HXD前后烟丝中烟碱及部分香味成分的变化

为研究卷烟加工过程中烟草化学成分的变化,采用同时蒸馏萃取结合气相色谱及气质联用技术,对两种牌号烟丝在HXD前后的酸性、碱性和中性香味成分进行了分析。采用内标法定量测定了烟丝中吡啶、吲哚等17种碱性香味成分;二氢大马酮、芳樟醇等18种中性香味成分;2-甲基戊酸、苯甲酸等12种酸性香味成分;采用溶剂萃取法对HXD前后烟丝样品中游离烟碱的变化进行了研究。结果表明,HXD工序对烟草总生物碱和游离生物碱的影响显著,总生物碱降低近16%,游离生物碱降低近30%;碱性香味成分总量和中性香味的酮类化合物呈下降趋势,而中性香味成分中的醇类化合物及酸性成分的总含量呈明显升高趋势。其中,酸性香味成分的变化最为显著,含量均大幅提高,增幅分别达18%和31%。     

微波烘丝前后烟丝中主要中性香味成分分析

为研究微波烘丝前后烟丝中主要中性香味成分的变化规律,在不同时间、不同微波输出功率条件下,对微波烘丝前后的烟样进行取样,采用同时蒸馏萃取法和毛细管气相色谱法,对烟样中的异佛尔酮、氧化异佛尔酮、茄酮等19种主要中性香味成分进行了分离、定性和定量。实验结果表明,随微波烘丝时间的延长,各类物质的总含量与对照相比呈降低趋势;当烘丝时间超过4min后,19种主要中性香味成分的含量都同时出现了回升现象,但仍低于对照;随微波输出功率的增加,6-甲基-5-庚烯-2-酮、异佛尔酮、氧化异佛尔酮、香叶基丙酮、β-紫罗兰酮等5种物质的含量变化不大,而茄酮、β-大马酮、β-二氢大马酮、巨豆三烯酮等4种物质的含量波动较大,总比各类物质的总含量均有所下降。     

中上部不同成熟度烤烟烟叶与主要化学成分和香味物质组成关系的研究

对中部和上部不同成熟度河南烤烟烟叶中的多种重要中性香味成分和常规成分进行了分析研究。采用同时蒸馏萃取装置结合毛细管GC及GC/MS对香味成分进行分离、定性和定量,分析测定了异佛尔酮、氧化异佛尔酮、β-大马酮、β-二氢大马酮等22种重要香味成分。根据行业标准测定了不同成熟度烟叶中总糖、总氮、总植物碱等常规成分含量。试验结果表明,大多数香味物质的含量及所测物质中醛类、酮类、醇类的总量都随着成熟度的增加而呈增加的趋势。上部烟叶随着其成熟度的增加,总植物碱的含量随之增加,还原糖、总糖的含量及糖碱比随之减小,总氮、蛋白质的含量则以尚熟时最高;对中部烟叶而言,还原糖、总糖、总挥发碱、蛋白质、总氮的含量以尚熟烟叶最高,总植物碱以成熟烟叶最高,糖碱比随着成熟度的增加而减小。      

‘玫瑰香’葡萄皮游离态和结合态香气成分分析

采用酸水解、同时蒸馏萃取(SDE)和气相色谱质谱联用(GC-MS)方法,对‘玫瑰香’葡萄皮游离态和结合态香气成分进行了定性、定量分析,检测出77种游离态香气成分,68种结合态香气成分,其中“泪柏醚”在葡萄中罕见报道。分析发现,‘玫瑰香’葡萄果皮中多数香气化合物以游离态和结合态两种形式存在,萜烯醇、芳香醇、脂肪酸等结合态含量高于游离态,芳樟醇、氧化芳樟醇、α-松油醇、橙花醇、雪松醇结合态含量分别是游离态的2.16、14.83、3.95、2.18、1.62倍。经对葡萄皮香气成分感官属性分析,其主体香韵为果香、花香、青香和脂蜡香,33种游离态香气成分OAV>1,结合态潜在香气物质主要为果香、花香、青香香韵的萜烯类(含氧单萜、倍半萜)和C₁₃降异戊二烯类化合物。因此认为‘玫瑰香’葡萄皮是一种重要的生物基香气物质资源,开发利用好这一资源具有经济和生态意义。     

