基于HS-SPME-GC-MS分析三种茶坯窨制桂花茶的香气成分

为探究3种茶坯窨制桂花后的香气差异,采用顶空固相微萃取-气相色谱-质谱联用技术（Headspace Solid-Phase Microextraction-Gas Chromatography-Mass Spectrometry,HS-SPME-GC-MS）、感官审评和香气活性值（Odor Activity Value,OAV）对桂花红茶、桂花美人茶和桂花乌龙茶的香气成分进行分析。结果显示,窨制后3种桂花茶中共检测出726种共有香气成分,324种差异香气成分（P<0.05）。桂花茶以杂环化合物、萜类、酯类、烃类及酮类为主,占比78.73%。桂花茶中的关键呈香成分（OAV>10）为呋喃酮、α-紫罗兰酮、芳樟醇、柠檬醛、脱氢芳樟醇、月桂醇等。其中桂花红茶主要香气成分为芳樟醇、月桂烯、α-紫罗兰酮、β-紫罗兰酮、乙酸芳樟酯、苯甲醇、月桂醇等;桂花美人茶中主要香气成分为苯乙醛、柠檬醛、脱氢芳樟醇、芳樟醇、萜品油烯、α-紫罗兰酮、β-紫罗兰酮等;桂花乌龙茶主要香气成分为α-紫罗兰酮、吲哚、β-紫罗兰酮、月桂醇等。研究表明,桂花窨制能明显改善不同茶坯香气,赋予茶坯较浓郁持久的桂花香,其...     

SPME-GC-MS联用法分析栀子红茶香气成分

采取固相微萃取和气相色谱-质谱(SPME-GC-MS)联用技术方法对栀子红茶香气成分进行分析,以期为栀子红茶产业化发展提供理论基础。共从栀子红茶中检测出93种香气成分,其中主要香气贡献成分包括醇类、酯类、其他类、酸类和醛类化合物,其中香叶醇、水杨酸甲酯、芳樟醇、六氢茴香素、苯乙醇、芳樟醇氧化物Ⅱ、苯甲酸甲酯、棕榈酸、芳樟醇氧化物Ⅳ、茉莉酮内酯、环丁甲酸己酯、芳樟醇氧化物Ⅰ、顺-3-己烯醇丁酸酯、反-异丁子香酚、苯甲醇、苯乙醛、α-法呢烯和柠檬醛等18种化合物是香气成分的主体物质,同时检出在对照茶坯中未检出的43种香气成分。六氢茴香素、苯甲酸甲酯、茉莉酮内酯、环丁甲酸己酯、反-异丁子香酚和α-法呢烯6种含量相对较高的成分可能是栀子红茶具有浓郁栀子花香的特殊成分。     

槐花绿茶窨制技术优化及其香气分析

本研究以绿茶为茶坯、槐花为花源,通过单因素实验和正交试验,分析花茶配比、窨制时间、窨制次数对槐花绿茶香气品质的影响,探讨窨制过程的最佳技术条件,利用顶空固相微萃取法(HS-SPME)和气相色谱-质谱联用仪(GC-MS)分析槐花绿茶的特征性香气成分。结果表明:槐花与绿茶配比3:5、窨制时间4 h、窨制次数3次为槐花绿茶窨制的最佳技术条件;槐花绿茶中主要存在(E)-β-金合欢烯、α-蒎烯、苯甲酸甲酯、萜品油烯、1-甲基萘、茉莉酮、2-庚酮、吲哚、对甲苯甲醚、3-蒈烯等特征性香气成分,其中α-蒎烯、萜品油烯、苯甲酸甲酯、3-蒈烯对槐花绿茶香气品质的影响更大,相关系数依次为0.86、0.83、0.82、0.77。     

