olea europaea var. Microcarpa alba) cultivated in Greece and Tunisia during one period of harvesting

The effects of geographical region, irrigation and ripening degree of olives on the profile of volatile compounds isolated by monovarietal virgin olive oils from Crete and Tunisia of Koroneiki variety (Olea europaea var. Microcarpa alba) using the SPME GC/MS technique were investigated. Fruits obtained from Greece (island of Crete) and Tunisia (Sfax region) were picked at three and two different growth stages respectively and then immediately processed. The most important compounds identified were esters, alcohols, carbonyl compounds and hydrocarbons. The main volatile compounds present in the oil samples were C6 derivatives, such as [E]-2-hexenal, [E]-2-hex-1-enol, [Z]-3-hexen-1-ol and 1-hexanol. In addition to C6 compounds, the aroma of the studied samples contained reasonable amounts of various classes of C5 components. The tested oil samples showed different volatile profiles. Specifically, the concentration of total esters, carbonyl, C6 and C5 compounds increased significantly with the ripening degree in Cretan, but not in Tunisian olive oils. Principal component analysis of the results indicated that primary maturity and geographical region rather than irrigation affected significantly the volatile’s profile of olive oil.     

基于ATD-GC-MS技术检测铁观音做青过程环境挥发性成分的动态变化

采用全自动热脱-气相色谱-质谱法捕集和检测铁观音做青关键工艺节点的环境挥发性成分，应用短时间序列表达挖掘器（short time-series expression miner,STEM）和偏最小二乘法判别分析（partial least squaresdiscriminantanalysis,PLS-DA）对铁观音做青过程中挥发性成分进行分析。结果显示，铁观音做青环境中共鉴定出122种挥发性成分，包括醇类、酯类、烯烃类、烷烃类、醛类、芳香烃类、酮类和其他化合物8大类，其中酯类是做青环境中的主要挥发物；STEM结果表明，检测出的挥发性成分可划分成19种变化趋势，且在2种趋势模型中有显著性富集，其中仲丁醇、乙酸乙酯、异戊醛、异戊醇、正己醇、2-庚醇、己酸甲酯、甲基庚烯酮、异丁酸辛酯等挥发性成分带有特殊香气并随着做青次数的增加而显著增加；PLS-DA结果表明，摇青和晾青两部分可有效区分开，并鉴定出7种共同特征挥发性成分（变异权重参数值>1）:(Z)-乙酸-4-己烯-1-酯、反-3-己烯基丁酯、叶醇、3-己烯醛、异戊腈、(3E)-4,8-二甲基壬-1,3,7-三烯、罗勒烯异构体混合物。...     

Flavour quality of tomatoes

Tomato volatiles present in essential oils obtained by steam distillation–continuous extraction and by head-space condensation were identified and evaluated organoleptically. Flavour quality of different samples of fresh tomatoes, evaluated by a panel, could be related to the occurrence and concentration of n-hexanal, trans-2-hexenal, cis-3-hexen-1-ol, 2-isobutylthiazole and some unidentified compounds in the head space condensation essential oil.     

Comparison of Volatile Release in Tomatillo and Different Varieties of Tomato during Chewing

ABSTRACT: The release of volatiles from tomatillos (Physalis ixocarpa Brot.) and tomatoes in the mouthspace and nosespace was measured in real-time using selected ion flow tube mass spectrometry (SIFT-MS). (Z)-3-Hexenal, (E)-2-hexenal, hexanal, and 1-penten-3-one increased, while isobutyl alcohol, nonanal, and methylbutanal showed no significant change in the first 30 s of chewing. Cherry tomato released more (E)-2-hexenal, (Z)-3-hexenal, and 1-penten-3-one than tomatillo, Roma tomato, and vine-ripened tomato during chewing. The proportion of the average concentration of volatiles in the mouthspace after swallowing to before swallowing (MSas/MSbs) varied from 2.8% to 73.9% between different volatiles and varieties. Methylbutanal, hexanal, and nonanal were retained at a higher percentage in the mouth after swallowing than (Z)-3-hexenal, (E)-2-hexenal, 1-penten-3-one, and isobutyl alcohol. The proportion of the average volatile concentration in the mouthspace, to the headspace in a glass container (MS/HS) of 1-penten-3-one, hexanal, methylbutanal, and nonanal, and the proportion of nosespace to headspace (NS/HS) for 1-penten-3-one, hexanal, (Z)-3-hexenal, and nonanal was significantly higher in tomatillo than in tomatoes. There was no difference between tomatoes of different varieties in NS/HS ratio. Practical Application: The real-time volatile release from tomatillos and tomatoes was measured and compared. The information obtained on the dynamic generation of volatile compounds provides a better understanding of volatile release in the headspace of tomatillo and tomatoes. The compounds and their volatile release patterns were similar for the tomatillo and tomatoes. The green aldehydes released during chewing were not significantly higher than most tomato varieties, except for Roma tomatoes. Cherry tomato released relatively more volatiles during chewing, whereas Roma tomatoes were generally poor in mouthspace volatiles. The lingering of volatiles in the mouth after swallowing was different for different volatiles and varieties, which may appear as a sensory difference detected by consumers.     