几种国内外混合型卷烟烟丝中香味物质的分析比较

本文采用同时蒸馏萃取(SDE)的前处理分离方法,以及气相色谱和气质谱联用分析鉴定技术,对9种国内外混合型卷烟烟丝中的半挥发性酸性、碱性和中性成分进行了分析研究,共鉴定出37种碱性成分,83种中性成分和12种酸性成分。采用内标法定量测定了烟丝中的噻唑、吡啶、四甲基吡嗪、吡咯和吲哚等18种碱性香味成分;芳樟醇、二氢大马酮、香叶基丙酮、氧化异佛尔酮和二氢猕猴桃内酯等47种中性香味成分;乙酸、3-甲基戊酸、十四酸和棕榈酸等12种酸性成分。以及酸性、碱性和中性成分的总量,评价了该方法的重复性和前处理过程的回收率。研究结果表明,烟丝中中性成分总量的平均值国外卷烟比国产卷烟略高;烟丝中酸性成分总量的平均值国外卷烟比国产卷烟略低;烟丝中碱性成分总量的平均值(烟碱除外)国外卷烟是国产卷烟的2.2倍。      

CO2膨胀前后不同部位烤烟香味成分的变化

采用同时蒸馏萃取、GC/MS和内标法,对CO2膨胀前后福建上部、中部和下部烤烟的酸性、中性和碱性香味成分进行了定性定量对比分析.测定出丙酸、2-甲基戊酸、苯甲酸和月桂酸等15种酸性成分;糠醛、芳樟醇、β-紫罗兰酮等17种中性香味成分;吡嗪、噻唑、吡咯等16种碱性香味成分.结果表明,烟丝经膨胀后,酸性香味成分中的异戊酸、戊酸、β-甲基戊酸、己酸、辛酸、壬酸、月桂酸、油酸和肉豆寇酸含量均下降,而丁酸、苯甲酸的含量明显增加;中性香味成分中,异佛尔酮和香茅醇的变化不明显,中部和下部烟丝中的大马酮含量显著增加,其余14种成分有不同程度的损失;碱性成分中,噻唑、吡咯、吡嗪、2-乙基-3-甲基吡嗪的含量变化与烟叶部位相关,其余成分的含量均减少.     

基于宏基因组学的霍氏肠杆菌发酵解析及其烟叶品质提升机制研究

利用宏基因组学技术分析霍氏肠杆菌F8-1(Enterobacter hormaechei F8-1)发酵烟叶期间表面微生物的动态变化,结合烟叶中性香味成分分析及感官分析,探究霍氏肠杆菌F8-1提升发酵烟叶品质的机制。结果表明：发酵后烟叶香气质提高、润甜感突出、杂气和刺激性降低;巨豆三烯酮、茄酮、(E)-β-大马酮和二氢大马酮含量较发酵前分别提高37.40%、59.87%、53.02%和46.61%;烟叶发酵过程中霍氏肠杆菌、铜绿假单胞菌、阴沟肠杆菌为优势菌;糖苷水解酶类数量最多,占发酵期间烟叶表面微生物碳水化合物活性酶的78.3%;肠杆菌属的相对丰度与茄酮、巨豆三烯酮、(E)-β-大马酮、二氢大马酮等中性香味成分含量呈正相关,糖苷水解酶1(GH1)家族的相对丰度与茄酮、法尼基丙酮、巨豆三烯酮等含量呈正相关;GH1家族中的糖苷水解酶可能是烟叶发酵后感官品质提升的关键因素。     

溶剂萃取-中心切割多维色谱-质谱法测定烟草主要中性香味成分

采用溶剂萃取-中心切割多维气相色谱-质谱技术(MDGC/MS)建立了一种烟草主要中性香味成分的分析方法.0.5 g烟样经5 mL乙醚萃取和2 mL 5％H2SO4酸洗,静置过夜后萃取液用多维气相色谱-质谱分析;以甲基丁子香酚为内标,对茄酮、β-大马酮、香叶基丙酮、β-紫罗兰酮、巨豆三烯酮和二氢猕猴桃内酯等中性香味成分进行了定性定量测定,并与同时蒸馏萃取(SDE)-气质联用(GC/MS)法进行比较.结果表明:各待测组分检出限在0.02～0.18μg/mL之间,回收率为80.0％～ 123.4％,日内相对标准偏差≤7.5％.该方法快速、简便、准确,适用于烟草中性香味成分的批量测试.     