不同普洱茶原料渥堆发酵过程中香气成分的变化研究

目的探讨不同普洱茶原料渥堆发酵过程中香气成分的变化情况。方法以三级晒青茶毛茶(1号堆)和叶片粗老含茶梗的老黄片(2号堆)为原料,通过设置不同的初始含水量和翻堆次数,采取全自动顶空固相微萃取(headspace solid-phase micro extraction,HS-SPME)和气相色谱-质谱(gas chromatography-mass spectrometry,GC-MS)法分析其香气成分,研究不同普洱茶原料渥堆发酵过程中香气组分的变化。结果随着翻堆次数的增加,不同原料普洱茶芳樟醇、苯甲醇、β-苯乙醇、二氢猕猴桃内酯均呈波浪式降低趋势,芳樟醇氧化物(Ⅱ、Ⅲ、Ⅳ)呈增加趋势,1,2,3-三甲氧基苯和1,2,4-三甲氧基苯呈波浪式增加趋势,α-柏木烯呈降低趋势,出堆时含量骤然增加;1号堆α-紫罗兰酮、香叶基丙酮、β-紫罗兰酮呈降低趋势,2号堆呈波浪式降低趋势,出堆时含量骤然增加,1号堆芳樟醇氧化物I和α-松油醇呈波浪式增加趋势,2号堆则呈波浪式降低趋势。结论渥堆发酵过程中,不同普洱茶原料主要的香气成分变化一致,不同普洱茶原料酮类物质及芳樟醇氧化物I和α-松油醇变化不同,本研究为普洱茶渥堆发酵工艺及品质稳定提供一定的技术支持。     

东方美人茶和铁观音香气成分的比较研究

选用东方美人茶和铁观音为研究对象,采用顶空-固相微萃取(HS-SPME)法富集其香气物质和GC-MS进行香气成分分析。结果表明：东方美人茶和铁观音在香气组成上存在明显差异;东方美人茶的香气成分比铁观音丰富,以醇类化合物为主,其醇类、酮类和酚类化合物含量均高于铁观音,而酯类和碳氢化合物等含量低于铁观音;东方美人茶的香气成分主要是香叶醇、2,6-二叔丁基对甲苯酚、β-芳樟醇、反式-氧化芳樟醇、芳樟醇氧化物Ⅰ、2,6-二甲基-3,7-辛二烯-2,6-二醇等;而铁观音的主要香气成分是反式-橙花叔醇、α-法呢烯、吲哚、丁酸-2-甲基-2-苯乙酯、丁酸苯乙酯等。     

负氧离子在仓储过程中对普洱生茶挥发性 成分的影响

目的提升有益内含香气成分和降低茶叶"烟味"杂异味以及提高生茶整体品质。方法采用蒸馏萃取法(simultaneous distillation extraction,SDE)富集其香气物质,并采用气相色谱-质谱联用法对负氧离子仓储前后普洱生茶进行香气成分对比和分析。结果 2003年的龙记生饼和2005年的古道生饼香气物质含量呈现很大差异。其中正己醛、莰烯、苯甲醛、苯甲醇、α-蒎烯、脱氢芳樟醇、异龙脑、萘、苯乙醛、藏花醛、3-蒈烯、2-甲基萘、吲哚、1-甲基萘、2-乙烯基萘、1,3-二甲基萘、二氢猕猴桃内酯、菲、萘、α-法呢烯、正二十烷、乙酸冰片酯、十四烷、烯萜类等物质存在"烟味",芳樟醇及其氧化物突出。经过负氧离子仓储后,"烟味"等杂异物质有所下降,整体口感明显提升。结论负氧离子仓储可改善普洱生茶品质。     

茉莉花茶香气成分与品质之间关系的初步研究

本文提取并分析了三种不同级别茉莉花茶的香气挥发性成分,讨论并确定了香气挥发油总量是决定香气浓度的基础;推测低沸点物质对香气的鲜灵度有着不可忽视的影响。此外,讨论了茉莉花茶香气成分与品质之间的关系,确定了芳樟醇,乙酸苄酯,顺-3-己烯醇,水杨酸甲酯,苯甲醇为茉莉花茶的主要香气成份,并且前四种物质与香气的品质呈正相关性。     

