阳离子树脂催化合成环氧化大豆油的研究

以强酸性阳离子交换树脂为催化剂,考察了催化剂用量、过氧化氢与油中双键摩尔比、反应温度、乙酸用量、反应时间等因素对环氧化反应的影响.在单因素实验的基础上,通过正交实验优化确定了最佳合成条件:催化剂用量为油质量的13％,乙酸加入量为油质量的20％,过氧化氢与油中双键摩尔比为1.7∶1,反应温度68℃,反应时间7.5h;在最佳条件下制得的环氧化大豆油为淡黄色黏稠状透明液体,环氧值为6.49％.     

酸性离子液体催化合成环氧大豆油工艺的研究

以大豆油为原料,Br?nsted酸性离子液体为催化剂,考察反应温度、乙酸用量、H2O2用量、催化剂量及反应时间等因素对大豆油环氧化反应的影响。在单因素实验的基础上通过响应面分析法优化环氧大豆油制备工艺。研究表明,N,N-二甲基苄基丙磺酸硫酸氢盐（[DMBPS]HSO4）离子液体具有较好的催化环氧化性能,离子液体强的Br?nsted酸性是其具有高催化活性的原因。以[DMBPS]HSO4为催化剂,通过响应面分析法优化的环氧大豆油最佳合成条件为：乙酸用量9%,反应温度110 ℃,H2O2用量77%,催化剂量6.1%,反应时间3.1 h,优化条件下环氧大豆油的环氧值为7.11,该结果与模型预测值基本相符。     

过氧化氢制备环氧葵花籽油的研究

研究了通过过氧化氢(提供氧源)在甲酸(起到转移活性氧的作用)催化下的制备环氧葵花籽油的工艺条件,考察了搅拌速度、甲酸用量、过氧化氢用量、反应温度等因素对产品环氧值的影响.确定最佳工艺条件为:甲酸用量0.5 mol(以油中双键摩尔数为基准),过氧化氢用量2.0 mol(以油中双键摩尔数为基准),反应温度60℃,反应时间6 h.在最佳条件下所得产品的环氧值达5.5%,碘值(I)为10 g/100 g.     

低共熔溶剂催化合成环氧大豆油工艺研究

以大豆油为原料,氯化胆碱-甲磺酸形成的低共熔溶剂为催化剂,考察反应温度、催化剂用量、乙酸用量、过氧化氢用量及反应时间等因素对环氧化反应的影响,并通过响应面分析法优化环氧大豆油制备工艺。研究表明,氯化胆碱-甲磺酸低共熔溶剂具有较好的催化环氧化反应性能,以其为催化剂,并通过响应面分析法优化的环氧大豆油最佳合成条件为：反应温度73 ℃,催化剂量4.8 wt%,H2O2用量为72 wt%,反应时间3.6 h,乙酸用量9 wt %,此条件下,环氧大豆油的环氧值为6.98,该结果与模型预测值基本相符。     

催化棉籽油环氧化的影响研究

通过以[Mim(CH_2)_4SO_3H][HSO_4]为催化剂,催化棉籽油的环氧化反应,研究发现[Mim(CH_2)_4SO_3H][HSO_4]催化棉籽油环氧化的适宜条件为:反应时间120 min,温度70℃,n(H_2O_2)∶n(不饱和双键)=2.5∶1,n(甲酸)∶n(不饱和双键)=0.6∶1,催化剂用量4%,该条件下催化棉籽油的环氧值为5.33%,转化率为71.95%。     

Al-Zr-SiO2固体酸催化大豆油环氧化的研究

以Al-Zr-SiO_2固体酸为催化剂制备环氧大豆油,考察反应时间、催化剂用量、反应温度、n(H_2O_2)∶n(双键)对环氧化反应的影响,并通过响应面试验对环氧化反应工艺条件进行优化。得到环氧化反应最佳工艺参数为,大豆油∶甲酸∶过氧化氢=1∶0.5∶2.5(摩尔比),Al-Zr-SiO_2固体酸催化剂用量为0.8%,反应温度为70℃,反应时间为4 h,在该条件下所得大豆油的环氧值为6.57%。     

四丁基溴化铵催化合成环氧大豆油

在无溶剂无羧酸条件下,以四丁基溴化铵为相转移催化剂,用65%的叔丁基过氧化氢(TBHP)为氧源直接合成环氧大豆油。考察了反应温度、反应时间、催化剂用量及TBHP与碳碳双键摩尔比对环氧化反应的影响,通过红外光谱对催化环氧化的机理进行了初步探究。结果表明:在反应温度65℃、反应时间3 h、催化剂用量3.0 g(10.0 g大豆油)、TBHP与碳碳双键摩尔比1.5∶1条件下,催化环氧化效果最好,环氧值、转化率和选择性分别达到3.5%、53.9%和77.5%。此方法操作简单,催化剂价格低,简化了工艺流程,降低了工艺成本,同时克服了传统方法使用羧酸和溶剂等造成的弊端。     

Cu-salen配合物催化大豆油环氧化合成环保塑化剂

以3,5-二叔丁基水杨醛和乙二胺(摩尔比2∶1)为原料合成了N,N’-二3,5 -二叔丁基水杨醛基乙二胺(salen配体),salen配体与Cu( OAC)2·H20的乙醇溶液混合回流得到Cu - salen配合物.对重结晶提纯后的salen配体及配合物进行了红外、紫外、核磁等表征.Cu - salen配合物作为大豆油环氧化反应催化剂,以叔丁基过氧化氢(TBHP)为氧源,最佳反应条件为:60℃下反应8h,催化剂用量为大豆油质量的2％,得到最佳环氧化效果,其环氧产物转化率为52.5％,选择性为59.6％.超声波辅助下,环氧值由2.2％提高到4.0％,环氧值提高了45％;转化率提高至71.4％,选择性提高到63.5％;反应时间由8h缩短至0.5h,催化剂用量减少为大豆油质量的0.5％.     

过氧化氢用量对猪油环氧化的影响

以甲酸作催化剂,在60℃下,用双氧水对猪油进行环氧化,考察了过氧化氢用量对产物碘值和环氧指数的影响。结果表明,随着过氧化氢用量的增加,产物碘值减小,环氧指数增大,H2O2/C C摩尔比为1.5：1时,碘值达到最小值,环氧化指数达到最大值,此后碘值基本不变,环氧指数减小;参与环氧化的碳碳双键与测定碘值所用双键不完全一致。     

酶碱法脱脂结合脱色制备豆渣膳食纤维的研究

以大豆渣为原料,采用酶碱法脱脂并结合H2O2脱色的方法制备不溶性膳食纤维。酶碱复合脱脂是先采用碱性脂肪酶再结合氢氧化钠碱处理,对豆渣进行脱脂,随后再进行H2O2脱色。结果表明：在温度50℃、pH值9.5、反应时间2h、酶液浓度120 U/mL、氢氧化钠浓度3%的脱脂优化工艺条件下,以及H2O2浓度0.3 mol/100g干豆渣、pH值为11、温度70℃、水料比15∶1、反应时间1h的脱色优化工艺条件下,可制备得到理想的豆渣不溶性膳食纤维,其白度值为74.51%,脱脂率达到98.81%。     

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.