不同部位、成熟度及颜色的云南烤烟中某些中性香味成分的分析研究

对我国不同部位、不同成熟度及不同颜色的云南烤烟中的某些中性香味成分进行了分析,烟叶经溶剂抽提和酸、碱、中和分离后,对中性抽提物用顶空技术分离出香味成分。用毛细管气相色谱测定了苯甲醛、6-甲基-5-庚烯-2-酮、苯甲醇、2-苯乙醇、异佛尔酮、氧化异佛尔酮、β-紫罗兰酮、二氢猕猴桃内酯、巨豆三烯酮(四个异构体)茄酮及新植二烯等十四种香味成分的含量。就所定量的香味成分而言,上部烟叶中香味成分的含量最丰富,中部烟叶次之,下部烟叶最少;成熟度好的烟叶中香味成分的含量比成熟度较差的烟叶丰富;桔黄色的烟叶中香味成分的总含量高于红棕色及柠檬黄色的烟叶。      

基于宏基因组学的不同陈化时间烟草源功能微生物筛选

利用宏基因组学解析云南烟叶在不同陈化时间表面微生物群落结构及功能基因演替,跟踪烟叶陈化过程中的中性香味成分动态变化,分析微生物、酶基因与中性香味成分的相关性,并指导筛选烟草源功能微生物。结果表明：在烟叶陈化第3、6、9和12个月时,其表面优势菌属分别为鞘氨醇单胞菌属(Sphingomonas)、肠杆菌属(Enterobacte)、泛菌属(Pantoea)和不动杆菌属(Acinetobacter);陈化过程中烟叶的中性香味成分如苯甲醇、苯乙醛、2-乙酰基吡咯、茄酮、大马酮、巨豆三烯酮等总体呈增长趋势,糠醛和β-环柠檬醛则呈现先增加后降低的趋势,烃类化合物含量呈下降趋势;克雷伯菌属(Klebsiella)与β-大马酮、巨豆三烯酮和茄酮等呈显著正相关,不动杆菌属(Acinetobacter)与2-乙酰基呋喃,芳樟醇、巨豆三烯酮呈显著正相关,大部分碳水化合物活性酶与苯乙醛、苯甲醛、糠醇和西柏烯等成分呈负相关,多数糖苷酶与中性香味成分呈正相关;在烟叶陈化过程中共筛选得到75株微生物,微生物种类及其功能与宏基因组分析结果基本吻合,说明宏基因组分析结果可以指导微生物筛选工作,增强筛选目的性,提高筛选...     

Contribution to aroma potential of Andean blackberry (Rubus glaucus Benth.)

Free and glycosidically bound volatiles of purees from Andean blackberry (Rubus Glaucus Benth.) fruit were determined. Free volatile compounds were extracted by two techniques: solvent extraction and Solid-Phase Micro-Extraction (SPME). The glycosidically bound volatiles were isolated using Solid Phase Extraction (SPE) technique. The analysis of free volatiles and enzymatically released aglycons were performed by GC-MS. Fifty five volatile compounds were identified and quantified from solvent extraction. The major class was the carboxylic acids (68.8%), dominated by palmitic acid (16.8%) and benzoic acid (15.0%). Alcohols were highly represented (23.4%), with 2-heptanol (10.6%) and terpinen-4-ol (5.7%) being prevalent compounds of this class. Using HS-SPME, among the seventy-one identified compounds, alcohols (47.3%) including 2-heptanol (17.9%) and terpinen-4-ol (20.0%), and esters (39.8%) with ethyl and methyl benzoate (33.9 and 3.8% respectively) were the two predominant classes. ??-damascenone, a potent flavour compound was detected using SPME method. Fifty-three aglycons were identified, acids (57.4%), norisoprenoids (15.4%), terpenic alcohols (10.3%) and some aliphatic and shikimic alcohols (15.0%) predominated in the glycosidically bound fraction. Acetylenic precursors of ??-damascenone were present at noticeable level in the glycosidic fraction.     

