HS-SPME-GC-MS分析伽师瓜籽油挥发性物质

采用顶空固相微萃取—气质联用法(HS-SPME-GC-MS)对冷榨伽师瓜籽油和不同烤籽温度下的热榨伽师瓜籽油的挥发性物质进行分析。结果表明:伽师瓜籽油中共检出115种挥发性物质,主要是羧酸类、醛类、酮类、杂环类、醇类、酯类和烷烃类化合物;冷榨伽师瓜籽油的挥发性物质主要是羧酸类、醛类及醇类化合物,相对质量分数分别为36.65%、29.50%、11.56%;烤籽温度为110℃和130℃下的热榨伽师瓜籽油主要挥发性物质为醛类化合物,且含量与冷榨伽师瓜籽油有较大差异;烤籽温度为150、170、190、210℃下热榨伽师瓜籽油的主要挥发性成分为吡嗪、呋喃等杂环类化合物和醛类化合物。     

HS-SPME-GC-MS分析冷榨和热榨葵花籽油的挥发性物质

采用顶空固相微萃取-气质联用法(HS-SPME-GC-MS)对冷榨葵花籽油和不同炒籽温度下的热榨葵花籽油的挥发性物质进行分析。结果表明:葵花籽油样品中共检测出59种挥发性物质,主要是萜烯类、醛酮类、烷烃类、杂环类及羧酸类物质;冷榨葵花籽油的挥发性物质主要是萜烯类、烷烃类及醛酮类物质,含量分别为38.96%、16.19%和12.20%;炒籽温度110、130、150℃下的热榨葵花籽油的主要挥发性物质的种类与冷榨葵花籽油的相似,但含量有很大区别,而170℃和190℃下的热榨葵花籽油的主要挥发性物质是吡嗪等杂环类物质和醛酮类物质。     

热榨和冷榨胡麻油挥发性物质与关键风味物质组成的分析

采用顶空固相微萃取-气相色谱-质谱联用技术,对比了冷榨和热榨胡麻油中挥发性物质的组成,并结合相对气味活度值法,分析了胡麻油中关键风味物质。结果表明:胡麻油中挥发性物质有醛类、醇类、杂环类、酮类、烷烃类、酸类和酯类,含量最高的是醛类物质,主要是己醛和反式-2,4-庚二烯醛;冷榨和热榨胡麻油醛类物质分别占挥发性物质总含量的40.79%和68.53%,两种胡麻油共有的关键风味物质有壬醛、己醛、反-2-辛烯醛和反式-2,4-庚二烯醛;冷榨和热榨胡麻油挥发性物质中对总体风味贡献最大的分别是壬醛和反式-2,4-癸二烯醛;热榨胡麻油的关键风味物质中还有2,5-二甲基吡嗪和2-戊基呋喃,这两种物质是热榨胡麻油特有的烤香味的来源。     

HS-SPME-GC-MS-O联用分析不同加工工艺亚麻籽油特征香气成分

以河北省张家口地区不同加工工艺的亚麻籽油为研究对象,采用顶空-固相微萃取法对亚麻籽油香气成分进行萃取分离,借助气相色谱-质谱联用技术分别分析热榨亚麻籽油和冷榨亚麻籽油的挥发性物质构成,并结合气相色谱-嗅觉技术对2?种不同加工工艺的亚麻籽油关键性香气成分进行分析。检测出热榨亚麻籽油特征性香气成分共16?种,包括7?种醛类、4?种杂环类、3?种醇类、1?种酸类、1?种酯类。冷榨亚麻籽油共鉴定出14?种特征性香气成分,包括6?种醛类、4?种醇类、3?种酸类、1?种酯类,冷榨亚麻籽油和热榨亚麻籽油共有香气成分7?种。2,5-二甲基吡嗪、2,3,5-三甲基吡嗪、(E)-2-己烯醛是热榨亚麻籽油特有香气成分,是其烤香味、油脂味的重要来源;乙酸是冷榨亚麻籽油特有香气成分。     

自制中式硬质干酪风味物质的研究

利用顶空固相微萃取气质联用技术(SPME/GC-MS)对自制中式硬质干酪的挥发性风味物质进行分离鉴定。首先通过单因素实验确定了顶空固相微萃取最优萃取条件为:平衡时间35min,萃取时间40 min,萃取温度50℃。共检测出42种挥发性风味化合物,其中羧酸类、醇类、酮类、醛类、酯类、烃类、杂环类化合物等是主要风味物质。     

番茄籽油的挥发性成分分析

番茄籽油是具有开发潜力的植物油。采用顶空固相微萃取-气相色谱质谱联用技术分析新疆、内蒙古、甘肃和浙江4个不同产地低温压榨番茄籽油的风味,共鉴定出58种挥发性风味物质,包括20种醛类化合物、5种烯类化合物、12种酯类化合物、6种醇类化合物、5种酮类化合物、3种酸类化合物、6种杂环类化合物和1种苯酚类化合物。综合而言,番茄籽油的特征风味成分主要包括油脂氧化产物和来源于番茄本身固有的香气成分。     