果色和成熟度对樱桃番茄（Solanum lycopersicum var. cerasiforme）果实挥发物分布的影响

为探究果色和成熟度对樱桃番茄果实挥发物的影响,用顶空固相微萃取-气相色谱-质谱联用法测定育种自交系材料金珠（橙）、黑樱桃1（紫）、1号（粉）、红珍珠（红）在绿熟期、转色期和红熟期的挥发物。分析发现,橙色番茄挥发物明显高于红色和粉色番茄。橙色番茄在绿熟期,紫色番茄在转色期和红熟期挥发物最高,而粉色番茄挥发物始终最低。气味强度由挥发物质量浓度和嗅觉阈值决定。3-甲基-丁醛、(E,E)-2,4-庚二烯醛、1-戊烯-3-酮、己醛、苯甲醛和(Z)-3-己烯-1-醇对番茄气味贡献较大。红色、橙色和紫色番茄分别在绿熟期、转色期和成熟期气味最浓。随着果实成熟,挥发物质量浓度持续增加,气味更加浓郁。果色和成熟度对挥发物有显著影响。     

白菜挥发性组分的气相色谱-质谱分析

利用顶空固相微萃取和气相色谱-质谱联用分析技术,对‘五月慢’、‘京冠’、‘苏州青’3个白菜品种进行风味物质成分分析,分别检测出42、41种和38种挥发性成分,主要为醛类、酮类、醇类、腈类、酯类、杂环类等化合物。其中2-己烯醛、2,4-庚二烯醛(E,E)、2,4-山梨醛(E,E)、2(5H)-5-乙基-呋喃酮、1-戊烯-3-酮、3-己烯-1-醇、2-戊烯-1-醇、苯丙腈、3-戊腈、苯乙基异硫氰酸酯是白菜的主要风味物质。     

基于主成分分析法的安溪铁观音香气质量评价模型的构建

从4个季节(每个季节两个等级)共8个安溪铁观音茶样中提取并分离出74种香气组分。通过主成分分析法鉴定出安溪铁观音中的主要特征香气成分,它们分别是：橙花叔醇、法呢烯、吲哚、苯乙醇、反-2-己烯醛、壬醛、苯乙醛、亚油酸甲酯、亚麻酸甲酯、棕榈酸甲酯、顺-己酸-3-己烯酯、苯甲酸-3-己烯-1-醇酯、辛酸-2-苯乙酯、5-正丁基-δ-戊内酯、顺式茉莉酮、法尼基丙酮、棕榈酸、香叶基芳樟醇异构体。利用主成分分析法,基于综合评价函数F＝β1F1＋β2F2＋…＋βkFk构建了安溪铁观音香气质量的评价模型,以不同特征值的方差贡献率βi(i＝1,2,…,k)为加权系数,利用所建立的模型计算各样本得分,然后进行排序评价各个茶样的香气质量。通过感官评价法进一步对模型评价结果进行了检验,结果显示两种方法具有很好的一致性,表明所建立的方法是可行的。     

基于OAV和AEDA对工夫红茶的PLSR分析

采用顶空蒸汽蒸馏提取结合气相色谱-质谱联用技术及气相色谱-嗅闻技术,对4?种中国工夫红茶进行定性、定量分析。根据香气成分的香气活力值和芳香萃取物稀释分析分别筛选出30、36?种挥发性成分作为香气成分,结合2?种方法确定22?种香气成分为工夫红茶的香气关键成分,并将其与感官属性和红茶样品进行偏最小二乘法相关性分析。确定对工夫红茶香气起重要作用的22?种关键香气物质为：1-戊醇、叶醇、1-辛烯-3-醇、反式氧化芳樟醇、芳樟醇、顺-6-壬烯醇、香叶醇、苯甲醇、苯乙醇、橙花叔醇、戊醛、己醛、反-2-己烯醛、糠醛、（反,反）-2,4-庚二烯醛、苯乙醛、（反,反）-2,4-癸二烯醛、水杨酸甲酯、丙位-壬内酯、2,3-丁二酮、2-庚酮和香豆素。     

