杨树桑黄胞外多糖的分子结构及抗氧化活性

对杨树桑黄胞外多糖(EPS)的相对分子质量、结构及抗氧化活性进行了研究。利用凝胶过滤法分离纯化EPS并测定多糖的相对分子质量,红外分析EPS结构的异头碳类型,GC/MS分析EPS的单糖组分,SEC/MALLS结合粘度法分析EPS的分子构象,利用·OH自由基和·DPPH自由基的清除率测定EPS的抗氧化活性。结果表明:杨树桑黄EPS分离纯化得到两个组分(Fr-Ⅰ和Fr-Ⅱ),其相对分子质量分别为627 500和55 000;红外分析可知,Fr-Ⅰ为含有α-和β-构型共存的吡喃型甘露糖苷酸性杂多糖,Fr-Ⅱ为含有α-吡喃型甘露糖苷酸性杂多糖;气质分析结果表明,Fr-Ⅰ和Fr-Ⅱ所含单糖组分为核糖、木糖、葡萄糖醛酸、半乳糖、葡萄糖、甘露糖和半乳糖醛酸;SEC/MALLS结果表明,EPS分散性很低,在水溶液中以球形构象存在,是一种高度紧密且具有分支结构的多糖聚集体。抗氧化测定表明,EPS质量浓度为10 mg/mL时,对·OH自由基的清除率为38.58%;质量浓度为5 mg/mL时,对·DPPH自由基的清除率高达59.17%,表现出良好的抗氧化活性。     

赤灵芝多糖分离纯化及体外抗氧化性研究

对赤灵芝多糖进行分离、纯化和体外抗氧化性研究。从赤灵芝中提取粗多糖,通过离子交换色谱、葡聚糖凝胶色谱对粗多糖进行分离纯化,采用凝胶渗透色谱、气相色谱进行分子量和单糖组成测试,对GLPa-2、GLPb-1、GLPc 3个级分进行了体外抗氧化性研究。结果表明,3个多糖级分主要由葡萄糖、阿拉伯糖、木糖、甘露糖组成,但单糖的摩尔比不同;GLPa-2、GLPb-1、GLPc的重均分子量分别为3.65×10~5,3.87×10~4,1.38×10~4 Da;各样品对自由基的清除率随浓度升高而增大,呈量效关系,分子量最大的GLPa-2抗氧化活性最佳,表明赤芝多糖的抗氧化活性与其组成相关。     

红曲霉菌胞外多糖的分离纯化、结构鉴定及抗氧化活性测定

目的:分离纯化红曲霉菌胞外多糖(Exopolysaccharide,EPS),测定各组分的抗氧化活性并对其结构进行初步表征。方法:红曲霉菌发酵液经乙醇沉淀获得胞外多糖,经精制除杂和DEAE-纤维素柱层析法分离纯化获得多糖组分,再分别用高效凝胶过滤色谱法(HPGFC)、柱前衍生PMP-HPLC法测定相对分子质量(Mw)和单糖组成,测定多糖组分清除DPPH和羟自由基的能力,评价其体外抗氧化活性。结果:EPS经分离得到三个组分EPS-1、EPS-2和EPS-3,相对分子质量分别为8673、143537、238742 Da。EPS-1、EPS-2均由甘露糖、鼠李糖、葡萄糖、半乳糖组成,摩尔比为1∶0.301∶2.052∶3.614和1∶2.475∶1.950∶1.532,EPS-3由甘露糖、鼠李糖、葡萄糖醛酸、葡萄糖、半乳糖组成,摩尔比为1∶0.401∶0.066∶0.307∶2.974。三个多糖组分对DPPH·和羟自由基均有清除能力,并与多糖浓度呈现正相关。当多糖浓度为1 mg/m L时,三个组分对DPPH清除率分别为16.4%、15.9%和14.8%;对清除羟自由基的清除率分别为40.4%、39.6%、63.8%。结论:红曲霉菌胞外多糖各组分的相对分子质量和单糖组成比例均有差异;对羟自由基、DPPH·的清除作用也存在差异,这种活性差异可能与各组分Mw及结构差异相关。     

