三氧化硫吡啶法酯化修饰海参岩藻聚糖硫酸酯的研究

该文对海参岩藻聚糖硫酸酯进行硫酸酯化修饰,并比较其酯化修饰前后的结构特征及抗氧化活性。分别采用三氧化硫-DMF法和三氧化硫-吡啶法制备硫酸酯化海参岩藻聚糖硫酸酯,以取代度为考察指标,研究了反应温度、酯化剂用量、反应时间对酯化效果的影响。结果表明,三氧化硫-DMF法的最佳修饰条件为:反应温度为40℃、酯化剂用量1. 2 g、反应时间为3 h,产品取代度可达15. 63;三氧化硫-吡啶法的最佳修饰条件为:反应温度为90℃、酯化剂用量1. 2 g、反应时间为3 h,产品取代度可达13. 31。抗氧化活性测定结果显示,硫酸酯化海参岩藻聚糖硫酸酯对DPPH·和·OH的清除率均显著提高,且三氧化硫-DMF法所得产品的抗氧化活性略高。     

抗消化性甘薯淀粉磷酸双酯制备工艺的优化

优化了三偏磷酸钠制备抗消化性甘薯淀粉磷酸双酯的工艺条件.采用响应面法Box-Behnken试验设计,分析了三偏磷酸钠、pH值、酯化温度以及酯化时间对甘薯淀粉磷酸双酯抗消化性能的影响.结果表明其最佳制备工艺为:三偏磷酸钠添加量3.6％(以甘薯淀粉计),pH 10.5,酯化反应温度50℃,酯化时间2.1h.在此条件下制备的甘薯淀粉磷酸双酯淀粉抗消化性为(58.73±0.04)％.经DSC和RVA扫描分析表明甘薯淀粉磷酸双酯仍具有与甘薯原淀粉相似的糊化特性.     

超声波辅助制备硫酸酯化苹果水溶性膳食纤维

采用超声波辅助氨基磺酸-N,N-二甲基甲酰胺(DMF)法制备硫酸酯化苹果水溶性膳食纤维(SSDF),以取代度为指标,通过单因素试验和正交试验设计研究硫酸酯化的最佳工艺条件。结果表明:最佳酯化工艺为,苹果水溶性膳食纤维(SDF)与氨基磺酸比例为1∶3(g∶g),SDF与DMF比例为1∶70(g∶m L),酯化反应起始温度60℃,超声波频率35 k Hz,酯化时间为1.5 h。在此条件下,SSDF取代度为0.97,红外光谱分析表明,硫酸酯化苹果SDF具有硫酸酯键的特征吸收峰。     

棉浆纤维磷酸酯化及其对打浆性能的影响

以棉浆纤维为原料,混合磷酸盐Na_2HPO_4-NaH_2PO_4为酯化剂,制备纤维素磷酸酯,研究酯化剂用量、反应温度、时间、pH值等对纤维润胀性能和取代度的影响。结果表明,制备纤维素磷酸酯的最佳条件为:酯化剂用量12%,反应温度120℃,反应时间1.5 h,pH值6.0、酯化剂配比1∶1,尿素用量4%,在此条件下,所制备的纤维素磷酸酯取代度为0.032,保水值从92.86%提高到134.12%;经磷酸酯化改性后的棉纤维表面发生了明显的局部塌陷与扭曲,破坏了束缚纤维细胞壁S_2层的初生壁及次生壁外层S1,显著改善了棉纤维的打浆性能。     

