Investigation of Volatile Components in Wines from Koshu and Zenkoji Grapes

A 3-hydroxyethyl-4-cyanoazetidin-2-one derivative (2) was synthesized from (2R,3R)-potassium 2,3-epoxybutyrate through two steps, and it was then further converted to a diazo derivative (7).     

Volatile Flavor Components of Dried Bonito (Katsuobushi). I. On Basic,Acidic and Weak Acidic Fractions

The aqueous extract of dried bonito (Katsuobushi) was distilled by using a thin film evaporator. The resulting distillate was extracted with diethyl ether, and the extract was separated into basic, acidic, weak acidic, and neutral fractions.

The basic, acidic, and weak acidic fractions were analyzed by gas chromatography and gas chromatography-mass spectrometry.

Seventy-four compounds, including 24 acids, 24 phenols, 8 pyridines, 12 pyrazines, 3 thiazoles, and 3 other compounds were identified. Thirty-six of these compounds were newly identified as volatile flavor compounds of Katsuobushi.     

Gas Chromatographic Analysis of Volatile Esters in Wines

We isolated a new aerobic gram negative collagenolytic bacterium, strain CRZV₁. This strain is yellow pigmented, non motile; it poorly degrades the sugars and its proteolytic activity corresponds to one enzyme, a collagenase which is produced in media with collagen, or collagen like substrates. The strain CRZV_l, presents many similarities with Flavobacteria. However, the GC content of the DNA, which is 65%, excludes our collagenolytic strain from the genus Flavobacterium, where all the species have GC content between 30 and 42%. All the strains, already described as Flavobacteria, the GC contents of which are situated between 55 and 70%, are actually unclassified. They could be included in the genus Empedobacter. This genus is not in the approved list of bacterial names, so we only consider this new collagenolytic bacteria as a gram negative, aerobic, yellow pigmented bacteria.     

Enzymatic Quantification of L-Tartrate in Wines and Grapes by Using the Secondary Activity of D-Malate Dehydrogenase

L-Tartrate in wines and grapes was enzymatically quantified by using the secondary activity of D-malate dehydrogenase (D-MDH). NADH formed by the D-MDH reaction was monitored spectrophotometrically. Under the optimal conditions, L-tartrate (a 1.0 mM sample solution) was fully oxidized by D-MDH in 30 min. A linear relationship was obtained between the absorbance difference and the L-tartrate concentration in the range of a 0.02-1.0 mM sample solution with a correlation coefficient of 0.9991. The relative standard deviation from ten measurements was 1.71% at the 1.0 mM sample solution level. The proposed method was compared with HPLC, and the values determined by both methods were in good agreement.     

Contents of Resveratrol,Piceid, and Their Isomers in Commercially Available Wines Made from Grapes Cultivated in Japan

The presence of resveratrol (3,5,4′-trihydroxystilbene) and its β-glucoside, piceid (resveratrol-3-β-D-glucopyranoside), together with their isomers in wine appears to be one of the beneficial factors conferring a protective effect against cardiovascular disease through red wine ingestion. A total of 42 red and white wines was collected in arears from Hokkaido to Kyushu in Japan. The wines were fractionated with a C₁₈ Sep-pak cartridge, and the active principles were eluted with ethyl acetate. Crude trans- and cis-piceid were extracted from a Chinese medicine, ‘Kojohkon’ (Polygonum cuspidatum), and their retention times and UV absorption were confirmed by HPLC. trans- and cis-Resveratrol, and trans- and cis-piceid were analyzed in a short C₁₈ HPLC column, and cis-resveratrol was quantified from the amount of cis-isomer converted from authentic trans-resveratrol that had been treated by UV irradiation. The content of piceid is shown as the resveratrol equivalent. The average content of total stilbene compounds was 4.37mg/liter in red wines, while only 0.68 mg/liter in white wines. Red wines made from Pinot noir, Merlot, and Zweigeltrebe grapes all had a high resveratrol content.     

