不同处理柑橘果汁发酵果酒中游离态及键合态风味物质分析

分别以大叶尾张蜜柑澄清果汁及带渣果汁为原料,接种酿酒酵母后以固相微萃取-气相色谱-质谱法分别分析酿造90 d后果酒中的游离态及键合态风味物质,并采用气相色谱-质谱-嗅闻法描述化合物的气味性质并确定气味强度。结果表明：不同处理的果酒发酵原料对柑橘果酒的酯类风味组成有重要的影响;果酒中的游离态及键合态风味物质的种类及含量均有较大的差异。具体表现为：在不同组果酒中,风味化合物主要可以归纳为烃类、醇类、醛类、酮类、酯类、酸类,并且游离态风味物质种类明显多于键合态风味物质。酯类及醇类是柑橘果酒中主要的风味物质;在发酵果酒中不存在以键合态存在的酸类风味前体物质。采用气相色谱-质谱-嗅闻检测技术得出,2 种不同原料对果酒的键合态及游离态特征风味物质有重要的影响;对以柑橘澄清果汁为原料（组1）的果酒的香气做出主要贡献的特征香味的物质主要有8 种,占总量的67.81%;检测到的键合态特征风味物质5 种,占总量的56.47%;而对于以带榨果汁为原料的果酒中（组2）,游离态及键合态特征风味物质分别有7 种和5 种,各占总量的48.35%、24.21%。因此可以看出,在果酒中键合态及游离态特征风味物质差异较大,并且以带渣果汁及澄清果汁为原料酿造的柑橘果酒在特征风味物质中存在较大差异。     

老鹰茶游离和键合态挥发性成分的分析

以武陵地区老鹰茶作为研究对象,结合顶空固相微萃取(headspace solid-phase microextraction,HSSPME)与针捕集(needle trap,NT)对老鹰茶挥发性成分进行萃取,鉴定出老鹰茶中游离态和键合态47种挥发性化合物。其中包括32种游离态挥发性化合物和26种键合态挥发性化合物。结果表明,老鹰茶主要游离态挥发性化合物是乙酸龙脑酯、杜松醇、α-桉叶醇,键合态挥发性化合物是γ-桉叶醇、α-芹子烯、愈创木烯。测定的游离态和键合态芳香化合物中有17种香气活度值(odor activity value,OAV)大于1。从鉴定出的挥发性成分香气特征可知,老鹰茶游离态香气成分主要是正癸醛、十二醛、乙酸异龙脑酯、桉叶油醇、2-十一酮、正己醛,键合态香气成分是大马士酮、桉叶油醇、芳樟醇、2-己酮、D-柠檬烯、2-十一酮、正癸醛。     

新型松茸黄酒发酵过程中键合态与游离态香气成分分析

通过比较新型松茸黄酒不同发酵阶段(松茸提取液、前发酵前期、前发酵后期、后发酵后期)键合态、游离态香气物质的组成及含量的具体差异,为松茸类黄酒的风味特性研究提供科学依据。以自制新型松茸黄酒为研究对象,采用官能化聚苯乙烯/二乙烯苯萃取柱(Cleanert polar enhanced polymer-solid phase extraction, Cleanert PEP-SPE)对新型松茸黄酒游离态和键合态化合物进行分离,结合顶空固相微萃取技术结合气相色谱-质谱联用仪(headspace solid-phase microextraction combined with gas chromatography-mass spectrometry, HS-SPME-GC-MS),对不同发酵阶段的新型松茸黄酒中游离态、键合态挥发性物质的种类和含量进行检测分析。结果显示,发酵过程中键合态、游离态香气成分共127种,其中键合态香气成分77种,主要以醇类、醛类和酚类为主(未检测到吡嗪类和呋喃类);游离态香气成分107种,以醇类和酯类为主(未检测到2-甲基丁醛等部分醛类),分析表明两种形态挥发性组分存...     

