无溶剂体系酶催化酯化反应合成共轭亚油酸油脂的研究

研究了无溶剂体系中脂肪酶催化共轭亚油酸(CLA)与甘油酯化反应制备共轭亚油酸油脂的影响因素。考察了酶量、体系水分、温度、时间、酶重复利用次数等因素对酯化反应的影响。结果表明，适宜的工艺条件是：酶量1％，水含量1％，温度70℃，在上述条件下反应24h，酯化率可达89．57％。研究了脂肪酶对共轭亚油酸异构体的底物选择性，结果表明，脂肪酶催化10，12-十八碳二烯酸酯化反应优于9，11-十八碳二烯酸。     

溶剂体系酶催化酸解反应合成富含共轭亚油酸油脂的研究

研究了溶剂体系中脂肪酶催化共轭亚油酸(CLA)与油脂酸解反应制备富含共轭亚油酸油脂的影响因素考察了温度、底物配比、酶量、体系水分、无机盐等因素对酯交换反应的影响结果表明,适宜的工艺条件是:水含量0.5％, 底物配比2:1,温度50℃,酶量200U/g油脂,在上述条件下反应12h,花生油中共轭亚油酸含量可达18％左右研究了溶剂体系中脂肪酶对共轭亚油酸异构体的底物选择性,结果表明,脂肪酶催化10,12-十八碳二烯酸酸解反应优于9,11-十八碳二烯酸酸     

酶法合成共轭亚油酸单甘酯的研究

采用脂肪酶G50(来源于Penicillium camembertii)作为生物催化剂,催化共轭亚油酸(CLA)和甘油酯化生成共轭亚油酸单甘酯(MAG)。研究了在无溶剂体系中,底物摩尔比、酶加量、体系含水量、反应温度和反应时间对产物中MAG含量和CLA酯化率的影响。结果表明,最佳反应条件为:底物摩尔比n(甘油)∶n(CLA)=4∶1,加酶量300U/g(基于反应底物总质量),体系含水量1%,反应温度15℃,反应时间24h。在最佳反应条件下,CLA的酯化率达到84.98%,MAG的含量为68.40%,共轭亚油酸双甘酯(DAG)含量为16.58%。通过分析产物的脂肪酸组成,发现Penicillium脂肪酶G50对CLA异构体没有拆分效果。     

无溶剂体系酶法催化合成共轭亚油酸薄荷酯

在无溶剂体系中采用脂肪酶AY 30催化共轭亚油酸(CLA)和L-薄荷醇反应,合成共轭亚油酸薄荷酯。研究了酶用量、水用量、反应温度和反应时间对酯化率和产物共轭亚油酸薄荷酯组成的影响。结果表明:最佳酯化率的反应条件为酶用量2%,水用量8%,反应温度45℃,反应时间48h;产物中c9t,11-CLA含量最高时的反应条件为酶用量2%,水用量4%,反应温度40℃,反应时间12 h,在此条件下,产物中c9,t11-CLA含量可达86.32%。     

超临界CO2状态下直接酯化法制备共轭亚油酸甘油酯

在超临界CO2状态下,采用脂肪酶催化共轭亚油酸(conjugated linoleic acid,CLA)与甘油反应制备共轭亚油酸甘油酯,分别应用单因素和正交试验考察分子筛添加量、酶用量、反应压力、温度和时间对CLA酯化率的影响。结果表明,最佳工艺条件为分子筛用量6%、酶用量4%、反应温度60℃、反应时间20h、反应压力11MPa,此条件下CLA的酯化率可达到90.98%。这种CLA甘油酯的脂肪酸组成中,9c,11t-CLA和10t,12c-CLA的含量分别为37.79%和41.66%。     

Novozym435酶促催化合成共轭亚油酸植物甾醇酯

以脂肪酶Novozym435为催化剂,在有机溶剂中催化合成共轭亚油酸植物甾醇酯.筛选出的最佳溶剂为正丁醇.采用单因素结合正交试验的方法,以甾醇酯化率为考察指标,对反应温度、反应时间、醇油摩尔比以及酶添加量进行了参数优选.结果显示,醇油摩尔比及酶添加量对酯化率影响不显著,反应时间对酯化率有一定影响,反应温度对酯化率的影响极显著.最优条件为:反应温度55℃,醇油摩尔比1:1,酶添加量8%,反应时间48 h.在此条件下,进行了共轭亚油酸植物甾醇酯酶促催化制备,并以气相色谱及红外光谱法对纯化后产物进行了分析确证.     

白地酶脂肪酶选择性酯化分离CLA异构体的研究

本文研究共轭亚油酸异构体的分离方法。利用白地霉脂肪酶(Geotrichumcandidumlipase,GCL)催化合成正丁酯的方法,考察温度、体系水分、酶用量、反应时间、底物配比对脂肪酶催化酯化率和脂肪酸丁酯中c9t11含量的影响。结果表明,经过酯化的脂肪酸丁酯层中c9t11CLA含量达到79.85%,t10c12CLA含量为4.59%;含有13.75%的油酸;c9t11CLA占共轭亚油酸两种异构体总含量的94.56%。形成c9t11CLA正丁醇酯的选择性系数平均为17.80。脂肪酸与正丁醇比例对脂肪酸酯中c9t11CLA含量具有显著性影响,在选取的范围内水分含量、酶用量的影响不显著。要得到较高c9t11CLA含量的脂肪酸产物,反应因子应选择:水分为0.50%,脂肪酸与正丁醇用量比为2.00∶1.00,酶用量为100U/g。白地霉脂肪酶对催化c9t11共轭亚油酸与正丁醇的酯化反应具有较高的选择性,因此,脂肪酶选择性酯化分离CLA异构体的方法是可行的。     

酶法拆分制备共轭亚油酸功能单体

研究利用Lipase AYS催化甲醇和共轭亚油酸(CLA)进行酯化反应,以期对共轭亚油酸异构体进行拆分制备共轭亚油酸功能单体。通过考察酯化反应的影响因素,确定了最优反应条件为:Lipase AYS加酶量180 U/g,反应温度40℃,CLA与甲醇摩尔比1∶1,缓冲液p H 6.5。在最优条件下反应8 h,总酯化率为49.5%,分离产物可以得到甲酯相与脂肪酸相,甲酯相中c9,t11-CLA甲酯的拆分效率达到86.2%,脂肪酸相中t10,c12-CLA的拆分效率达到80.0%,两者回收率分别为72.4%和54.2%。     

响应面法优化皱褶假丝酵母脂肪酶催化合成甾醇共轭亚油酸酯

以皱褶假丝酵母(Candida rugosa)脂肪酶为催化剂,在正己烷体系中催化植物甾醇与共轭亚油酸合成甾醇共轭亚油酸酯.以植物甾醇酯化率为考察指标,通过单因素实验和响应面实验确定最佳工艺参数为:酸醇摩尔比6∶1,反应温度40℃,酶用量9.6％(占底物质量),反应时间87 h.在此条件下,酯化率达97.5％.     

酶法合成没食子酸叶黄素酯的研究

以叶黄素和没食子酸为原料,在脂肪酶Novozym435 的催化下,合成没食子酸叶黄素酯,并用IR 对其结构进行表征。研究脂肪酶催化叶黄素与没食子酸合成没食子酸叶黄素酯的影响因素,考察酶量、溶剂、体系水分、温度、时间等因素对酯化反应的影响。结果表明,适宜的工艺条件为酶用量10mg/mL、溶剂为氯仿、初始加水量60mg/g、温度40℃、反应时间30h,在上述条件下没食子酸转化率可达81.8%。     

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.     

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.     

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.     

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.