Volatile Basic Compounds Identified from a Heated d-Glucose/l-Alanine Mixture

Volatile basic compounds from a heated d-glucose/l-alanine mixture were analyzed by gas chromatography and coupled gas chromatography-mass spectrometry. By comparison of mass spectra with corresponding reference spectra, the following compounds were identified: pyrrolidine, β-picoline, pyrazine, 2-methylpyrazine, 2,5-dimethylpyrazine, 2,3-dimethylpyrazine, 2-ethyl-5-methylpyrazine. 2,3,5-trimethylpyrazine and 2,5-dimethyl-3-ethylpyrazine. 2-Methyl-3,5-diethylpyrazine, 2-methyl-5,6-diethylpyrazine and two alkylpyrazines with M. W. 164 and 178 were also tentatively identified.

No evidence for the presence of N-nitrosamine with low molecular weight was found.     

Comparison of soluble proteins in juice and wine from Koshu grapes

Proteins were separated from Koshu grape juice and wine by precipitation with ammonium sulfate. The protein fractions were further fractionated by gel electrophoresis and gel isoelectric focusing, followed by amino acid analyses. The juice contained more than eleven protein fractions with molecular weights between 13,000 and 65,000, and their isoelectric points were between 3.6 and 10.5. The wine also contained more than eleven protein fractions with molecular weights between 21,000 and 65,000, while their isoelectric points were between 3.6 and 11.0. All the juice proteins and some major wine proteins were glycoproteins. The same three protein fractions were present in both juice and wine. The other juice proteins were lost during wine-making and thus, were not detected in the wine. About half of the proteins detected in the wine were not observed in the juice. Some juice proteins were bound to the flavonoid phenolics extracted from the wine and were removed as insoluble precipitates. There was specific interaction between wine flavonoids and juice proteins.     

Major Volatile Components Formed from Casein during Roasting

The volatiles, produced from casein during roasting at 250°C for 1 hr, were fractionated and analyzed by various methods including the combination of gas chromatography and mass spectrometry. The following kinds of compounds were tentatively or conclusively identified: six aliphatic aldehydes, benzaldehyde, acetophenone, hydrogen sulfide, methanethiol, dimethyl disulfide, five primary alkylamines, piperidine, N-ethylcyclohexylamine, two alkylpyrazines, ethylmethylpyridine, three aliphatic carboxylic acids, pyruvic acid, benzoic acid, six aliphatic alcohols, and three aromatic hydrocarbons. α-Dicarbonyls were not formed in any detectable amount.

The results obtained above are discussed in comparison with those of pyrolysis of some kinds of α-amino acid and also with those of some roasted foods.     

光叶三角梅'Formosa'叶片挥发性组分的GC-MS分析

三角梅不仅观赏性强,而且具有多方面的保健作用。为了阐明三角梅的次生代谢机制,本研究采用水蒸气蒸馏法提取光叶三角梅（Bougainvillea glabra‘Formosa’）叶的挥发性成分,并通过GC-MS法进行定性和定量分析。本试验共分离出61种成分,经NIST数据库检索、与标准谱图比较,鉴定出47个化学组分,占总挥发性组分含量的90％以上。结果表明,该三角梅叶中舍有叶醛、植醇、棕榈酸,对乙烯基愈创木酚、柠檬烯等对人体有益的化合物。     

药用野生稻和栽培稻挥发油的化学成分比较研究

本文采用水蒸气蒸馏法提取抗褐飞虱品种药用野生稻(Oryza officinalis)和感褐飞虱品种栽培稻(O.sativa)的挥发油,并运用气相色谱-质谱法(GC/MS)对二者的化学成分进行种类和含量的比较分析。结果表明,两种植物材料的挥发油在种类和含量上存在明显差异,如,糠醛(药用野生稻7.60%栽培稻0%;2,3-苯并二氢呋喃(药用野生稻10.80%,栽培稻3.32%);4-乙烯基-2-甲氧苯酚(药用野生稻22.99%,栽培稻7.32%)。推测含量较高的糠醛、2,3-苯并二氢呋喃和4-乙烯基-2-甲氧苯酚可能是药用野生稻对褐飞虱的活性成份。     

离体蒜苗挥发物的化感作用及其成分分析

采用半密闭容器法研究了离体蒜苗挥发物对黄瓜、番茄、萝卜的化感作用,并对其成分进行了GC-MS分析。结果表明:蒜苗挥发物对黄瓜的种子萌发及幼苗生长表现为低促高抑的双重浓度效应,对番茄和萝卜则表现出抑制作用,并且随供体蒜苗质量的增大,抑制作用增强;供体蒜苗质量低于400g时,受体植株SOD、POD、CAT、PPO、PAL等活性增强,供体质量为400g时,受体作物上述酶活性均降低;离体蒜苗挥发物的主要化学成分为二烯丙基二硫化物(23.33%)、1,3-二噻烷(18.34%)和邻苯二甲酸二丁酯(6.30%)。     