树莓汁中游离态和键合态香气物质的成分分析

采用Amberlite XAD-2树脂吸附洗脱分离的方法,对树莓汁中的游离态和键合态香气物质进行了分离,对提取得到的键合态香气物质进行酸法或酶法(β-D-葡萄糖苷酶)水解释放,并采用气相色谱进行检测分析,以明确树莓汁中游离态和键合态香气物质的种类和含量。结果表明,在树莓汁中共检出23种游离态香气物质,主要为脂肪醇类、酮类和酯类物质,苯甲醛是游离态组分中含量最高的物质;酶法水解后共检出20种键合态香气物质,主要为苯系物和脂肪醇类物质;酸法水解后共检出11种键合态香气成分,主要为萜烯类和脂肪醇类物质。     

不同陈皮中游离态与键合态挥发性化合物成分分析

为比较不同产地品种陈皮中游离态与键合态挥发性化合物的差异,采用沸水浸泡和树脂洗脱/β-葡萄糖苷酶水解方式制备广东茶枝柑、福建芦柑和浙江蜜桔三种陈皮中游离态与键合态挥发性化合物,利用顶空固相微萃取-气相色谱-质谱(headspace-solid phase microextraction-gas chromatography-mass spectrometry, HS-SPME-GC-MS)分析陈皮游离态与键合态挥发性化合物的组成。GC-MS分析显示三种陈皮共检出24种游离态挥发性成分,均以单萜烯类化合物为主,其中广东茶枝柑陈皮的单萜烯类化合物含量最高且种类最丰富,且广东茶枝柑陈皮相比福建芦柑与浙江蜜桔陈皮具有较高含量的邻甲氨基苯甲酸甲酯、p-伞花烃和酚类化合物,以及较低的D-柠檬烯/g-萜品烯比值,同时三种陈皮均有其特有的倍半萜烯类物质；三种陈皮共检出32种键合态挥发性化合物,其中福建芦柑陈皮与浙江蜜桔陈皮均以醇类和酯类化合物为主,广东茶枝柑陈皮以单萜烯类化合物为主。此外,不同陈皮均有游离态挥发性化合物的总含量高于键合态挥发性化合物,且许多键合态成分呈萜烯类结构(如醇类、醛类、单萜烯类)。本研究结果可为不同产地品种陈皮的区分,以及后续陈皮陈化过程中挥发性化合物的变化机理提供参考。     

不同蒸馏法对葫芦巴精油得率和化学成分的影响

以葫芦巴为研究对象,采用水蒸气蒸馏法、同时蒸馏萃取法提取其精油,采用气相色谱-质谱分析法(GC-MS)对精油进行成分分析并比较。结果显示,水蒸气蒸馏法所得精油颜色为浅黄色,得率为0.24%, GC-MS分析其成分为27种,匹配度较高的有19种化合物,精油中含量较高化合物占精油总物质的64.999%;同时蒸馏萃取法所得精油颜色为淡黄色,得率为0.37%,精油中化学成分为25种,匹配度较高的有23种化合物,精油中含量较高化合物占精油总物质的89.447%。对2种方法得到的精油综合比较,同时蒸馏萃取法在得率上、相同物质含量上都超过水蒸气蒸馏法,并且同时蒸馏萃取法操作更简单,更节省试剂。故优于水蒸气蒸馏法。     

刺梨皮渣和籽仁中游离态和键合态香气物质的比较

采用顶空-固相微萃取法提取刺梨皮渣、籽仁中游离态香气物质和酶法释放刺梨皮渣、籽仁中键合态香气物质,结合气相色谱-质谱法分析技术对刺梨皮渣和籽仁中的游离态和键合态香气物质进行定性和定量研究。结果表明,检出的刺梨皮渣中游离态香气物质有21 种,萜烯类物质最丰富,其次是酯类物质和酮类物质;检出的键合态香气物质有23 种,其中酸类物质最为丰富,其次是酚类物质和醇类物质。皮渣中游离态和键合态香气物质有很大差异,只有辛酸1 种物质都以游离态和键合态的形式存在。刺梨籽仁中检出游离态香气物质有9 种,萜烯类物质最为丰富,其次是醇类物质和酚类物质;检出的键合态香气物质有18 种,包括酸类8 种、酚类3 种、醇类3 种、羟基醛类2 种,羟基酯类和羟基酮类各1 种。籽仁中被释放出来的香兰素（3-甲氧基-4-羟基苯甲醛）和异香草醛（3-羟基-4-甲氧基苯甲醛）2 种羟基醛是重要的键合态香气物质。     

