沙棘多糖分离纯化及抗氧化活性

分离纯化沙棘多糖（sea buckthorn (Hippophae rhamnoides) polysaccharides,SBP）,并对其单糖组分、结构表征及体外抗氧化活性进行分析。通过水提醇沉、Sevag法除蛋白得到沙棘粗多糖,利用DEAE-52纤维素柱对其进行分离纯化得到中性多糖SBP-I和酸性多糖SBP-II、SBP-III 3 种组分。单糖组分结果表明,SBP-I由物质的量比为1.18∶1∶2.20∶32.17∶1.45的阿拉伯糖、木糖、甘露糖、葡萄糖及半乳糖组成;SBP-II由物质的量比为1∶0.28∶1.02∶0.20的木糖、甘露糖、葡萄糖及半乳糖组成;SBP-III由物质的量比为1∶2.15∶0.28的木糖、葡萄糖及半乳糖组成;红外光谱测定表明,3 种组分均具有多糖的特征吸收峰;体外抗氧化实验结果表明,粗多糖及3 种纯化多糖组分均具有较好的抗氧化性且随样品质量浓度的增加抗氧化活性也随之升高,抗氧化能力大小顺序为：VC＞SBP-III＞SBP-II＞SBP-I＞粗多糖。     

香加皮多糖的分离纯化、单糖组成及其抗氧化活性研究

目的：分离纯化香加皮多糖(Cortex Periplocae Polysaccharides,CPP)，并对其进行单糖组成和抗氧化活性研究，以期为香加皮多糖在食品领域的开发和应用提供参考。方法：通过水提醇沉和Sevag法除蛋白得到香加皮粗多糖，经DEAE-52纤维素柱分离纯化得到4种多糖组分CPP0、CPP1、CPP2和CPP3，并对其进行化学成分检测、分子量测定、单糖组成分析、红外光谱和抗氧化活性分析。结果：4种多糖的糖含量分别为82.20%、77.13%、75.23%和72.85%，且都含有糖醛酸；相对分子量分别为685、477、411和572 kDa。4种多糖均为甘露糖、鼠李糖、半乳糖醛酸、葡萄糖、半乳糖和阿拉伯糖按照不同摩尔比组成的杂多糖。红外光谱表明4种多糖含有β-糖苷键且具有呋喃环。抗氧化实验结果显示4种多糖均具有一定的抗氧化性，总体抗氧化能力顺序为：CPP0>CPP3>CPP1>CPP2。结论：从香加皮中提取得到的4种酸性多糖，糖含量高、相对分子量大且均具有抗氧化活性，其中CPP0组分抗氧化活性最好。     

化橘红多糖的提取纯化及抗氧化活性研究

对化橘红粗多糖及其纯化组分的抗氧化活性进行研究。化橘红粉末经热水提取、乙醇沉淀、sevage法脱蛋白、透析得到粗多糖,粗多糖经DEAE-52纤维素阴离子交换层析柱分离,得到2个纯化组份ECP1和ECP2。采用化学法分别测定了粗多糖及其纯化组分的体外清除自由基(DPPH.,.OH,ABTS.+)能力、还原能力。粗多糖的多糖含量为74.29%,经DEAE-52纯化的组分ECP1和ECP2的多糖含量分别为83.39%和85.77%。结果表明粗多糖及其两个纯化组分均具有较好的抗氧化清除自由基的能力,并且抗氧化能力与多糖浓度之间存在良好的相关性。其中ECP2的抗氧化清除自由基能力强于ECP和ECP1,但是低于对照VC。     

安徽产地桑叶多糖分离纯化、结构鉴定与抗氧化活性研究

利用水提醇沉法提取桑叶多糖,采用DEAE-52-纤维素阴离子交换树脂和Sephadex G-100葡聚糖凝胶柱层析分离纯化桑叶多糖(MLP),得到2种纯化多糖MLP-1和MLP-2,并对其结构和抗氧化活性进行研究。结果表明,MLP-1分子量为9.31×104 Da,单糖组成包括甘露糖、鼠李糖、葡萄糖、半乳糖、木糖和阿拉伯糖,其摩尔比为0.26∶0.36∶1.00∶0.41∶1.34∶1.02。MLP-2的分子量为2.22×106 Da,由甘露糖、鼠李糖、葡萄糖、半乳糖和阿拉伯糖组成,其摩尔比为0.18∶1.22∶1.00∶0.14∶1.72。红外光谱分析表明,MLPs各组分具有典型的糖特征吸收峰。超氧阴离子(O2·-)、H2O2自由基清除能力和还原力测定体外抗氧化活性研究表明,MLP-1和MLP-2均具有一定抗氧化能力,强弱顺序依次为VC> MLP-1> MLP-2。     