压饼处理对白茶陈化香气的影响

本文研究经压饼处理后不同等级陈化白茶散茶和饼茶香气成分的差异,探明压饼处理对陈化白茶香气的影响,为白茶加工提供科学依据。采用顶空固相微萃取(Headspace solid-phase microextraction,HS-SPME)萃取茶叶香气,通过气相质谱联用(Gas chromatography/mass spectrometer,GC-MS)进行检测。同时,采用国标GB/T 23776-2018的方法对茶叶进行感官审评。结果表明,在陈化白茶中共检出53种挥发性香气成分,其中主要有苯甲醛、苯甲醇、芳樟醇及其氧化物、苯乙醇、α-萜品醇、香叶醇、α-雪松烯、β-雪松烯、石竹烯以及雪松醇等。对比以散茶、饼茶陈化白茶的香气成分差异,发现陈化白茶压饼后芳樟醇及其氧化物、己酸甲酯与β-紫罗酮等许多花果香物质减少,其中芳樟醇及其氧化物明显下降;而雪松醇、雪松烯、酸龙脑酯与α-蒎烯等具有木香、药香物质增加,其中雪松醇与雪松烯大幅增加。压饼处理对白茶陈化香气种类和含量都有着较大的影响,使得陈化白茶饼的陈香更显,枣香、药香等特征香型更加突出,而散茶则在花果香的保留上更具优势。进一步分析不同等级陈化白茶间的香气差异,与白毫银针相比,白牡丹和寿眉压饼陈化后香气品质更佳。     

顶空固相微萃取-气相色谱-质谱法对比分析毛火温度对信阳毛尖茶香气成分的影响

目的 研究毛火温度对信阳毛尖茶香气成分的影响。方法 选取不同品种、干燥毛火温度的信阳毛尖茶,并采用顶空固相微萃取-气相色谱-质谱法(headspace-solid phase microextraction-gas chromatography-mass spectrometry, HS-SPME-GC-MS)对供试样茶香气物质进行分析。结果 醛类、醇类、酯类、酮类、酸类、芳香烃以及碳氢、杂环氧化物是信阳毛尖茶的主要香气化合物种类。140℃毛火烘焙群体种信阳毛尖茶供试样中β-环柠檬醛与顺式芳樟醇氧化物(呋喃)含量最高; 140℃毛火烘焙乌牛早信阳毛尖茶供试样中柠檬烯、γ-松油烯、肉桂烯含量最高;110℃毛火烘焙群体种信阳毛尖茶供试样中1-反-(+)-橙花叔醇含量最高;110℃毛火烘焙乌牛早信阳毛尖茶供试样中芳樟醇和反式芳樟醇氧化物(吡喃)含量最高。140℃毛火烘焙信阳毛尖茶供试样的表没食子儿茶素没食子酸酯(epigallocatechin gallate, EGCG)、表没食子儿茶素(epigallocatechin, EGC)的含量均低于110℃毛火烘焙信阳毛尖茶供试样。结论 在信阳...     

桂花红茶窨制技术及香气成分HS-SPME/GC-O-MS分析

为了探究桂花红茶的最佳窨制工艺及特征香气成分,设置正交试验并采用顶空固相微萃取结合GC-O-MS技术分析香气成分。由正交试验和感官审评可知:最佳窨制工艺为花茶配比3:10、窨制3次、每次窨制4 h;GC-MS分析表明桂花红茶吸附的香气成分主要有环己烯醇、壬醛、丙位癸内酯和植酮等4种,窨制过程增加的其它香气成分有:1-辛烯-3-醇、2-甲基-2-壬烯-1-醇、4-氯-双环[2.2.1]庚-2-酮、3-甲基-2-呋喃甲基丁酸酯、正戊酸己酯、正戊酸叶醇酯、丁酸苯乙酯等7种,推测这11种成分是桂花红茶香气形成的主体成分;GC-O结果表明:其中壬醛有油脂和甜橙香,丙位癸内酯有愉快桃子香,1-辛烯-3-醇有干草香,正戊酸叶醇酯有奶油香、果香,丁酸苯乙酯有蜜甜香,认为这5种成分是桂花红茶表现桂花香的特征性成分;此外,桂花红茶窨制过程中醇类物质相对含量显著降低,而酮类和酯类成分明显增加。     

Reliable identification of grapevine rootstock varieties using RAPD PCR on woody samples

Since grapevine ( Vitis spp .) rootstock material is being traded increasingly as disbudded woody material a lack of distinctive morphological features on such material necessitates an alternative and reliable means of identification. Methods described here were developed for rapid and efficient extraction of DNA from woody samples rich in phenolic compounds and polysaccharides, and for subsequent identification of varieties by RAPD PCR. Using these methods, and with the application of only one selected RAPD primer, we were able to differentiate sixteen rootstock varieties, including the seven varieties most commonly used in Germany. Problems commonly encountered with reproducibility of RAPD patterns were avoided by choosing primers with a dinucleotide sequence and a high G/C content that allowed a rather high annealing temperature of 45°C. Methods described here should also be useful for other horticultural crops, especially those with woody tissues rich in phenolic compounds and polysaccharides.     