兰州百合多糖硫酸酯的制备及其抗氧化活性的测定

从兰州百合鳞茎中提取百合多糖（LPs）,用氯磺酸-吡啶法制备百合多糖硫酸酯（LPsS）。以百合多糖硫酸酯的硫含量为评价指标,依据响应面设计对反应温度、时间和酯化剂比例（氯磺酸∶吡啶）三个影响因素进行优化。得出最佳条件为反应时间1.5 h,反应温度43 ℃,氯磺酸与吡啶的体积比为1∶1。在此条件下,百合多糖硫酸酯中硫含量可达到10.98%。傅里叶红外光谱扫描显示在波数1 236 cm-1、813 cm-1处出现新吸收峰,说明百合多糖已被硫酸化。气质联用（GC-MS）分析百合多糖硫酸酯由甘露糖、葡萄糖、半乳糖3种单糖组成,其摩尔比为18:14:1。体外抗氧化活性试验结果表明百合多糖硫酸酯具有较好的清除DPPH自由基能力,并且抗氧化活性比未酯化前有所提高。     

硫酸酯化洋葱多糖的制备及其抗氧化活性的研究

以洋葱为原料,采用水提醇沉法制备洋葱多糖。用浓硫酸法对洋葱多糖进行硫酸酯法修饰,采用硫酸酯取代度为指标,对硫酸酯化反应的浓硫酸与正丁醇的体积比和反应时间进行优化,并对不同浓度的硫酸酯化洋葱多糖进行体外抗氧化实验。结果表明,制备硫酸酯化洋葱多糖的较佳工艺为浓硫酸和正丁醇体积比3∶1,反应时间20min和反应温度0℃,在此条件下多糖硫酸根取代度为0.51。同时,洋葱多糖硫酸酯化改性后可显著提高抗氧化性。     

平菇多糖硫酸酯制备工艺优化及抗氧化活性研究

以取代度为考察指标,研究了浓硫酸加入量、反应温度和反应时间等因素对平菇多糖硫酸化的影响;在单因素的基础上,通过L9(34)正交试验优化平菇多糖硫酸酯的制备工艺条件;采用FT-IR光谱仪对平菇多糖和平菇多糖硫酸酯进行结构鉴定,并通过测定还原力、DPPH自由基、超氧阴离子自由基和羟自由基清除率探索了平菇多糖硫酸酯的抗氧化活性。结果表明:平菇多糖硫酸酯制备优化工艺条件为平菇多糖1.00g,浓硫酸加入量10mL,反应温度60℃,反应时间90min,该条件下平菇多糖硫酸酯的取代度为0.48。FT-IR光谱分析证明硫酸基与平菇多糖形成了平菇多糖硫酸酯。平菇多糖硫酸酯对DPPH自由基、超氧阴离子自由基和羟基自由基的IC50(半数清除率)分别是0.816,1.882,1.611mg/mL;平菇多糖硫酸酯的还原力和对3种自由基的清除力均优于平菇多糖。说明平菇多糖经硫酸酯化后抗氧化能力增强。     

硫酸酯化丝素的最佳反应条件研究

采用浓硫酸-正丁醇法对丝素进行硫酸酯化,将硫酸基团接枝到丝素蛋白上.以硫酸酯化丝素质量和酯化丝素中硫酸基质量分数作为考察指标,采用L16(43)正交试验,探讨反应温度、反应时间、硫酸质量分数对硫酸酯化丝素产量和产物中硫酸基质量分数的影响.结果表明,各因素对硫酸酯化丝索的产量影响大小顺序是:温度>时间>硫酸质量分数,各因素对硫酸酯化丝素的硫酸基质量分数影响大小顺序是:硫酸质量分数>时间>温度;经进一步单因素实验,结果表明硫酸酯化丝素的反应最优化条件是硫酸质量分数为95%,反应温度为0℃,反应时间为4 h.     