绿豆多糖制备及抗氧化特性研究

采用响应面法对绿豆仁中多糖碱液提取工艺进行优化,在此基础上进一步开展分离纯化及抗氧化特性研究。结果表明,碱法提取绿豆多糖(Alkali extraction mung bean polysaccharides,AEMP)最佳工艺参数为碱液浓度0.02 mol/L,液料比20∶1 mL/g,提取温度50℃,提取时间3 h,最终AEMP得率9.70 mg GE/g DW。进一步采用DEAE-2纤维柱和SephadexG-100凝胶柱分离纯化绿豆多糖,得到一个中性组分AEMP-1和一个酸性组分AEMP-2。抗氧化特性结果表明AEMP及其纯化组分对羟自由基和DPPH自由基均有良好清除效果,AEMP-2抗氧化活性最强,对羟自由基和DPPH自由基半数抑制浓度IC50值分别为4.71 mg/mL和1.03×10-1mg/mL。表明绿豆多糖具有良好的抗氧化特性。     

香菇多糖纯化前后结构和生物活性的比较

为了比较香菇多糖纯化前后的结构特性和生物活性。分别对香菇粗多糖样品(命名为L0)及其纯化后的3个多糖组分(依次命名L1、L2和L3)进行结构特性(紫外光谱,红外光谱,扫描电镜,粘均相对分子质量,刚果红络合物)和生物活性(抗氧化活性和抑菌活性)的测定。紫外光谱结果显示纯化后多糖组分基本不含有核酸和蛋白质;红外光谱结果表明多糖纯化前后均有显著的多糖特征吸收峰和β-糖苷键,其中L1与L0的结构更相似,吸收峰更明显;扫描电镜结果显示,纯化前后组分有一定的差异,其中L2和L3表面结构呈现出碎屑状堆积,而L1呈现出有一定凸起和褶皱的块状;刚果红络合物结果表明,L0和L1中含有三螺旋结构;L0、L1、L2和L3的粘均相对分子质量分别为2.19×105、8.34×104、4.40×104、3.66×104。抗氧化实验表明,L0具有更好的抗氧化效果;对金黄色葡萄球菌抑菌圈的测定发现L1具有更好的抑菌效果。实验结果表明,纯化前后香菇多糖在结构和活性上均有一定的差异,为活性多糖组分的制备和利用提供了一定的依据。     

黄花倒水莲多糖的纯化、表征与体外抗氧化活性研究

提取纯化黄花倒水莲多糖(polysaccharide of Polygala fallax Hemsl.,PFP),对其结构进行表征,并测定其体外抗氧化活性。采用水提醇沉法提取PFP,运用Sevag法除蛋白、活性炭脱色以及G-75葡聚糖凝胶柱层析对其进行纯化分离获得不同的多糖组分。分别用红外光谱(infrared spectrum,IR)、凝胶渗透色谱(gel permeation chromatography,GPC)与1-苯基-3-甲基-5-吡唑啉酮(1-phenyl-3-methyl-5-pyrazalone,PMP)柱前衍生高效液相色谱(high performance liquid chromatography,HPLC)法对PFP组分进行表征分析。最后测定PFP组分对DPPH自由基、羟基自由基、超氧阴离子自由基和ABTS+自由基的清除率来评价其体外抗氧化活性。经分离纯化得到两种PFP组分(PFP1与PFP2)。其中PFP1的分子量为20 794 Da,多分散指数为1.32,红外光谱中呈现多糖的典型特征吸收峰,PFP1是由甘露糖、半乳糖醛酸、鼠李糖、葡萄糖、半乳糖、阿拉伯糖与一种未知单糖组成的一种杂多糖,且摩尔比为0.09∶1∶0.48∶0.64∶0.71∶0.35。PFP1对4种自由基均有清除能力,且在一定浓度范围内呈正相关。因此PFP在体外具有抗氧化活性,为今后进行更深入的研究与开发利用提供依据。     