An internet compendium of analytical methods and spectroscopic information for monomers and additives used in food packaging plastics

An internet website (http://cpf.jrc.it/smt/) has been produced as a means of dissemination of methods of analysis and supporting spectroscopic information on monomers and additives used for food contact materials (principally packaging). The site which is aimed primarily at assisting food control laboratories in the European Union contains analytical information on monomers, starting substances and additives used in the manufacture of plastics materials. A searchable index is provided giving PM and CAS numbers for each of 255 substances. For each substance a data sheet gives regulatory information, chemical structures, physico-chemical information and background information on the use of the substance in particular plastics, and the food packaging applications. For monomers and starting substances (155 compounds) the infra-red and mass spectra are provided, and for additives (100 compounds); additionally proton NMR are available for about 50% of the entries. Where analytical methods have been developed for determining these substances as residual amounts in plastics or as trace amounts in food simulants these methods are also on the website. All information is provided in portable document file (PDF) format which means that high quality copies can be readily printed, using freely available Adobe Acrobat Reader software. The website will in future be maintained and up-dated by the European Commission's Joint Research Centre (JRC) as new substances are authorized for use by the European Commission (DG-ENTR formerly DGIII). Where analytical laboratories (food control or other) require reference substances these can be obtained free-ofcharge from a reference collection housed at the JRC and maintained in conjunction with this website compendium.     

Chlorohydrins of bisphenol A diglycidyl ether (BADGE) and of bisphenol F diglycidyl ether (BFDGE) in canned foods and ready-to-drink coffees from the Japanese market

BADGE.2HCl and BFDGE.2HCl were determined in 28 samples of ready-to-drink canned coffee and 18 samples of canned vegetables (10 corn, 5 tomatoes and 3 others), all from the Japanese market. HPLC was used as the principal analytical method and GCMS for confirmation of relevant LC fractions. BADGE.2HCl was found to be present in one canned coffee and five samples of corn, BFDGE.2HCl in four samples of canned tomatoes and in one canned corn. No sample was found which exceeded the 1mg/kg limit of the EU for the BADGE chlorohydrins. However the highest concentration was found for the sum of BFDGE.2HCl and BFDGE.HCl.H₂O at a level of 1.5mg/kg. A Beilstein test confirmed that all cans containing foods contaminated with BADGE.2HCl or BFDGE.2HCl had at lest one part coated with a PVC organosol.     

European priorities for research to support legislation in the area of food contact materials and articles

A strong science base is required to underpin the planning and decision-making process involved in determining future European community legislation on materials and articles in contact with food. Significant progress has been made in the past 5 years in European funded work in this area, with many developments contributing to a much better understanding of the migration process, and better and simpler approaches to food control. In this paper this progress is reviewed against previously identified work-areas (identified in 1994) and conclusions are reached about future requirements for R&D to support legislation on food contact materials and articles over the next 5 or so years.     

Aroma characterization of various apricot varieties using headspace–solid phase microextraction combined with gas chromatography–mass spectrometry and gas chromatography–olfactometry

The characterization of the aromatic profile of several apricot cultivars with molecular tracers in order to obtain objective data concerning the aromatic quality of this fruit was undertaken using headspace–solid phase microextraction (HS–SPME). Six apricot cultivars were selected according to their organoleptic characteristics: Iranien, Orangered, Goldrich, Hargrand, Rouge du Roussillon and A4025. The aromatic intensity of these varieties measured by HS–SPME–Olfactometry were defined and classified according to the presence and the intensity of grassy, fruity and apricot like notes. In the six varieties, 23 common volatile compounds were identified by HS–SPME–GC–MS. Finally, 10 compounds, ethyl acetate, hexyl acetate, limonene, β-cyclocitral, γ-decalactone, 6-methyl-5-hepten-2-one, linalool, β-ionone, menthone and (E)-hexen-2-al were recognized by HS–SPME–GC–O as responsible of the aromatic notes involved in apricot aroma and considered as molecular tracers of apricot aromatic quality which could be utilized to discriminate apricot varieties.     