灵芝孢子粉多糖的分离纯化、结构表征及免疫活性初探

采用水浴回流法提取灵芝孢子粉粗多糖,再依次使用DEAE Sepharose Fast Flow离子交换柱和Sepharose CL-6B凝胶色谱柱分离纯化得到2种多糖组分GLP1a和GLP1b,HPSEC法测得2种组分均呈单一峰,重均分子量分别为1.12×106和1.21×105。HPLC、红外光谱和核磁共振分析的结果表明,GLP1a和GLP1b主要由葡萄糖组成,主链都是以β-(1,6)糖苷键连接,GLP1b在部分1→6连接的葡萄糖的3位和4位有分支。MTT实验表明,2个多糖级分均具有一定的免疫活性,而且都存在明显的量效关系,GLP1b的免疫活性明显高于GLP1a。     

长白山区核桃青皮多糖分离纯化、鉴定及抗氧化活性分析

对核桃青皮多糖（polysaccharide of walnut green husks,JPs）进行分离纯化,并对得到的多糖进行单糖组成及体外抗氧化活性分析。利用超声波辅助提取JPs,经醇沉、除蛋白、透析等一系列处理后,先后利用DEAE-Sepharose和Sephadex?G-100柱色谱分离纯化JPs得到了两种均一多糖（JPs-1-1和JPs-2-1）;利用高效凝胶渗透色谱法测定两种均一多糖的分子质量分别为5.45×104、5.22×104?u;利用PMP-柱前衍生高效液相色谱法测定了两种均一多糖的单糖组成,均是由鼠李糖（Rha）、葡萄糖醛酸（GlcA）、半乳糖（Gal）、葡萄糖（Glc）、半乳糖醛酸（GalA）、木糖（Xyl）及阿拉伯糖（Ara）以不同的物质的量比组成。总抗氧化能力实验、1,1-二苯基-2-苦味基肼自由基和羟自由基清除实验结果表明JPs及分离纯化得到的两种均一多糖均具有较好的抗氧化活性,而且抗氧化活性的能力与样品的质量浓度呈正相关。     

金针菇锌多糖分离纯化及其结构特征

目的：以金针菇为原料,经过逐步分离纯化得到两个锌多糖组分并研究其理化性质、光谱学特性及结构特征。方法：金针菇锌多糖采用热水浸提的方法提取,经DEAE纤维素-52和Sephadex G-100凝胶色谱柱逐步分离纯化后通过火焰原子吸收法测定多糖中锌的含量,高效凝胶过滤色谱法鉴定组分的均一性,并测定其分子质量及单糖组成,采用紫外光谱、红外光谱和刚果红实验对锌多糖的结构特征进行相关研究。结果：通过分离纯化得到两个锌多糖组分CF1、CF2,纯品提取率分别为20.97%与12.25%,其中锌含量分别为191、429 μg/g,平均分子质量分别为890、1 244 kD。CF1组分由葡萄糖、半乳糖等6 种单糖组成;CF2组分主要由甘露糖、葡萄糖、岩藻糖等8 种单糖组成,且两个多糖组分均具有三股螺旋分子结构。     

生姜皮多糖的分离纯化及其结构组成分析

以生姜皮为原料,经热水浸提法,乙醇醇沉得到生姜皮粗多糖。再经DEAE-纤维素-52阴离子交换柱和Sephadex?G-100凝胶柱对所得粗多糖进行层析纯化,得到3种水溶性生姜皮多糖(GE-1、GE-2、GE-3)。利用高效液相色谱与蒸发光散射检测器联用测定各多糖组分的分子质量,利用柱前衍生高效液相色谱法分析各多糖组分的单糖组成,通过紫外光谱扫描、红外光谱扫描进一步分析各组分多糖结构。结果表明3种纯化多糖组分总糖含量分别为(98.06±0.15)%、(97.41±0.42)%、(97.89±0.22)%,分子质量分别为462、194 k D和376 k D。GE-1的单糖组成主要为甘露糖、葡萄糖、木糖,含有微量的半乳糖,其物质的量比为1.25∶6∶1;GE-2的单糖组成主要为甘露糖、葡萄糖和岩藻糖,其物质的量比为2.51∶9.25∶1;GE-3的单糖组成主要为甘露糖、核糖、半乳糖、阿拉伯糖,其物质的量比为17.39∶1∶1.89∶1.23。紫外光谱扫描结果显示3种多糖组分无明显的核酸和蛋白质吸收峰,红外光谱结果分析得出GE-1、GE-2和GE-3含有多糖类物质的特征吸收峰。     