华北落叶松枝叶挥发性成分

利用水蒸气蒸馏法提取华北落叶松枝叶的挥发油,进一步采用气相色谱-质谱联用方法对其化学成分进行分析,共分离鉴定出79种化学成分,主要有大根香叶烯（11．35％）、1-异丙基4,7．二甲基-1,2,4a,5,8,8a-六氢萘酚（6．53％）、石竹烯（5．84％）、长叶松节烷（5．23％）、7-甲基4-亚甲基-1-（1-甲基乙基）-1,2,3,4,4a,5,6,8a-八氢萘（5．21％）、（E）-3,7,11-三甲基-1,6,10-十二烷三烯-3-醇（5．17％）、．tau．-muurolol（4．55％）、α-杜松醇（4．31％）、α-石竹烯（4．22％）等,其中萜烯类及其含氧衍生物占较大比例。     

Glial Fibrillary Acidic Protein in the Cytoskeletal and Soluble Protein Fractions of the Developing Rat Brain

The distribution of glial fibrillary acidic protein (GFAP) into cytoskeletal and soluble protein fractions during development of the rat brain has been studied by quantitative immunoblotting and enzyme-linked immunosorbent assay (ELISA). These assays indicate that cytoskeletal GFAP accounts for nearly all the total GFAP in the adult rat brain, and that the developmental increase in the GFAP content of the rat brain is due to accumulation of GFAP into the cytoskeleton. A small and constant amount of the total GFAP was detected in the soluble protein fraction. This GFAP had an apparent molecular mass (Mr) similar to that of the highest Mr form of GFAP detected in the cytoskeletal fraction. In contrast to the assays for cytoskeletal GFAP, no significant increase in the GFAP concentration of the soluble protein fraction could be measured during development. Sensitive, calibrated immunoblotting of cytoskeletal and soluble protein with [125I]protein A confirmed these findings, and showed that both cytoskeletal and soluble GFAP are first detected during the same period of foetal rat brain development. A finite and reproducible amount of lower Mr forms of GFAP were observed in the cytoskeletal fraction even when prepared in the presence of stringent proteolytic inhibitors. These presumed proteolytic degradation products of GFAP increased in abundance during development, parallel to the increase in cytoskeletal GFAP content of the rat brain. However, the abundant proteolytic degradation products of GFAP found in the cytoskeletal fraction were not detected in the soluble protein fraction at any age studied.(ABSTRACT TRUNCATED AT 250 WORDS)     

不同产地丁香挥发性成分分析

采用顶空固相微萃取-气相色谱-质谱联用技术对产自国内外4个地区的丁香(Eugenia caryophyllata Thunb.)挥发性成分进行了检测,并以峰面积归一化法计算了各组分的相对含量。结果显示,从4个产地13批次丁香中共鉴定出挥发性成分72种(匹配度均高于75),其中,主要成分含量排名前两位的均为丁香酚、(-)-α-芹子烯,排名第三位的挥发性成分分别为:顺式-α-没药烯(马达加斯加塔马塔夫,平均为3.75%)、罗勒烯(中国广东,平均为4.21%)、亚麻三烯(中国广西,平均为3.74%)、丁香烯(印度尼西亚爪哇岛,平均为3.60%)。表明同一产地的丁香挥发性成分具有一定的相似性,不同产地丁香挥发性成分也有一定的差异,这对丁香产地的鉴别具有重要意义。主成分分析和聚类分析的结果既可以将4个产地的丁香很好地区分开来,又能反映出它们之间的亲缘关系。本研究采用HS-SPME-GC-MS方法检测不同产地丁香挥发性成分并结合主成分分析(PCA)及聚类分析法,能有效区分4个产地的丁香,该方法可作为丁香产地的鉴别方法,也为进一步比较不同产地丁香挥发性成分的差异及质量控制提供了新思路。     