毛细管气相色谱法测定卷烟中的游离氨基酸

本试验描述了一种用于烟草中游离氨基酸测定的毛细管气相色谱方法,这种方法基于氯甲酸乙酯衍生化。1g烟样用75%乙醇经超声波振荡提取后,游离氨基酸用阳离子交换树脂纯化,然后在水溶液中用氯甲酸乙酯(ECF)衍生化。该方法简单、衍生化可在水溶液中进行且速度快(常温下仅需5秒)、衍生物较稳定、重现性和回收率实验结果均令人满意。用该法对加料前后的烟草和卷烟中的游离氨基酸进行了分析,结果发现,加料后游离氨基酸尤其是脯氨酸含量呈减少趋势。23个品牌的国内外卷烟分析表明,云南产的卷烟中游离氨基酸平均含量最高,国外卷烟略低,安徽、上海等华东地区生产的卷烟含量最低。其中云南卷烟所含脯氨酸比其它卷烟要高得多,而国外卷烟的天冬氨酸、天冬酰氨含量较高。      

SDE and SPME Analysis of Flavor Compounds in Jin Xuan Oolong Tea

Simultaneous distillation‐extraction (SDE) and solid phase micro extraction (SPME) are procedures used for the isolation of flavor compounds in foods. The purpose of this study was to optimize SDE conditions (solvent and time) and to compare SDE with SPME for the isolation of flavor compounds in Jin Xuan oolong tea using GC‐MS and GC‐O. The concentration of volatile compounds isolated with diethyl ether was higher (P < 0.05) than for dichloromethane and concentration was higher at 40 min (P < 0.05) than 20 or 60 min extractions. For SDE, 128 volatiles were identified using GC‐MS and 45 aroma active compounds using GC‐O. Trans‐nerolidol was the most abundant compound in oolong tea. The number of volatiles identified using GC‐MS was lower in SPME than SDE. For SPME, 59 volatiles and 41 aroma active compounds were identified. The composition of the volatiles isolated by the 2 methods differed considerably but provided complementary information.     

加料复烤对烤烟烟叶主要化学成分、香味成分和感官质量的影响

研究了打叶复烤加料以及烤后放置不同时间的部分国产烤烟烟叶主要化学成分、香味成分和感官质量的变化。结果表明:①加料与未加料的复烤烟叶样品的总糖、总烟碱、焦油、烟气烟碱和CO都随着烘烤和烤后放置时间的延长而逐渐降低;②复烤后放置3～6个月,大多数加料烟叶样品的总糖、总烟碱、焦油和烟气烟碱等的下降幅度明显大于未加料样品,且随着放置时间的延长,二者的区别逐渐减小;③CO的降幅二者基本接近;④加料与未加料复烤烟叶样品的香味物质总量随着烤后放置时间的延长都逐渐增加,但加料样品香味物质增幅要大于未加料样品,尤其是复烤后放置3～6个月,其香味物质的增幅明显高于未加料样品;⑤加料与未加料复烤烟叶样品的感官质量随着复烤后放置时间的变化与其总香味物质的变化一致。     

Characterisation of bound volatile compounds of a low flavour kiwifruit species: Actinidia eriantha

Aroma compounds in fruit are known to occur in free and glycosidically bound forms. The bound volatile fraction of a low flavour kiwifruit species, Actinidia eriantha, was studied. The fruit have a bland and grassy flavour. Glycosidic precursors were isolated from juice by adsorption onto an Amberlite XAD-2 column. After enzymatic hydrolysis with Rapidase AR2000, the released aglycones were analysed by GC–MS. Alcohols, terpenoids and phenolics were the most numerously represented compound classes. Alcohols, benzenoids and phenolics showed the highest concentrations. Major compounds were 2-phenylethanol, furfuryl alcohol, (Z)-3-hexen-1-ol, coniferyl alcohol, isoamyl alcohol and linolenic acid. Several of the bound compounds found, including linoleic, linolenic and benzoic acids and coniferyl alcohol, are precursors of odorous volatiles. Many compounds detected as bound volatiles have not been previously reported as free volatiles in A. eriantha. The bound volatile composition of A. eriantha also showed differences with those of other kiwifruit species.     

