SPME/GC/MS法检测蒜薹中的挥发性成分

采用两种萃取头(50/30μm DVB/CAR/PDMS和100μm PDMS),利用顶空固相微萃取(SPME)-气质联用(GC/MS)分析四个大蒜主产地蒜薹中的挥发性成分。研究结果表明,100μm PDMS萃取头适合分析蒜薹中的挥发性成分,永年、惠民、商河、广饶四个产地的蒜薹共有的含硫化合物为二烯丙基二硫醚、甲基烯丙基三硫醚、二烯丙基三硫醚、二烯丙基硫醚、3-乙烯基-1,2-二硫杂-4-环己烯、1,3-二硫酸-2-硫酮、3,4-二甲基噻吩、1,3-二噻烷,其中二烯丙基二硫醚的含量最高。进一步分析表明,蒜薹不同部位的含硫化合物含量有一定差异,蒜薹含硫化合物含量:根部茎中部茎上部。本研究对于促进蒜薹加工利用,拓宽蒜薹产业链具有重要意义。     

SPME萃取头对大菱鲆鱼肉挥发性成分萃取效果分析

采用DVB/CAR/PDMS、PDMS/DVB和CAR/PDMS 3种萃取头进行顶空-固相微萃取(HS-SPME),提取新鲜大菱鲆鱼肉的挥发性成分,结合气质联用仪(GC-MS)进行分析鉴定,确定最佳的萃取头.结果表明,3种萃取头固相微萃取法共检测出81种挥发性成分,主要是醛、酮、醇、烯烃、烷烃和胺类化合物.使用DVB/CAR/PDMS、PDMS/DVB和CAR/PDMS萃取头分别检测出51、37和29种挥发性成分,其中使用DVB/CAR/PDMS萃取头检测出的挥发性物质总峰面积最大且种类最多.因此,DVB/CAR/PDMS萃取头较适合于大菱鲆鱼肉挥发性成分的提取.     

基于HS-SPME-GC-MS和PCA的不同萃取头对鸡肉香精香气成分萃取效果比较

为提高鸡肉香精香气成分分析的可靠性,比较不同纤维涂层萃取头萃取鸡肉香精香气成分的效果,采用顶空固相微萃取(headspace solid-phase micro-extraction,HS-SPME)结合气相色谱质谱联用仪(gas chromatography-mass spectrometry,GC-MS)检测技术对热反应鸡肉香精中的挥发性风味物质种类和组成进行提取分析,通过灵敏性及主成分分析(principal component analysis,PCA)法比较香气成分数量及含量建立香气品质评价模型,研究不同纤维涂层萃取头(75μm CAR/PDMS、65μm DVB/PDMS、85μm PA、50/30μm DVB/CAR/PDMS)与所萃取挥发性物质间的相关性。结果表明,75μm CAR/PDMS萃取头为萃取鸡肉香精样品挥发性物质的最优萃取头,萃取得到样品中共含有146种挥发性物质,包括醇类24种(16.44%)、醛类16种(10.96%)、吡嗪类12种(8.22%)、呋喃(酮)类13种(8.91%),含硫化合物10种(6.85%)等多种香气物质,检测到2-甲基-3-呋喃硫醇、2-甲基-3-戊烷硫醇、(E,E)-2,4-癸二烯醛、(E,E)-2,4-庚二烯醛及反式-2-壬烯醛等关键肉香味化合物。     

不同萃取头固相微萃取分析小米清酒挥发性成分的研究

采用PA、PDMS、PDMS/DVB、CAR/PDMS和DVB/CAR/PDMS 5种萃取头,并通过固相微萃取（SPME）与气质联用（GC-MS）对小米清酒中挥发性成分进行提取、鉴定,运用聚类热图分析不同SPME萃取头提取小米清酒挥发性成分差异。结果表明：5种萃取头SPME检测到小米清酒挥发性成分含有醇、酯、醛、碳氢化合物、含苯衍生物和其他化合物,使用不同萃取头进行固相微萃取能得到较为相似的主挥发性成分：1-戊醇、苯乙醇、正己酸乙酯、丁二酸二乙酯、辛酸乙酯、十六烷,DVB/CAR/PDMS萃取头检测效果最好。聚类热图显示,不同萃取头SPME提取到的挥发性成分效果差异较大,按萃取效果可分为PA萃取头、PDMS萃取头和复合萃取头（PDMS/DVB、CAR/PDMS和DVB/CAR/PDMS）三类,使用不同种萃取头SPME可较为全面地了解小米清酒挥发性成分构成。     

SPME和SDE结合GC-MS分析荷叶中挥发性成分

分别采用同时蒸馏萃取(SDE)法和固相微萃取(SPME)法并结合气相色谱-质谱联用(GC-MS)技术分析荷叶的挥发性风味成分。SPME法选用3种萃取头(CAR/PDMS、DVB/CAR/PDMS、PDMS/DVB)与SDE法对定性结果进行比较分析。结果表明,SDE法所鉴定出的挥发性成分有97种,相对含量为94.86%,且以烃类物质为主;SPME(CAR/PDMS)法所鉴定出的挥发性成分有29种,相对含量为89.26%,以醇类为主;SPME(DVB/CAR/PDMS)法所鉴定出的挥发性成分有62种,相对含量为85.97%,以醛类为主;SPME(PDMS/DVB)法所鉴定出的挥发性成分有59种,相对含量为86.96%,以醛类为主。由此可见,在荷叶挥发性成分分析中,四种方法萃取到的挥发性成份种类数从多到少依次是,SDE、SPME(DVB/CAR/PDMS)、SPME(PDMS/DVB)、SPME(CAR/PDMS)。     

