固相微萃取与气质联用法分析鱼肉中气味成分

本文采用固相微萃取技术萃取鱼肉中的挥发性成分，并通过气相色谱质谱联用法来分析、鉴定鱼肉中的气味成分。经NIST质谱数据库检索和文献对照，共检出25种成分，确定20种成分，其中以羰基化合物和醇类为主。相对含量比较多的有1-辛烯-3醇、2，5-辛二酮、2，4-己二烯醇、2-壬烯醇等。     

复合乳酸菌发酵六齿金线鱼肉的挥发性风味成分探究

为改善传统腌制六齿金线鱼肉风味,通过在腌制鱼上接种复合乳酸菌快速发酵,并采用顶空固相微萃取-气相色谱-质谱(HS-SPME-GC-MS)联用法对发酵鱼肉的风味成分进行分离鉴定,比较分析复合乳酸菌发酵鱼肉和传统高盐腌制鱼肉的风味成分变化。结果表明:复合乳酸菌发酵鱼肉中检测出92种挥发性成分,其中,醛类18种、醇类15种、酮类8种、酯类7种、酸类2种、烃类34种、其他8种;传统高盐腌制鱼肉中检测出62种挥发性成分,其中,醛类12种、醇类9种、酮类4种、酯类3种、酸类3种、烃类25种、其他6种;进一步分析发现,构成两种腌制鱼肉独特风味的主要成分是醛、醇、酮类化合物,复合乳酸菌发酵鱼肉的醛、醇、酮类化合物种类总量达41种,较传统高盐腌制鱼肉增加16种。其中,(E)-2-己烯醛、(E)-2-辛烯醛、(Z)-4-癸烯醛、(E,E)-2,4-癸二烯醛、十四醛、庚醇、2-乙基-1-己醇、十二醇、6-甲基-2-庚酮、3,5-壬二烯-2-壬酮、D-柠檬烯、长叶烯是发酵鱼肉特有风味成分,丰富了发酵鱼肉风味,改善了鱼肉品质。所以,复合乳酸菌发酵六齿金线鱼,不仅能改善传统高盐腌制鱼肉风味,而且未检出胺类等致癌物质,保证了产品品质和安全性。     

固相微萃取-气-质联用法测定大菱鲆鱼肉挥发性成分条件的优化

采用顶空固相微萃取-气相色谱-质谱联用法分析大菱鲆鱼肉中的挥发性成分,对影响萃取效率的关键因素进行优化,分析各因素对不同相对分子质量化合物萃取效果的影响。结果表明:在3 g鱼肉中加入6 mL饱和氯化钠溶液(0.36 g/mL),用50/30μm DVB/CAR/PDMS的萃取头于50℃下萃取40 min,能够达到较好的萃取效率。在最佳萃取条件下提取大菱鲆鱼肉的挥发性成分,结合GC-MS共鉴定出38种主要挥发性物质,包括醛类、醇类、烃类、酮类和胺类化合物,其中醛类和醇类化合物的相对含量较高,分别为36.98%和33.15%,为新鲜大菱鲆鱼肉的主要挥发性成分。     

固相微萃取-气相色谱-质谱法分析带鱼肉的挥发性成分

采用固相微萃取-气相色谱-质谱联用技术分析带鱼肉的挥发性成分,以鱼肉中8种主要挥发性物质为参照对象,对影响萃取效率的关键因素进行了优化。结果表明:在2g鱼肉中加入6mL饱和氯化钠溶液(0.36g/mL),用50/30μm DVB/CAR/PDMS的萃取头于50℃下萃取50min能够达到较好的萃取效果;在此条件下提取带鱼肉的挥发性成分,共鉴定出40种化合物,其中醛类、醇类、芳香族和烯烃类化合物的相对含量较高,分别为45.11%、17.47%、14.49%和13.99%,为带鱼肉的主要挥发性成分。     

