甲壳素传统法与微波法制备壳聚糖的比较

针对甲壳素脱乙酰制备壳聚糖采用的两种方法——微波法与传统法,从反应时间、壳聚糖的得率和品质(脱乙酰度和粘均分子量)等方面进行了比较分析。结果表明,甲壳素传统法一次脱乙酰反应很难制备脱乙酰度大于78%高粘均分子量的壳聚糖;与传统方法相比,甲壳素微波法脱乙酰制备壳聚糖不仅大大减少了反应时间,同时还能避免高温长时间处理导致壳聚糖产品的分子量和粘度下降,从而提高壳聚糖的质量指标。     

利用黑曲霉菌丝体制备壳聚糖的研究

本试验以试验室发酵的黑曲霉菌丝体为原料,采用酸碱交替法从中提取甲壳素,然后将甲壳素脱乙酰转化为壳聚糖。运用碱煮法由甲壳素脱乙酰基制备壳聚糖时,在反应前采用盐酸对甲壳素进行预处理,并通过单因素试验和正交试验分析了反应时间、碱液浓度、温度等对壳聚糖脱乙酰度和产率的影响,得出了制备高脱乙酰度壳聚糖的最优条件为：NaOH浓度40%,反应温度110℃,反应时间6h。     

响应面法优化丰年虫卵壳脱乙酰度壳聚糖提取工艺

以丰年虫卵壳制备的甲壳素为原料,通过单因素试验和响应面设计法,确定丰年虫卵壳壳聚糖微波辅助提取技术的最佳工艺条件为微波时间33.4min、乙醇浸泡时间86min、碱液质量分数57.27%。按此工艺条件提取可获得脱乙酰度为84.12%的丰年虫壳聚糖。     

微波条件下南美白对虾壳聚糖的制备及其动力学分析

本文研究了微波辐射对南美白对虾甲壳素制备壳聚糖的影响。试验结果表明：采用微波加热（300W）制备壳聚糖时碱液浓度应低于50％,加热时间应低于15min,这样可以制备出不同脱乙酰度的壳聚糖。所制得壳聚糖具有标准壳聚糖红外光谱特征峰。反应动力学分析表明,壳聚糖脱乙酰反应为一级反应,反应速率常数为0．0704。     

壳聚糖制备方法比较及其性能研究

目的研究壳聚糖的制备方法。方法以甲壳素为原料,分别采用微波法和间歇碱液法制备壳聚糖,分析不同方法制备壳聚糖的粘均分子量、黏度、抗氧化性、吸湿保湿性能及表面形态的差异。结果微波法制备壳聚糖的最佳工艺条件为:氢氧化钠浓度为55%,料液比为1:15(g/mL),微波功率为400 W,时间20 min;间歇碱液法制备壳聚糖的最佳工艺条件为:氢氧化钠浓度为55%,料液比为1:20(g/mL),温度100℃,时间10 h,5 h更换碱液1次。2种方法相比,微波法反应时间短,碱液用量少,制备的壳聚糖粘均分子量和黏度较高,对羟基(·OH)自由基的清除效果好,吸湿性佳;间歇碱液法制备的壳聚糖脱乙酰度较高(88.95%),对1,1-二苯基2-三硝基苯肼(DPPH)自由基的清除效果较好,对原料的破碎化程度较高,但反应时间长,碱液用量多。结论从节能高效、绿色环保的角度考虑,微波法制备壳聚糖较理想。     

黑曲霉电解法制备甲壳素的研究

本试验以实验室发酵的黑曲霉菌丝体为原料,采用电解法从中提取甲壳素,再将甲壳素碱法脱乙酰转化为壳聚糖。通过单因素试验和正交试验分析了电解时间、电压、碱浓度及料液比对壳聚糖的脱乙酰度、得率、粘均分子量等指标的影响,以此间接反映电解法各因素对甲壳素产品的影响。黑曲霉电解法制备甲壳素的最优条件为:电解时间1.25h,NaOH浓度3%,电压8V,液料比12:1。试验证明,利用电解法从黑曲霉中提取甲壳素实践上是可行的。     

蝇蛆壳制备壳聚糖的工艺条件研究

本试验探索了蝇蛆壳制备壳聚糖的最佳工艺条件。以蝇蛆壳中甲壳素为原料,采用碱液法制备壳聚糖。通过单因素试验考察了碱液浓度、液料比、反应时间对壳聚糖脱乙酰度的影响;根据Box-Benhnken中心组合试验设计原理,采用三因素三水平响应面分析法优化脱乙酰基反应条件,依据回归分析确定工艺条件的主要影响因素,以壳聚糖脱乙酰度为响应值作响应面和等值线图。通过分析各个因素的显著性和交互作用,得出脱乙酰基反应的最佳工艺条件为:液料比57.49:1(V/m),碱液浓度50%,反应时间7.3 h。在此条件下所得壳聚糖的脱乙酰度理论值为83.18%,实测值为79.45%,并得到白色粉末状壳聚糖。     

超声协同CDA酶法制备龙虾壳聚糖

建立环境友好型的酶法制备高脱乙酰度壳聚糖的最佳工艺。以淡水小龙虾壳为原料,经EDTA法提取甲壳素,采用超声辅助CDA酶法制备壳聚糖;在预实验基础上,利用响应面法优化超声辅助CDA酶法制备壳聚糖工艺。结果表明:酶法制备高脱乙酰度壳聚糖的最佳条件为超声时间60 min,超声功率476 W,加酶量9.45%,酶解温度50℃,酶解时间3.5 h,在此条件下制备的壳聚糖脱乙酰度高达91.09%,黏度为95 m Pa·s,相对得率81.87%。该制备方法与单一超声法及传统碱法相比具有无任何环境污染、产品脱乙酰度高、产品性质稳定等优势。     

蚕蛹壳聚糖制备条件研究

对蚕蛹甲壳素脱乙酰制备壳聚糖的条件进行了研究。通过单因素实验考察了NaOH浓度、处理温度、时间以及甲壳素与NaOH溶液的配比对脱乙酰的影响,在此基础上经正交实验优化蚕蛹壳聚糖制备条件。结果表明,NaOH浓度对蚕蛹甲壳素脱乙酰的影响最大,其次为处理温度,处理时间和固液比影响较小,优化后的处理条件为:NaOH浓度50%、处理温度90℃、时间10h、固液比1:15。经验证实验,在该条件下,制得的蚕蛹壳聚糖脱乙酰度可达到74%。     

超声波预处理醇碱体系进行甲壳素脱乙酰工艺的研究

以自溶法脱蛋白、EDTA·Na2螯合脱钙制备的甲壳素为原料,采用超声波预处理醇碱体系进行甲壳素脱乙酰工艺的研究.以脱乙酰度(D.D.)为考察指标,依据单因素实验结果,采用L9(34)正交试验考察乙醇浓度(A)、氢氧化钠质量浓度(B)、反应时间(C)及超声波处理时间(D)对脱乙酰度(D.D.)的影响.实验结果表明脱乙酰工...     

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.     

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.     

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.     

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.     

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.