锦橙果肉和果皮中游离态和键合态香气物质研究

以锦橙为研究对象,应用AmberliteXAD-2吸附和溶剂洗脱分离锦橙果肉和果汁中游离态和糖苷键合态的芳香化合物,并采用GC-MS检测了锦橙果肉和果皮中的芳香物质。结果表明,锦橙果肉中检出游离态香气31种,键合态香气21种,锦橙果皮中检出游离态香气33种,键合态香气29种。果肉和果皮中游离态和键合态香气组分的构成差别较大,果肉中主要为正己醇、3-羟基己酸乙酯、丁酸乙酯、癸醛和异环柠檬醛等;果皮中则主要为芳樟醇、反金合欢醇、δ-杜松烯、柠檬醛和榄香醇等。     

山楂中游离态和键合态风味化合物

应用ＡｍｂｅｒｌｉｔｅＸＡＤ－２柱吸附，选用不同溶剂洗脱从山楂中提取分离出游离和键合态风味组分。键合态组分经β－葡萄糖苷酶或酸水解释放出挥发性糖苷配基。用ＧＣ－ＭＳ在游离态和键合态组分中分别检测出９种和１３种化合物，认为顺－３己烯醇、甲酸己酯、顺－３－己烯醇乙酸酯等是山楂游离态风味的主要成分。发现山楂中含有较多的键合态风味组分，数量上和含量上都远比游离态组分多，特别是丁香酚、甲酸已酯、苯甲醇、苯乙醇、水杨酸甲酯、苯甲醛等组分。酶法水解对山楂有明显的增香作用。并对山楂风味化合物的生物合成途径进行了讨论。     

柠檬汁中游离态和键合态萜类化合物的研究

应用Amber lite XAD-2柱吸附,选用不同的溶剂洗脱从柠檬汁中提取和分离出游离态和糖苷键合态的香气组分。键合态组分经β-D-葡萄糖苷酶水解释放出挥发性糖苷配基。用气相色谱和质谱联用仪在游离态和键合态中分别检出了16种和9种萜类化合物,其中有5种为首次在柠檬香气中发现。酶法水解对柠檬香气有明显的增香作用。HPLC分析苷元可能是葡萄糖和鼠李糖。     

基于电子鼻和GC-IMS分析复热对香菇汤挥发性风味物质的影响

以即食型香菇汤产品为对象,利用电子鼻和气相离子迁移色谱(GC-IMS)分析了蒸汽复热和微波复热对香菇汤风味特征的影响。电子鼻结果表明,复热后香菇汤气味特征变化显著(P0.05)。经GC-IMS分析,复热前后香菇汤中均定性出56种单体及部分物质的二聚体,挥发性风味物质的种类虽相同,但含量差异较大。柠檬烯、辛醛及其二聚体、庚醛及其二聚体、2-环己烯-1-酮、2-糠醛及其二聚体、戊醛及其二聚体、2-甲基丙醛在微波复热香菇汤中的含量要高于蒸汽复热和未复热香菇汤。二甲基三硫、对甲酚、二甲基二硫、5-甲基-2-糠醛、1-己醇及其二聚体,在蒸汽复热香菇汤中含量要高于未复热和微波复热香菇汤。复热处理对香菇汤的挥发性风味物质影响较大,且复热后香菇汤中挥发性风味物质含量更高。     

Volatiles of apples (var. 'Schone van Boskoop'): isolation and identification

A simple method for the analysis of apple volatiles has been developed. By means of a modified vacuum-cold trap distillation an aqueous solution of volatiles, ready for direct GLC-analysis, is obtained.
Formation of artefacts (e.g. volatile aldehydes) during homogenization of the apple tissue was prevented by addition of trichloroacetic acid. About fifteen volatiles of the apple variety 'Schone van Boskoop' have been identified and quantified. More than 85% of the total volatile fraction are alcohols. The recovery for the different volatiles ranged from 60 to 95% depending on the nature of the compounds.
In a dichloromethane extract of the distillate a few minor compounds, mostly esters, were identified by mass spectrometric analysis.     