ω-3 LCPUFAs模拟热加工鱼肉脂肪氧化形成风味物质的研究

为探索热加工过程中鱼肉脂肪氧化形成风味物质的过程,以鱼肉典型脂肪酸——ω-3 LCPUFAs(EPA、DPA、DHA)为代表,分别采用脂肪氧化酶处理和加热处理,采用固相微萃取-气相色谱-质谱联用技术分析。结果显示:经两种方式处理,3种脂肪酸共产生8大类107种风味特性各不相同的成分,其中具有土腥味和鱼腥味等鱼肉特征风味成分包括2-辛酮、2-壬酮、3-辛烯-2-酮、反-2-戊醇、3-辛醇、1-辛烯-3-醇、十二醇。产物中含量最大的成分是芳香族化合物,其它产物含量大致顺序为醛、酮、醇或烷烃、呋喃或酯,脂肪氧化型产物(醛、酮、醇、呋喃)占总含量的6.0%～63.7%。3种脂肪酸产物总含量顺序为EPADHADPA,推测3种脂肪酸稳定性顺序为DPADHAEPA。两种处理方式相比,加热处理形成比例更高的脂肪氧化型产物,而低温脂肪氧化酶处理主要形成芳香族化合物。提示受热作用更利于鱼肉形成风味良好的产物。     

白姑鱼和小黄鱼肉中挥发性风味物质的鉴定

采用新型固相萃取整体捕集剂（Mono-Trap）结合气相色谱-质谱-嗅闻技术对白姑鱼和小黄鱼肉的挥发性风味物质进行鉴定,分别得到42 种和49 种挥发性成分。进一步通过芳香萃取物稀释分析法分别从白姑鱼和小黄鱼肉挥发物中筛选出12 种和6 种挥发物,其中9 种挥发物经质谱和线性保留指数鉴定。进一步结合校准频率（modified frequency,MF）法,各筛选出2 种鱼肉中排名前10的气味物质。白姑鱼中香气稀释（flavor dilution,FD）因子最高为40的化合物为三甲胺、2-辛烯-1-醇、壬醛及金属味未知化合物。结合MF排名,得到三甲胺和2-辛烯-1-醇对白姑鱼贡献较大;小黄鱼中FD因子最高为40的化合物为己醛和2-辛烯-1-醇,但结合MF排名,对其气味贡献较大的是三甲胺和未知烧烤味化合物。6-甲基-5-庚烯-2-酮为2 种鱼中均鉴定出的一种带金属味或血腥味成分,根据MF排名,该化合物对白姑鱼影响更大。2,3-戊二酮、1-戊烯-3-醇为小黄鱼中MF较靠前的物质,结合三甲胺和未知烧烤味化合物以及白姑鱼中未鉴定到的二甲基二硫醚,这些挥发物可能是造成其与白姑鱼气味感知差异的原因。     

加热温度对花鲈鱼肉挥发性成分的影响

以花鲈鱼为研究对象,通过电子鼻和固相微萃取-气相色谱-质谱对不同温度条件下花鲈鱼肉挥发性风味成分进行鉴定,分析经过不同温度处理的花鲈鱼肉挥发性物质的种类和相对含量发生的变化,探索出花鲈鱼肉挥发性成分与加热温度的关系。结果表明:电子鼻可以较好地区分出不同温度条件下的花鲈鱼肉。主成分分析显示不同温度条件下的花鲈鱼肉气味成分有明显的差异,45℃和60℃的花鲈鱼肉的气味成分差异最小。通过气相色谱-质谱检测分析,在35、45、60、80℃和95℃的花鲈鱼肉中分别确定出25、40、52、56种和59种挥发性成分;花鲈鱼肉中所含挥发性成分的种类随着检测温度的升高而增多,醛类、酮类、醇类、烃类和芳香族类化合物的相对含量随着温度的升高发生明显变化;对花鲈鱼肉的风味形成有重要贡献的挥发性物质为己醛、壬醛、庚醛、癸醛、十一醛、2-辛烯醛、2,4-癸二烯醛、庚醇、1-辛烯-3-醇、二甲苯等化合物。     

不同温度条件下草鱼肉挥发性成分的检测

采用固相微萃取-气相色谱-质谱分析不同温度条件下草鱼背肉挥发性风味成分。固相微萃取-气相色谱操作条件：采用65 μm PDMS/DVB萃取头,萃取时间40 min;色谱条件采用程序升温：柱初温40 ℃,保持2 min,以4 ℃/min升至160 ℃,而后以10 ℃/min升至250 ℃,保持5 min。经气相色谱-质谱分析检测,草鱼背肉在30、45、60、80、95 ℃分别确定出23、43、52、68、74 种挥发性成分;随着温度的升高,草鱼背肉挥发性成分的种类也随之增多,醇类、醛酮类、烃类及芳香族等化合物的相对含量有明显变化;80 ℃与95 ℃检测到的挥发性成分大部分差异不显著,可以认为代表熟鱼肉的风味特征。挥发性成分中的1-己醇、1-辛烯-3-醇、己醛、2,3-辛二酮及其他饱和醛通常被认为对水产品风味有较大影响,当温度变化时,含量变化也较大。     