花生炒籽工艺条件与小榨花生油风味品质的相关性研究

为制备风味品质较优的小榨花生油,在不同炒籽条件下处理花生仁,压榨制备小榨花生油。对小榨花生油进行感官评价,基于主成分分析(PCA)分析炒籽条件与小榨花生油风味类型的相关性,并对小榨花生油风味物质含量进行了测定。结果表明：炒籽温度低于160℃时小榨花生油呈生香味、甜香味,风味弱,在炒籽温度160～165℃时呈甜香味、熟坚果味,在炒籽温度170℃时开始表现出煳味,并且随着炒籽温度的升高煳味增大;当入炒水分由4.09%升高到7.12%时,小榨花生油的风味类型没有明显改变,风味强度略有增加;在炒籽温度145～160℃条件下,醛类和吡嗪类化合物为主要呈味物质,在炒籽温度165℃以上时,吡嗪类化合物是最主要的呈味物质,并且随着炒籽温度的升高,吡嗪类化合物占比呈现逐渐增加趋势,醛类化合物占比呈现逐渐降低趋势;在入炒水分4.09%和7.12%、炒籽温度145～175℃条件下,风味物质总量分别为15.7～43.2 mg/kg和11.5～39.8 mg/kg。综上,选择165℃的炒籽温度,可得到具有较好风味品质的小榨花生油。     

焙炒处理对不同植物油品质特性的影响北大核心CSCD

为了研究焙炒对植物油品质的影响,以油菜籽、亚麻籽、花生、葵花籽和芝麻为原料,经焙炒处理后采用液压压榨法制油(热榨油),分析植物油的理化指标(酸值、过氧化值、水分及挥发物、色泽)、主体组分(脂肪酸组成及含量、甘三酯组成及含量、挥发性组分)和总酚含量,并与未焙炒处理直接压榨制取的油(冷榨油)作对比。结果表明:热榨油酸值和过氧化值显著高于冷榨油(p<0.05),其中,热榨亚麻籽油酸值(KOH)最高(0.96 mg/g),热榨菜籽油过氧化值最高(1.02 mmol/kg);冷榨油水分及挥发物含量显著高于热榨油(p<0.05),其中冷榨花生油水分及挥发物含量最高(0.16%);热榨油的色泽较冷榨油深,其中热榨菜籽油的色泽最深(R1.1,Y31);焙炒对植物油脂肪酸和甘三酯组成及含量无显著影响(p>0.05);热榨油中醇类、醛类和酸类等挥发性组分较少,但杂环类物质较多;热榨菜籽油、亚麻籽油、花生油、葵花籽油和芝麻油总酚含量分别是其冷榨油的1.38、1.57、1.51、1.80倍和1.27倍。因此,焙炒对植物油品质影响较大,应根据生产需要选择合适的预处理方式。     

加工方式对大豆油中挥发性物质的影响

为探究加工方式对大豆油风味物质的影响,采用电子鼻与顶空固相微萃取-气相色谱-质谱联用相结合的方法分析浸提、热榨和冷榨3种方式加工的大豆油挥发性物质的差异。结果表明：在3种大豆油样品中共检出86种挥发性物质,其中浸提油53种,热榨油54种,冷榨油45种,主要包括醛类、醇类、酮类、酸类、酯类、萜烯类、杂环类（呋喃和吡嗪）以及烃类等化合物。在3种大豆油中检出相同的挥发性物质有24种。主成分分析和层次聚类分析结果表明加工方式对大豆油风味的影响较大。采用气味活度值（OAV）判定3种大豆油样品的关键风味物质,浸提油中检出关键风味物质15种,以3-壬烯-2-酮等物质为主,使浸提油具有浆果风味。热榨油中检出关键风味物质16种,其中2,5-二甲基吡嗪等杂环类物质使热榨油具有独特的烘焙风味。冷榨油中检出12种关键风味物质,以（E,E）-2,4-庚二烯醛等醛类物质为主,使冷榨油具有天然油脂风味。偏最小二乘回归分析表明电子鼻与气相色谱-质谱联用的检测结果间存在较好相关性。     

压榨和精炼核桃油挥发性成分的比较及其电子鼻判别

利用气相色谱-质谱联用(GC-MS)结合电子鼻技术,从挥发性成分和整体气味两方面对冷榨、热榨和精炼核桃油进行了差异分析。结果表明:冷榨、热榨和精炼核桃油共有的挥发性成分中醛酮类占较大比例,相对含量分别为18.83%、21.86%和50.13%,其中又以己醛的相对含量最高;冷榨油的特异性挥发成分是酯类和萜类化合物,可能是核桃仁/油原始风味的基础物质;热榨油中吡嗪类等杂环类化合物相对含量最高,达42.95%;同时糠醛的生成表明Maillard反应的存在及戊糖组分对热榨油风味的重要影响;精炼油中挥发性成分以脂肪酸氧化产物醛酮类物质为主,核桃仁/油原始风味成分和Maillard风味成分在精炼后损失严重;基于挥发性成分的主成分分析和电子鼻检测结果一致,均能对3种核桃油进行有效区分。因此,可利用GC-MS结合电子鼻,从特征挥发性成分和整体气味两个方面对核桃油进行工艺控制和品质评价。     

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.     

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.     

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.     

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.