Volatile constituents from Romanesco cauliflower

The volatile and semi-volatile constituents of Brassica oleracea L. var. Botrytis L., Romanesco group, Navona variety, were extracted by steam distillation from leaves and inflorescence, using a Likens–Nickerson-type apparatus. The extracts from fresh, ripening and frozen vegetables were investigated by gas chromatography and mass spectrometry. From the fresh leaves extract, a total of 61 compounds were identified, representing 96.8% of the oil. The major constituent was found to be hex-3(Z)-enol (61.1%). From fresh disrupted inflorescence tissues of Romanesco, 35 compounds were detected, representing 97.7% of the extract. Dimethyl disulfide, dimethyl trisulfide and hex-3(Z)-enol were identified as major constituents of the hydrodistillation products, representing, respectively, 30.2, 24.2 and 21.7% of the volatiles. From ripening and frozen inflorescence tissues, dimethyl disulfide and trisulfide were again detected as predominant components. In the latter, hex-3(Z)-enol had almost disappeared (0.8%) whereas dimethyl trisulfide represented 49.7% of the oil. This is the first report concerning the steam distillation compounds present in the leaves and inflorescence tissues of this species.     

烫漂方式对香菇挥发性成分的影响

比较微波、蒸汽和沸水烫漂对香菇挥发性成分的影响。采用顶空固相微萃取-气相色谱质谱联用技术进行挥发性成分定性分析,并对苯甲醛与1-辛烯-3-醇进行外标法定量分析。结果表明:新鲜香菇的主要挥发性化合物分为五类25种,包括醇类6种、醛类4种、酮类2种、烃类5种和含硫化合物8种,苯甲醛与1-辛烯-3-醇分别为0.28 ng/g和308.44 ng/g。微波烫漂的香菇中1-辛烯-3-醇含量为515.65 ng/g;蒸汽烫漂与沸水烫漂对醇类与含硫化合物的相对含量影响较大,其中蒸汽烫漂使香菇中醇类相对含量由22.49%降至3.93%,含硫化合物相对含量由64.57%增至87.64%,苯甲醛与1-辛烯-3-醇含量分别为0.45 ng/g和245.64 ng/g;香菇经沸水烫漂,醇类相对含量达87.89%,含硫化合物(2.85%)显著降低,1-辛烯-3-醇含量为1482.46 ng/g。以上表明,从挥发性成分组成来看,蒸汽烫漂与沸水烫漂处理对其差异影响较大,特别是醇类与含硫化合物的相对含量有明显区别。     

Study on the volatile profile characteristics of oyster Crassostrea gigas during storage by a combination sampling method coupled with GC/MS

In this work, a combination sampling method, including headspace solid-phase microextraction (HSSPME) and steam distillation (SD), was used to study the oyster volatiles during storage followed by GC–MS detection. Twenty and twenty seven volatile compounds of fresh and deteriorated oysters were identified respectively by HSSPME, and 16 oyster volatiles were isolated by SD. HSSPME and SD were suitable for low-boiling-point and high-boiling-point volatiles, respectively. Therefore, the combination of HSSPME and SD could obtain more species of oyster volatiles during storage than any single method. Different volatile profile characteristics during oyster storage obtained by HSSPME were specified by principal component analysis. The top ten volatiles contributing most to the difference of oyster volatile profile characteristics during storage were distilled by common model analysis. The results tentatively suggested that the difference of entire volatile profile characteristics during oyster storage would provide more precise alarming information for oyster deterioration during storage than individual volatiles.     

A study of volatile flavour substances in Dalmatian traditional smoked ham: Impact of dry-curing and frying

Volatiles from Dalmatian prosciutto were isolated by solvent extraction (SE), simultaneous distillation extraction (SDE) and nitrogen purge and steam distillation (NPSD) and analyzed by GC and GC–MS. In all, 46 compounds were identified by SDE and SE (including fatty acids, aldehydes, phenols, esters, ketones and others), while 81 compounds were identified by NPSD (headspace volatiles including phenols, aldehydes, hydrocarbons, ketones, alcohols, esters and heterocyclic compounds). Regarding the impact of dry curing period on the volatiles, an increase in the percentages of aldehydes and esters during the ripening of the prosciutto was observed. Quantitative percentage differences among fried and raw samples were particularly evident in respect of aldehydes (SDE and SE). The NPSD method provided additional information of the volatiles from fried ham, since the pyrazines and most of the lower aldehydes that are important thermally derived flavour compounds were only isolated by NPSD (not by SE and SDE).     