超高压处理对鲈鱼挥发性成分的影响

目的:研究不同超高压处理条件下鲈鱼挥发性成分的差异。方法:采用固相微萃取-气质联用技术分析不同超高压处理条件对新鲜鲈鱼挥发性成分的影响,用主成分分析法对其挥发性物质组成进行分析。结果:在对照组、100 MPa、200 MPa和300 MPa处理的鱼肉中分别检测出15,18,17及15种主要的挥发性物质,包括醛类、酮类、醇类和烃类化合物。通过主成分分析得到不同超高压处理条件下鲈鱼鱼肉特有的挥发性物质组合,其中100 MPa处理组鱼肉的主要挥发性成分是壬醛、苯乙酮、(E)-2-戊烯-1-醇、1-辛烯-3-醇和2,4-二叔丁基苯酚,300 MPa处理组的主要挥发性成分为(Z)-2-戊烯-1-醇、长叶烯和二乙基二硫代氨基甲酯,对照组的主要挥发性成分为(Z)-2-戊烯-1-醇、1-庚醇、二乙基二硫代氨基甲酯。这些挥发性物质的组合,形成了各自的风味特征,决定了不同超高压处理条件下鲈鱼鱼肉风味的差异。     

植物乳杆菌发酵草鱼肉挥发性成分的变化规律

研究植物乳杆菌发酵草鱼的过程中挥发性成分变化规律。利用电子鼻、顶空固相微萃取和气相色谱-质谱联用技术对草鱼发酵不同时间段的挥发性成分进行分析。结果表明,电子鼻能够较好地区分发酵不同阶段的鱼肉样品的风味,各阶段的成分有显著差异,进一步采用气相色谱-质谱法对不同时间的草鱼发酵样品中的挥发性成分进行分析,鉴定出54 种挥发性物质,在发酵过程中,土腥味的己醛、庚醛等醛类物质逐渐减少;蘑菇香味的1-辛烯-3-醇含量逐渐增多,发酵后期产生了有薄荷香味的丙酮,以及有奶油香味的乙偶姻等增香成分,这和感官评定的结果一致。     

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.     

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.     

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.     

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.     

Analysis of benzo[a]pyrene in spiked fatty foods by second derivative synchronous spectrofluorimetry after microwave-assisted treatment of samples

A simple, rapid and inexpensive method has been developed for the determination of benzo[a     

The development of reference materials for paralytic shellfish poisoning toxins in lyophilized mussel. II: Certification study

This paper describes the second part of a project undertaken to develop certified mussel reference materials for paralytic shellfish poisoning toxins. In the first part two interlaboratory studies were undertaken to investigate the performance of the analytical methodology for several PSP toxins, in particular saxitoxin and decarbamoyl-saxitoxin in lyophilized mussels, and to set criteria for the acceptance of results to be applied during the certification exercise. Fifteen laboratories participated in this certification study and were asked to measure saxitoxin and decarbamoyl-saxitoxin in rehydrated lyophilized mussel material and in a saxitoxin-enriched mussel material. The participants were allowed to use a method of their choice but with an extraction procedure to be strictly followed. The study included extra experiments to verify the detection limits for both saxitoxin and decarbamoyl-saxitoxin. Most participants (13 of 15) were able to meet all the criteria set for the certification study. Results for saxitoxin.2HCl yielded a certified mass fraction of <0.07 mg/kg in the rehydrated lyophilized mussels. Results obtained for decarbamoyl-saxitoxin.2HCl yielded a certified mass fraction of 1.59+/-0.20 mg/kg. The results for saxitoxin.2HCl in enriched blank mussel yielded a certified mass fraction of 0.48 +/- 0.06 mg/kg. These certified reference materials for paralytic shellfish poisoning toxins in lyophilized mussel material are the first available for laboratories to test their method for accuracy and performance.     

Announcing a new international peer-reviewed journal:Food Science and Human Wellness now accepting manuscript submission in English

<正>We are pleased to announce the launch of a new international peer-reviewed journal-Food Science and Human Wellness,ISSN 2213-4530,which is an open access journal,produced and hosted by Elsevier B.V.on behalf of Beijing Academy of Food Sciences.Food Science and Human Wellness is an international peer-reviewed English journal that provides a forum for the dissemination of the