Analysis of Volatile Components in Rice Bran

Volatiles stripped from rice bran are analyzed by gas chromatography and thin-layer chromatography either directly or after converted into 2, 4-DNPH’s or 3, 5-DNB’s. Most of prominent peaks revealed by a direct gas chromatography of the volatiles condensates behave as alcohols against classification reagents and are identified as methanol, ethanol, n-propanol, sec-butanol, isobutanol, n-butanol, isopentanol, n-pentanol and n-hexanol, respectively. Ethanol and methanol, being major components in the condensates are also detected by thin-layer chromatography of their 3, 5-DNB’s. Carbonyls identified by a flash exchange gas chromatography of 2, 4-DNPH’s of the volatiles are ethanal, propanal, isobutanal, acetone, n-butanal, isopentanal, n-pentanal and n-hexanal. Thin-layer chromatography of 2, 4-DNPH’s reveals presence of ethanal, acetone, isopentanal or/and isobutanal and n-hexanal in the volatiles. The experimental data have been integrated to furnish a basis for extensive comparison with other rice products and by-products.     

基于香气成分含量对酿酒红葡萄品种的分类研究

利用顶空固相微萃取与气相色谱质谱联用(HS-SPME-GC-MS)技术测定了26种酿酒红葡萄的香气成分以及部分重要组分的含量,并采用聚类分析与主成分分析法,探讨利用香气成分含量对酿酒红葡萄品种的分类。结果显示:(1)在26种酿酒红葡萄品种中共检测到49种香气成分并分为6大类,分别为C6-醇和醛类化合物、醇类化合物(除C6-醇类)、酯类化合物、醛类(除C6-醛类)和酮类化合物、萜烯类化合物、有机酸类化合物。(2)聚类分析结果显示,26种酿酒红葡萄分成了三大类,其中:第Ⅰ类有赤霞珠等11个品种,香气成分以C6-醇和醛类化合物为主,其总含量高达66.4%;第Ⅱ类有宝石解百纳等6个品种,香气成分以C6-醇和醛类化合物以及醇类化合物(除C6-醇类)为主,分别为40.73%和30.21%;第Ⅲ类有梅鹿辄等9个品种,香气成分以酯类化合物为主,占总香气成分的71.06%;而且三类酿酒红葡萄中有机酸含量均最低,分别为0.18%、0.08%和0.005%。(3)主成分分析结果表明,第Ⅰ类酿酒红葡萄中可以用前6个主成分代表原有的变量信息,第Ⅱ类和第Ⅲ类均可以用前4个主成分代表原有的变量信息。(4)利用判别分析创建了酿酒红葡萄香气成分判别模型,并对其进行验证,其准确率达85.7%。研究表明,利用香气成分建立的判别模型可以对酿酒红葡萄进行分类,可为酿酒红葡萄品种改良及葡萄酒质量控制提供理论依据。     

抱茎蓼挥发油成分及其抗菌活性的研究

水蒸气蒸馏法从抱茎蓼全草中提取挥发油,用气相色谱-质谱联用技术对其挥发油组分进行分离和鉴定,运用气相色谱面积归一化法确定各组分的相对含量,并利用正构烷烃系列物质对各组分进行定性确定,从抱茎蓼全草的挥发油中检出41个组分,占全油的99.21%,鉴定出38个组分,其主要组分是石竹烯(16.98%)、3-己烯-1-醇(14.69%)、3-辛烯-3醇(8.89%)、a-里哪醇(7.13%)、β-环柠檬醛(6.36%)等。对抱茎蓼全草的挥发油做了抗菌试验,其挥发油对大肠埃希菌(ATCC25922株)、肠炎沙门菌(50040株)、金黄色葡萄球菌(ATCC25925株)有显著地抑制和灭活作用。     

三角梅属四个品种花挥发性组分的GC-MS分析

三角梅不仅观赏性强,而且具有多方面的保健作用。为了揭示三角梅的次生代谢机制,本研究采用水蒸气蒸馏法提取三角梅属四个品种(Bougainvillea glabra ‘Magnifica’、Bougainvillea glabra ‘Pink Pixie’、Bougainvillea glabra ‘Formosa’和Bougainvillea×buttiana ‘Mahara’)花的挥发性成分;通过GC-MS法对所提取的成分进行定性和定量分析。共分离出85种成分,经NIST数据库检索,并与标准谱图比较共鉴定出72个化学组分,占总挥发性组分含量的90%以上。结果表明,4个三角梅品种的花中含有植醇、丁子香酚、亚油酸、亚麻酸以及维生素E等对人类有益的化合物。