Untersuchungen des Trauben- und Weinaromas

The free aroma compounds of wines were isolated by liquid-liquid extraction with a mixture of trichlorofluoromethane/dichloromethane whereas the enrichment of glycosidically bound aroma components was carried out by adsorption on XAD and subsequent elution with various solvents. The glycosidic compounds were liberated enzymatically byβ-glucosidases. The extracts were analysed by gas chromatography. In 92 wines of the varieties Riesling, Weißburgunder, Silvaner and Ruländer of three vintages (1989, 1990, 1991), from different regions and wine producers 160 free aroma compounds were quantitatively determined. By use of statistical analysis the components were reduced to 23 significant aroma constituents. Analytical characterization of the investigated grape varieties was possible with these components. Terpene compounds, unsaturated C₆-alcohols and some components of the amino acid metabolism were especially typical for the varietal character. Using 18 glycosidically bound aroma substances it could be shown that these components can also contribute significantly to the characterization of grape varieties where monoterpenes and norisoprenoids play an important role. Computing at the same time free and glycosidically bound aroma components in discriminant analysis the characterization of neutral grape varieties (Silvaner, Ruländer, Weissburgunder) can be considerably improved.     

云南烤烟复烤烟片B2F加料陈化研究

研究了自然陈化过程中加料和未加料云南复烤烟片B2F香味成分(中性、酸性和碱性)、pH值以及感官质量的变化。结果表明:与未加料的样品相比,加料陈化改变了B2F醇类成分和酯类成分的变化态势,使中性香味成分达到最大值的时间提前;酸性成分的变化趋势虽然未变,但在陈化初期的变化幅度不同;pH值的下降速度变慢。香味成分总量达到最大值的时间提前,一些重要香味成分在高值区的持续时间缩短;感官质量的峰值区提前出现,且最佳时间区间相应缩短。结论是加料加快了云南烤烟复烤烟片B2F的自然陈化速度,致使其感官质量出现下降的时间提前,因此,加料复烤B2F应在最佳陈化时间区间内尽快使用。     

The effect of air-drying on glycosidically bound volatiles from seasonally collected origano (Origanum vulgare ssp. hirtum) from Croatia

The glycosidically bound volatiles were isolated from fresh and airdried origano by exhaustive percolation with ethyl acetate. After the purification of glycosidic fraction, the enzymatic hydrolysis with beta-glucosidase was performed. The obtained aglycones were analysed by GC-MS. Eighteen compounds were identified. The seasonal variations of main aglycone contents from the fresh plant material were: thymoquinone (3.10-6.18 mg/kg), benzyl alcohol (1.33-3.62 mg/kg), 3,5,5-trimethyl-4-(3-hydroxy-1-buthenyl)-2-cyclohexen-1-on (0.51-3.35 mg/kg), 2-phenyl ethanol (0.42-2.98 mg/kg), eugenol (0.93-2.55 mg/kg), thymol (0.70-1.40 mg/kg) and carvacrol (0.88-1.40 mg/kg). The season of collecting influenced the content and composition of the glycosidically bound volatiles of origano. Air-drying effected mostly the yield of these compounds.     

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).     

顶空固相微萃取和同时蒸馏萃取法分析猪肉汤的挥发性成分

采用顶空固相微萃取法(HS-SPME)和同时蒸馏萃取法(SDE)提取清炖猪肉汤中挥发性成分,结合气相色谱-质谱联用技术(GC-MS)进行分析,结果共检测出77种挥发性化合物,其中烃类和醛类最多,均有22种,其次是醇类17种和酸类6种,另外酯类、酮类和杂环类分别有4、3、3种。HS-SPME法和SDE法分别鉴定出42种和49种挥发性组分。两种提取方法相比较,采用SPME法提取到醛类的种类明显多于SDE法,而烃类、醇类和酯类的种类明显少于SDE法。SDE法适合对高沸点、低挥发性物质的分离;SPME法具有快速简便、不使用溶剂和样品检测非破坏性等优点,适合易挥发性化合物的检出。只有将两种方法结合起来,才能得到对产品的挥发性物质的综合评价。