红枣白兰地香气成分萃取中固相微萃取纤维的选择

目的:针对红枣白兰地香气成分气相色谱分析的要求,比较3种固相微萃取纤维萃取红枣白兰地香气成分的效果。方法:选取常用的CAR/DVB/PDMS、PDMS/DVB、PDMS 3种固相微萃取纤维进行红枣白兰地香气成分的富集和浓缩处理,然后用气-质联用法检测香气成分。通过对不同固相微萃取纤维萃取香气成分的数量、化学种类以及各类化合物累积峰面积标准化值的比较,评价供试固相微萃取纤维萃取红枣白兰地香气成分的效果。结果:红枣白兰地香气成分中,酯类、醛酮类、醇类、萜烯类是主要成分,酸类和烷烃类等是微量成分。不同固相微萃取纤维萃取的化合物存在明显差异,用DVB/CAR/PDMS萃取化合物118种,总含量较多;用PDMS萃取出119种,总含量较少;用PDMS/DVB仅萃取出88种,总含量最多。累积峰面积标准化值分析表明,DVB/CAR/PDMS萃取2类酯、醇类、萜烯类和醛酮类的效果最好,萃取其他成分效果居中;PDMS萃取酸类效果最好,而萃取甲乙酯、醇类、萜烯类和醛酮类效果最差;PDMS/DVB萃取乙酯类化合物的效果最好,萃取其他酯、酸类的效果最差。结论:在供试的3种固相微萃取纤维中,DVB/CAR/PDMS是萃取富集绝大多数红枣白兰地挥发性成分的最佳纤维。     

顶空固相微萃取-气相色谱-质谱联用法分析椪柑芳香水中挥发性成分

采用顶空固相微萃取-气相色谱-质谱联用法(HS-SPME-GC/MS)分离鉴定椪柑芳香水中的挥发性成分,研究固相微萃取头种类(PDMS/DVB 65μm,CAR/PDMS 75μm和DVB/CAR/PDMS 50/30μm)、吸附温度(30~50℃)、吸附时间(5~30 min)和样品体积(2~10 m L)对椪柑芳香水分离效果的影响。试验结果表明,采用DVB/CAR/PDMS固相微萃取头,样品体积8 m L,在温度40℃下吸附20 min,能达到最佳吸附效果。椪柑芳香水中主要的挥发性成分为:d-柠檬烯40.85%,乙醇17.17%,α-萜品醇15.61%,1-辛醇6.20%,β-月桂烯3.48%,3-甲基-1-丁醇3.01%,β-芳樟醇2.93%,樟脑2.88%,辛酸乙酯2.34%,α-蒎烯1.47%,占峰面积总和的95.94%。对顶空固相微萃取法进行重复性试验,10种挥发性成分的相对标准偏差(RSD)均低于7.0%,表明应用HS-SPMEGC/MS联用技术可对椪柑芳香水中挥发性成分进行快速、准确地分析。     

固相微萃取结合气质联用法分析一种奶味香精中的挥发性成分

应用固相微萃取法采用3种不同萃取纤维,结合气相色谱-质谱联用技术,剖析1种国外奶味香精样品中的挥发性成分。结果表明;以Carboxen/聚二甲基硅氧烷(carboxen/polydimethylsiloxane,CAR/PDMS)为萃取纤维的方法鉴定出39种挥发性成分,以聚二甲基硅氧烷/二乙烯基苯(polydimethylsiloxane/divinylbenzene,PDMS/DVB)为萃取纤维的方法鉴定出41种挥发性成分,以二乙烯基苯/Carboxen/聚二甲基硅氧烷(Divinylbenzene/Carboxen/Polydimethylsiloxane,CAR/PDMS/DVB)为萃取纤维的方法鉴定出40种挥发性成分;3种纤维萃取的分析结果相互补充,共鉴定出51种挥发性成分,其中酯类、醛酮类和内酯类化合物的含量最高,分别为26.12%、25.95%和15.16%,是该种奶味香精的主要组成成分。     

萃取头对甜面酱中挥发性成分分析的影响

采用顶空固相微萃取(HS-SPME)与气质联用(GC-MS)相结合对甜面酱中挥发性成分进行了初步分析,比较了4种不同涂层纤维的萃取头(30μm PDMS,65μm PDMS/DVB,75μm CAR/PDMS,50/30μm DVB/CAR/PDMS)对甜面酱挥发性成分的萃取效果和特点。结果表明:在相同实验条件下,50/30μm DVB/CAR/PDMS萃取头萃取到的色谱总峰面积和化合物种类最多,而75μm CAR/PDMS萃取头可以萃取到最多的香气成分。因此50/30μm DVB/CAR/PDMS萃取头最适合甜面酱挥发性成分的检测,同时可以用75μm CAR/PDMS萃取头来进行补充。     

HS-SPME结合GC-MS分析着色香葡萄中挥发性香气成分

利用顶空固相微萃取(HS-SPME)结合气相色谱-质谱联用(GC-MS)分析着色香葡萄中的挥发性香气成分。优化后的HS-SPME条件为:样品超声20 min,采用50/30μm PDMS/CAR/DVB萃取头,样品量8 mL,加盐3 g,40℃萃取40 min。此条件下GC-MS测出36种挥发性香气物质,主要为醇类、醛类、酯类和酮类化合物,其中决定其特征香气的物质包括己醛、2-己烯醛、(E)-2-己烯醇、芳樟醇、脱氢芳樟醇及α-萜品醇等。     

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