Textural Properties of Cold-set Gels Induced from Heat-denatured Whey Protein Isolates

A 9% whey protein (WP) isolate solution at pH 7.0 was heat-denatured at 80°C for 30 min. Size-exclusion HPLC showed that native WP formed soluble aggregates after heat-treatment. Additions of CaCl2 (10–40 mM), NaCl (50–400 mM) or glucono-delta-lactone (GDL, 0.4–2.0%, w/v) or hydrolysis by a protease from Bacillus licheniformis caused gelation of the denatured solution at 45°C. Textural parameters, hardness, adhesiveness, and cohesiveness of the gels so formed changed markedly with concentration of added salts or pH by added GDL. Maximum gel hardness occurred at 200 mM NaCl or pH 4.7. Increasing CaCl2 concentration continuously increased gel hardness. Generally, GDL-induced gels were harder than salt-induced gels, and much harder than the protease-induced gel.     

Tests of potential functional barriers for laminated multilayer food packages. Part I: Low molecular weight permeants

The advent of the functional barrier concept in food packaging has brought with it a requirement for fast tests of permeation through potential barrier materials. In such tests it would be convenient for both foodstuffs and materials below the functional barrier (sub-barrier materials) to be represented by standard simulants. By means of inverse gas chromatography, liquid paraffin spiked with appropriate permeants was considered as a potential simulant of sub-barrier materials based on polypropylene (PP) or similar polyolefins. Experiments were performed to characterize the kinetics of the permeation of low molecular weight model permeants (octene, toluene and isopropanol) from liquid paraffin, through a surrogate potential functional barrier (25 μm-thick oriented PP) into the food simulants olive oil and 3% (w/v) acetic acid. These permeation results were interpreted in terms of three permeation kinetic models regarding the solubility of a particular model permeant in the post-barrier medium (i.e. the food simulant). The results obtained justify the development and evaluation of liquid sub-barrier simulants that would allow flexible yet rigorous testing of new laminated multilayer packaging materials.     

Occurrence of bisphenol-F-diglycidyl ether (BFDGE) in fish canned in oil

The levels of bisphenol-F-diglycidyl ether (BFDGE) were quantified as part of a European survey on the migration of residues of epoxy resins into oil from canned fish. The contents of BFDGE in cans, lids and fish collected from all 15 Member States of the European Union and Switzerland were analysed in 382 samples. Cans and lids were separately extracted with acetonitrile. The extraction from fish was carried out with hexane followed by re-extraction with acetonitrile. The analysis was performed by reverse phase HPL C with fluorescence detection. BFDGE could be detected in 12% of the fish, 24% of the cans and 18% of the lids. Only 3% of the fish contained BFDGE in concentrations considerably above 1mg/kg. In addition to the presented data, a comparison was made with the levels of BADGE (bisphenol-A-diglycidyl ether)analysed in the same products in the context of a previous study.     

Contribution of European research to risk analysis

The European Commission's, Quality of Life Research Programme, Key Action 1—Health, Food & Nutrition is mission-oriented and aims, amongst other things, at providing a healthy, safe and high-quality food supply leading to reinforced consumer confidence in the safety of European food. Its objectives also include the enhancing of the competitiveness of the European food supply. Key Action 1 is currently supporting a number of different types of European collaborative projects in the area of risk analysis. The objectives of these projects range from the development and validation of prevention strategies including the reduction of consumers risks; development and validation of new modelling approaches; harmonization of risk assessment principles, methodologies, and terminology; standardization of methods and systems used for the safety evaluation of transgenic food; providing of tools for the evaluation of human viral contamination of shellfish and quality control; new methodologies for assessing the potential of unintended effects of genetically modified (genetically modified) foods; development of a risk assessment model for Cryptosporidium parvum related to the food and water industries; to the development of a communication platform for genetically modified organism, producers, retailers, regulatory authorities and consumer groups to improve safety assessment procedures, risk management strategies and risk communication; development and validation of new methods for safety testing of transgenic food; evaluation of the safety and efficacy of iron supplementation in pregnant women; evaluation of the potential cancer-preventing activity of pro- and pre-biotic ('synbiotic') combinations in human volunteers. An overview of these projects is presented here.