烤烟上部鲜烟叶多糖的结构及保润性能

为研究烤烟上部烟叶多糖的结构和保润性能,用碱提法提取大田烤烟上部鲜烟叶多糖并精制后,分别采用HPLC法测定其单糖组分、FTIR法对其官能团进一步表征、SEC/MALLS/RI法测定多糖的分子量及构象,并研究了多糖的热裂解产物和保润性能。结果表明:(1)烟叶多糖为由42.91%葡萄糖醛酸、8.89%葡萄糖、32.31%甘露糖和15.89%阿拉伯糖组成的酸性杂多糖;为酸性β-吡喃糖。(2)烟叶多糖的重均分子量为6.587×104;多分散系数MW/Mn为1.557,均方根旋转半径与重均分子量双对数模型中的α值为0.279,表明多糖分子量分布较为均一,在水溶液中为球形并高度分支的构象。(3)烟叶多糖在600℃和900℃下的裂解产物分别有17和21种。(4)烟叶多糖具有一定的保润性,其效果低于丙二醇。     

洋甘菊多糖的分离纯化、性质结构及抗氧化活性分析

对热回流提取得到的洋甘菊多糖进行了分离纯化,并对得到的多糖的性质结构及抗氧化活性进行分析。经处理后的洋甘菊多糖先后利用DEAE-Sepharose和Sephadex G-100柱色谱分离纯化得到了2种均一多糖(MCP-1-1和MCP-2-1);经测定2种均一多糖总糖含量分别为82.23%、84.09%,糖醛酸含量分别为4.11%、5.38%,蛋白质含量分别为0.58%、1.05%,溶解度分别为98.36%、98.44%,分子质量分别为30902、7244 Da;单糖组成实验结果表明MCP-1-1是由鼠李糖(Rha)、葡萄糖醛酸(GlcA)、半乳糖(Gal)、葡萄糖(Glc)、木糖(Xyl)和阿拉伯糖(Ara)6种单糖组成,MCP-2-1是由GlcA、Gal、Glc、GalA、Xyl和Ara六种单糖组成,2种均一多糖均是不含三螺旋结构的酸性多糖,均含有吡喃环和β-糖苷键,MCP-1-1含有α-糖苷键;2种均一多糖具有良好的热稳定性。体外清除自由基试验结果显示MCP-1-1和MCP-2-1对DPPH自由基和·OH均有清除作用,而且清除能力与均一多糖的质量浓度正相关,MCP-2-1对2种自由基的清除能力明显高于MCP-1-1。研究结果表明,分离纯化得到的洋甘菊多糖可作为天然抗氧化剂,用于食品和化妆品中。     

野阳合多糖及其纯化组分对胆汁酸的结合能力

以野阳合为原料,采用水提醇沉法提取粗多糖,经离子交换柱层析和凝胶柱层析,得到4?种多糖组分YP1-1、YP2-1、YP2-2和YP3-1。采用高效液相色谱与蒸发光散射检测器联用,进行纯度鉴定及分子质量测定,利用柱前衍生高效液相色谱法分析各多糖组分的单糖组成,通过紫外光谱分析、傅里叶变换红外光谱进一步分析多糖结构,并通过模拟肠道内环境,测定多糖体外结合胆汁酸的能力。结果显示：野阳合粗多糖提取率为2.41%,总糖质量分数为96.35%;YP1-1、YP2-1、YP2-2和YP3-1均不含核酸和蛋白质,均为均一多糖,分子质量分别为3.52×106、3.08×106、1.93×106?Da和3.35×106?Da;主要为吡喃型糖苷环骨架,糖苷键以β-构型为主;YP1-1和YP3-1的单糖组成为甘露糖、鼠李糖、阿拉伯糖、葡萄糖和半乳糖,YP2-1和YP2-2的单糖组成为鼠李糖、阿拉伯糖、甘露糖、岩藻糖、葡萄糖和半乳糖。以上4?种多糖对胆汁酸有较强的结合能力,结合率均高于97%。     

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.     

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.     

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.     

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.     

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.