榨前分离苹果皮多糖的鉴定及抗氧化活性研究

以榨前分离苹果皮为原料,采用超声波辅助法提取多糖,通过改变洗脱液的极性对多糖进行分离纯化,并对各组分的抗氧化活性进行分析。结果表明:多糖样品经过DE-52纤维素柱梯度洗脱得到三个含量较大的洗脱峰,分别为水、0.3mol/L NaCl和0.9mol/L NaCl洗脱组分。采用Sephadex G-200凝胶柱对洗脱组分进一步纯化,得到APPSH2O、APPS-0.3mol/L和APPS-0.9mol/L三种不同组分的多糖纯品。抗氧化实验表明:三种不同组分多糖均有一定的还原力、清除·OH、DPPH·,O-2·的能力,但其抗氧化能力均小于粗多糖和V C。     

冬枣多糖的分离纯化及抗氧化活性研究

目的：分离纯化冬枣多糖,并研究其组分、结构特征和抗氧化活性。方法：采用水提醇沉、脱蛋白脱色、DEAE-52纤维素柱和Sephadex G-100凝胶色谱柱分离纯化冬枣多糖;利用Sephadex G-100凝胶色谱柱进行纯度鉴定和分子质量的测定;通过紫外光谱、红外光谱、气相色谱法进行了初步结构分析;采用邻二氮菲法和1,1-二苯基-2-三硝基苯肼（1,1-diphenyl-2-picrylhydrazyl,DPPH）体系对纯化多糖进行抗氧化活性的研究。结果：冬枣多糖经DEAE-52分离和Sephadex G-100纯化得到2 个组分DPA和DPB,经Sephadex G-100鉴定均为均一组分,DPA和DPB分子质量分别为1.04×104、3.02×105 D,不含蛋白质和核酸,为吡喃型糖苷环骨架,DPA的单糖组成为阿拉伯糖、甘露糖、葡萄糖、半乳糖,其物质的量比为6.66∶1.00∶6.75∶2.09;DPB的单糖组成为鼠李糖、阿拉伯糖、甘露糖、葡萄糖、半乳糖,其物质的量比为4.33∶10.90∶1.00∶3.25∶4.78;DPA和DPB均具有一定的抗氧化活性,随着多糖质量浓度的增加,其抗氧化活性增强,在质量浓度为8 mg/mL时对羟自由基清除率分别为28.52%、78.79%,在质量浓度为0.4 mg/mL时对DPPH自由基清除率分别为9.97%、24.54%。结论：DPA和DPB均具有一定的抗氧化活性。     

铁观音茶末多糖的分离纯化和抗氧化活性

为实现废弃茶叶资源的再利用以及探究铁观音茶叶末活性多糖的抗氧化活性,以水提醇沉法提取铁观音茶末粗多糖,然后通过DEAE-52纤维素和Sephadex-100葡聚糖凝胶分级两次纯化,并进行纯度鉴定、红外光谱分析、分子量的测定以及体外抗氧化活性的测定等。结果表明,90%的乙醇终浓度得率最高,为1.97%;两次分级纯化后得到TPS-1A和TPS-4C,纯度分别为96.2%、95.1%;红外光谱图谱表明两种多糖均为β-型糖苷键多糖;分子量分别为15792、21722 Da;两种多糖组分抗氧化活性均随着组分浓度的增加而逐渐增强,当质量浓度为1.2 mg/mL时TPS-1A和TPS-4C,对DPPH自由基的清除率分别为95.41%、97.71%,羟自由基清除率分别为93.39%、94.21%,总还原力测得吸光度值为0.699、0.712。由此说明铁观音茶末多糖具有较强的抗氧化活性,且TPS-4C强于TPS-1A。     

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.     

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.     

Influence des ions sur le pouvoir hydratant de l'ure e: e tude sur peau de porc ex vivo

This study deals with the influence of ions (NaCl and MgSO4) in a W/O emulsion containing 10% urea. Moisturization kinetics are assessed by corneometry on pig skin ex vivo. The formula's influence on urea penetration is measured by infrared spectrometry with an ATR device and the stripping method. Corneometry and spectroscopy were chosen to record simultaneously the hydratation levels and urea localization into superficial cell layers. Urea crystallization after evaporation of emulsions and aqueous solutions is described. Results show that urea does not hydrate nor penetrate when applied to the skin through an aqueous gel. In a W/O emulsion, sodium chloride increases the ability of urea to moisturize without improving penetration. In vitro urea crystallization is disturbed by sodium chloride or magnesium sulphate for solutions and emulsions. This stabilization by ions is correlated with good moisturization values. The stabilization of urea in the solute state provided by ions increases its water epidermal binding capacity without enhancing penetration.     

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.