纤维素硫酸酯水溶液性质的研究

本文以α-纤维素为原料,ClSO_3H-DMF为酯化剂,采用多相硫酸酯化法制备纤维素硫酸酯(Cellulose Sulfate,CS)。通过元素分析确定了CS的硫酸酯基取代度为2.0左右,13C-NMR测试表明,CS的硫酸酯基取代模式是C-6完全硫酸酯基取代和C-2部分或完全取代。CS在去离子水中具有良好的溶解性。根据相近取代度的CS系列产物的分子量与特性粘度的关系,通过Mark-Houwink拟合,确定了CS的糖链在稀溶液中呈现一种较为紧密的构象。在浓溶液中,CS的动力粘度随浓度增加而增大;外加盐能够促进CS聚电解质的电荷排斥作用,导致其动力粘度增加;添加二价盐Ca~(2+)可产生CS糖链的络合,显著提高CS的动力粘度;溶液pH环境为影响CS动力粘度的主要因素之一,在中性条件下动力粘度最大,酸性或碱性环境都会使其动力粘度下降。     

籽瓜多糖硫酸酯的制备工艺、化学结构及其抗氧化活性研究

从籽瓜中提取籽瓜多糖(SWP),用氯磺酸-吡啶法制备籽瓜多糖硫酸酯(SSWP)。以籽瓜多糖硫酸酯中硫含量为指标,依据响应面设计对影响硫酸酯中硫含量的反应时间、温度和酯化试剂的比例(氯磺酸∶吡啶)三个因素进行优化组合。得出最佳组合条件为:反应时间3.2h,温度61℃,酯化试剂的比例(氯磺酸∶吡啶)1∶1.3。在此条件下,籽瓜多糖硫酸酯中硫含量可达到11.98%。用红外光谱对籽瓜多糖进行了扫描,在1250.76、810.74cm-1处出现了新的吸收峰,说明硫酸化是成功的。用GC-MS分析其单糖组成,结果表明籽瓜多糖硫酸酯由鼠李糖、阿拉伯糖、木糖、甘露糖、葡萄糖、半乳糖六种单糖组成,摩尔比为4.29∶11.72∶8.66∶5.35∶13.62∶56.36。用体积排阻色谱测得籽瓜多糖硫酸酯的分子量,重均分子量Mn=2.717×105,数均分子量Mw=1.232×105。通过测定籽瓜多糖和籽瓜多糖硫酸酯对DPPH自由基、羟自由基的清除率,表明籽瓜多糖硫酸酯对羟基自由基及DPPH自由基的清除率比未酯化前显著提高。     

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.     

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.     

低温带皮菜籽粕微粉的不同粒级部分的功能特性

为研究低温带皮菜籽粕微粉的不同粒级部分的功能特性,以经低温脱脂的带皮菜籽粕为原料,经微粉碎后筛分成212~425μm、150~212μm和106~150μm的3个不同粒级的微粉样品,检测这些样品的吸水性、吸油性、乳化性和乳化稳定性、蛋白质体外消化率。结果表明:1 3个不同粒级的微粉样品之间的粗纤维含量存在显著差异,表明三者的结构组成成分有一定差异。23个微粉样品的乳化活性和乳化稳定性随粒度级别的减小而显著增加(P0.01)。33个微粉样品的蛋白质体外消化率随粒度级别的减小而显著增加(P0.01)。4不同粒级带皮菜籽粕微粉样品的吸水性与吸油性受其结构组成物质不同和粒度的双重影响,与粒度的相关性不明显。     

Microbiology of food taints

Fresh and processed foods are often spoilt by the presence of undesirable flavours and odours caused by microbial action. The aim of this paper is to review the current knowledge of microbiologically induced taints that occur in a wide range of foodstuffs, including meats, poultry, fish, crustaceans, milk, dairy products, fruits, vegetables, cereals and cereal products. Examples have been chosen where the compounds responsible for the taint have been identified and sufficient data obtained to demonstrate the involvement of microorganisms. However, in some cases the full identity of the causative organism may not have been elucidated. The types of microorganisms covered by this review include bacteria, fungi, yeasts, actinomycetes and cyanobacteria. Although cyanobacteria do not in general infect foods, their presence in aqueous systems and water supplies can lead to off-flavours in aquatic organisms and processed foodstuffs. Several examples of each of these processes are discussed. Wherever possible, the likely biosynthetic pathway used by the microorganism to produce the offending compound in a foodstuff is indicated.