同时蒸馏萃取-气质联用分析乌梅中的挥发性成分

采用同时蒸馏萃取法提取两种不同工艺制成的乌梅中的风味成分。所得到的挥发性成分用气相色谱/质谱(GC/MS)法分离并分析鉴定,共鉴定出了69种挥发性成分。其中酚类15种,酸类8种,醇类2种,醛类5种,酯类6种,烃类26种,其它杂环类7种。两种乌梅的挥发性风味成分的种类和含量虽有差异,但是风味的主体成分基本相同。酚类及其衍生物应是提供乌梅烟熏香的最重要的成分。     

Isolation of volatile oil from thyme (Thymbra spicata) by steam distillation

The effects of steam flow rate (1.03 and 0.64 L/h), distillation time, and particle size (0.50, 1.00, 2.05 mm) of Thymbra spicata on essential oil yield and sequence of extraction of compounds were studied. A logarithmic model fitted well to experimental data. The composition of the essential oil obtained by steam distillation was investigated for whole leaves only since the grinding had an adverse effect on yield. The oil obtained was very rich with respect to its carvacrol content. For both steam flow rates, oxygenated monoterpenes were recovered the most rapidly. Using whole leaves (2.05 mm) and a higher steam flow rate (1.03 L/h) for 75 min of distillation was chosen as the optimum which gives the lowest amount of monoterpene hydrocarbons, the complete recovery of oxygenated compounds, and the highest yield in a shorter time. Yield was 1.57% at this optimum condition. The oil was composed of 53.1% oxygenated compounds, 25.7% monoterpene hydrocarbons, 4.4% sesquiterpenes, and 14.1% p-cymene.     

旋转椎体柱法及水蒸汽蒸馏法提取咖啡中的挥发性香气成分研究

旋转椎体柱技术可在真空状态下通过蒸汽来提取液体或浆料中的挥发性成分,充分维持原材料的自然特性,已在多个领域得到了广泛运用。本文利用水蒸汽蒸馏法和旋转锥体柱技术提取咖啡中的挥发性香气成分,借助GC-MS对两种提取方法获得的香气成分进行对比分析。结果表明旋转锥蒸馏柱提取获得的挥发性香气成分得率高,约是水蒸汽蒸馏法的9.6倍,感官体验上更加真实。在种类和含量上,旋转锥体柱提取和水蒸汽蒸馏所得挥发性成分分别鉴定出52种和24种,旋转锥体柱得到的挥发性成分含有更多的吡嗪、吡咯、吡啶和酯类影响咖啡风味的关键物质。     

武陵青花椒壳挥发油成分及脂肪酸分析

分别采用水蒸气蒸馏法和同时蒸馏萃取法提取武陵青花椒壳中的挥发油成分,提取率分别为6.4%和8.5%。再用气相色谱-质谱法(GC-MS)对挥发油成分进行分析,用峰面积归一化法确定各组分的相对含量。两种方法均鉴定出43种化合物,其中水蒸气蒸馏法以β-芳樟醇(66.91%)、反式-橙花叔醇(6.28%)、D-柠檬烯(5.24%)、4-萜烯醇(2.6%)为主,同时蒸馏萃取法以β-芳樟醇(64.32%)、D-柠檬烯(5.97%)、反式-橙花叔醇(4.17%)、反式-9-十八烯酸(3.09%)为主。同时对挥发油进行甲酯化,然后用GC-MS对挥发油中含有的脂肪酸进行了分析,共分离鉴定出6种脂肪酸。结果表明:两种方法提取的挥发油的组成及含量存在差异,挥发油中主要为不饱和脂肪酸。水蒸气蒸馏法对无极性和弱极性的萜烯和萜醇类化合物提取效果较好,而同时蒸馏萃取法适于各种极性化合物,对极性稍强的脂肪酸和酯类有较好的提取效果。