萎凋时间对“英红九号”白茶香气的影响

采用顶空固相微萃取和气相色谱-质谱联用法,分析不同萎凋时间"英红九号"白茶香气化合物的组成及含量。结果表明,"英红九号"白茶的香气总量随萎凋时间的延长呈现先增后降趋势,萎凋24 h含量最高,达到858.40 ng/g。白茶香气主要由醇类、酯类、醛类、酮类和烃类组成,其中醇类化合物所占比例最大。不同萎凋时间白茶的香气化合物组成比较相似。顺-3-己烯-1-醇、芳樟醇、乙酸-顺-3-己烯酯、丁酸-顺-3-己烯酯、水杨酸甲酯、己酸-顺-3-己烯酯、己醛、苯甲醛、反,反-2,4-庚二烯醛、壬醛、反,反-3,5-辛二烯-2-酮、3,5-辛二烯-2-酮、β-紫罗兰酮、β-香叶烯、柠檬烯、反-β-罗勒烯和β-罗勒烯,这17种香气化合物在多数样品中含量较高,其含量总和占各样品香气总量的67.3%~76.0%,对香气总量变化影响较大;其中芳樟醇、水杨酸甲酯等多数化合物含量随着萎凋进行先增后降;而苯甲醛和β-香叶烯含量在30 h的萎凋过程中总体持续上升。     

基于AEDA和OAV值确定西瓜汁香气活性化合物的比较

本研究采用溶剂辅助风味蒸发提取西瓜汁的香气成分,利用气相色谱-质谱联用结合嗅闻仪定性定量分析其香气活性化合物,共鉴定出49种化合物,主要是小分子的酮、醛、硫醚等物质,酯类物质中只检测到一种物质,即乙酸乙酯,且浓度较低。本研究首次检测到醚类物质。OAV计算和AEDA两种方法共同鉴定出11中物质,顺,顺-3,6-壬二烯醛、顺-3-壬烯-1-醇、反,顺-3,6-壬烯-1-醇、反-2-壬烯醛、壬醛、1-壬醇、2-戊基呋喃、己醛、辛醛、顺-6-壬烯醛、反-2-辛烯醛。其中有五种香气活性物质,即顺,顺-3,6-壬二烯醛、顺-3-壬烯-1-醇、顺-6-壬烯醛、顺-2-壬烯醛、反,顺-3,6-壬烯-1-醇都能被实验员嗅闻到,且具有较高的OAV值。这表明,AEDA和OAV计算在西瓜汁香气活性化合物分析上具有一定的相似性。     

Volatile organic compounds in the aril juices and seeds from selected five pomegranate (Punica granatum L.) cultivars

A study was conducted to investigate the distribution of volatile organic compounds in the juice and seed of the most popular five pomegranate cultivars (“Ek?i,” “Devedi?i,” “Hicaz,” “Kat?rba??,” and “Keben”) in Turkey. The volatile organic compounds were analyzed using solid phase micro-extraction and gas chromatography–mass spectrometry. A total of 60 volatile organic compounds, belonging to six chemical groups including aldehydes, alcohols, esters, terpenes, ketones, acids, and phenol were identified. There were 11 volatile organic compounds (1-hexanol, [Z]-3-hexen-1-ol, 1-octanol, α-terpineol, β-myrcene, limonene, [E]-α-bergamotene, β-caryophyllene, hexanal, [E]-2-hexenal, and guaiacol) common to all five pomegranate juices and seeds. Hexalin, phenylacetaldehyde, 3-methyl butanal, and methyl-(1-methylethenyl) benzene were found in seeds only. According to discriminant analysis based on Eigenvalues, volatile organic compounds recovered in the juices could be used to discriminate and classify the pomegranate cultivars. “Devedi?i” and “Hicaz” were the most promising cultivars with respect to the largest volatile organic compounds, high total soluble solid and deep red color.     

Identification and Quantification of Impact Aroma Compounds in 4 Nonfloral Vitis vinifera Varieties Grapes

ABSTRACT:  The aroma compounds in grapes of Cabernet gernischt, Cabernet sauvignon, Cabernet franc, and Merlot have been studied by gas chromatography–olfactometry (GC–O). The GC–O study revealed the presence of 58 aroma compounds in which 53 odorants were identified. The most significant odor active volatiles in 4 grape berries were β-damascenone, hexanal, ( Z )-3-hexen-1-ol, ( E,Z )-2,6-nonadienal, β-ionone, and unknown (RI = 1612). The quantification of volatile aroma compounds in grapes was developed using headspace solid phase microextraction (HS–SPME) coupled with gas chromatography–mass spectrometry (GC–MS). The influences of SPME fiber, extracting temperature, and time on the extraction of volatile compounds in grape were investigated. The aroma compounds in 4 grapes were quantified. According to the odor activity values (OAVs), ( E,Z )-2,6-nonadienal (OAV from 334 to 777), β-damascenone (OAV 245–790), β-ionone (OAV 97–193), and acetic acid (OAV 7–165) had comparatively high OVA values.