SO_3H-功能化酸性离子液体催化合成苯甲醛乙二醇缩醛

以苯甲醛和乙二醇为原料,SO3H-功能化酸性离子液体为催化剂,合成苯甲醛乙二醇缩醛。选取醇醛物质的量比、反应时间、离子液体用量、带水剂量4个因素进行中心组合优化试验,运用响应面法得出苯甲醛乙二醇缩醛最佳合成工艺条件为:醇醛物质的量比1.4∶1,反应时间2 h,离子液体用量为醛用量的4.5%,带水剂量10m L。在此最佳反应条件下苯甲醛乙二醇缩醛收率为88.6%,此结果与模型预测值基本相符。     

磷钼酸催化法制备某些缩醛(酮)的研究

缩醛（酮）合成反应的传统催化剂为无机强酸,但由于副反应多、腐蚀性强和易污染环境等缺点,其使用受到限制．用磷钼酸为催化剂,通过醛（酮）与乙二醇直接反应得到了三种缩合产物．对影响反应的诸因素进行研究,结果表明,用磷钼酸作催化剂,用量小,活性高,产品收率较高,且重复使用性能较好．     

复合固体超强酸催化合成苯甲醛乙二醇缩醛

以四氯化锡和过硫酸铵为主要原料,采用沉淀-浸渍法制备新型固体超强酸催化剂S2O82-/SnO2,并用于苯甲醛乙二醇缩醛的合成反应.该催化剂制备的最优条件为：焙烧温度为500℃,（NH4）2S2O8浸渍浓度1.0 mol/L,焙烧时间2.5 h.采用该催化剂合成苯甲醛乙二醇缩醛的最佳条件为：n（乙二醇）∶n（苯甲醛）=1.7∶1,反应时间1.5 h,V（环己烷）=8 mL,m（S2O82-/SnO2）=0.6 g.此时苯甲醛乙二醇缩醛收率可达89.29%.该实验催化剂可重复使用,产品纯度≥98.0%.     

3种海参与3种贝类中脂肪酸及烯醚键基团的 气相色谱/质谱分析比较

本文研究了用气相色谱/质谱法测定比较3种海参与3种贝类脂肪酸及脂肪醛二甲基缩醛的方法。该6种原料经Folch法提取总脂,用10%硫酸-甲醇溶液对其进行甲酯化反应,通过气相色谱/质谱法对其脂肪酸及脂肪醛二甲基缩醛的组成进行分析。实验结果表明：10%硫酸-甲醇溶液能有效地对脂肪酸进行甲酯化衍生;同时促使烯醚键断裂,并与甲醇发生缩醛反应生成脂肪醛二甲基缩醛。通过气相色谱/质谱分析,从3种海参与3种贝类的气相色谱/质谱图中共鉴定出24种脂肪酸,海参中脂肪酸以C16:0,C16:1(n-7)和C20:4(n-6)为主;贝类中脂肪酸以C16:0,C20:5(n-3)和C22:6(n-3)为主;海参与贝类中脂肪醛二甲基缩醛均以C18:0DMA为主。海参和贝类中的脂肪酸及脂肪醛二甲基缩醛的组成与含量都相差较大。     

苯甲醛与乙二醇缩醛化反应的研究

研究了苯甲醛与乙二醇在732#强酸性阳离子交换树脂催化下的合成条件,得到了缩醛化反应的最佳合成条件:醛/醇摩尔比为1∶1.75,带水剂用量(苯)为40mL,催化剂用量为1.5g,反应时间为90min,并在产物的后处理时采用了减压过滤除去催化剂和减压蒸馏分离产物。     

3种海参与3种贝类中脂肪酸及烯醚键基团的气相色谱/质谱分析比较

目的采用气相色谱/质谱法测定比较3种海参与3种贝类脂肪酸及脂肪醛二甲基缩醛的方法。方法6种原料经Folch法提取总脂,用10%硫酸-甲醇溶液对其进行甲酯化反应,通过气相色谱/质谱法对其脂肪酸及脂肪醛二甲基缩醛的组成进行分析。结果 10%硫酸-甲醇溶液能有效地对脂肪酸进行甲酯化衍生,同时促使烯醚键断裂,并与甲醇发生缩醛反应生成脂肪醛二甲基缩醛。通过气相色谱/质谱分析,从3种海参与3种贝类的气相色谱/质谱图中共鉴定出24种脂肪酸,海参中脂肪酸以C16:0,C16:1(n-7)和C20:4(n-6)为主;贝类中脂肪酸以C16:0,C20:5(n-3)和C22:6(n-3)为主;海参与贝类中脂肪醛二甲基缩醛均以C18:0DMA为主。结论海参和贝类中的脂肪酸及脂肪醛二甲基缩醛的组成与含量相差较大。     

H3PW12O40/TiO2催化合成肉桂醛乙二醇缩醛

用溶胶-凝胶法合成出具有Keggin结构的杂多酸H3PW12O40/TiO1复合催化材料,用FT-IR等方法研究了其结构形态,并考察了复合催化剂催化合成肉桂醛乙二醇缩醛的应用研究,其中重点考察了反应物配比、催化剂用量、反应时间及催化剂的重复使用性能等对产品收率的影响.结果表明,合成肉桂醛乙二醇缩醛的较优反应条件为肉桂醛0.1 mol、n(肉桂醛)/n(乙二醇)=1.0,1.5(mol/mol)、催化剂的用量为反应物总质量的2.0%、带水剂环已烷12 mL、回流反应3 h,肉桂醛乙二醇缩醛的产率可达83.0%以上.     

硫酸铁钾盐加合物催化合成香兰素1,2-丙二醇缩醛

以铁钾盐加合物为催化剂,通过香兰素与1,2-丙二醇反应合成了香兰素1,2-丙二醇缩醛。考察了铁钾盐加合物的催化活性,研究了醛醇摩尔配比、反应时间、催化剂用量及稳定性等对产物收率的影响。实验结果表明,铁钾盐加合物是合成香兰素与1,2-丙二醇的理想催化剂,其较优反应条件为:香兰素0.1mol、n(香兰素)/n(1,2-丙二醇)=1.0/2.4(mol/mol),催化剂的用量为反应物总质量的2.0%,16mL苯带水剂,回流反应3.0h,香兰素1,2-丙二醇缩醛的收率可达86.0%以上。     

Vc缩醛和异Vc缩醛对茶籽油的抗氧化性研究

参照我国规定的有关抗氧化剂在食用油脂中的最高允许浓度,分别将辛醛Vc缩醛、辛醛异Vc缩醛、月桂醛Vc缩醛和月桂醛异vc缩醛等抗氧化剂加入到新鲜茶籽油中,在60℃下进行抗氧化试验.过氧化值(POV)数据表明,缩醛化后的Vc、异vc具有更好的抗氧化性;碳链长的缩醛比碳链短的缩醛具有更好的抗氧化性;异Vc缩醛比相应的Vc缩醛具有更好的抗氧化性;月桂醛Vc缩醛和月桂醛异Vc缩醛的抗氧化性均比PG好,但比TSHQ稍差.     

基于十二碳烯醛的番茄红素全合成

以6,10-二甲基-3,5,9-十一烷三烯-2-酮(8)与亚甲基二磷酸四乙酯(7)经Wittig-Horner反应得到2,6,10-三甲基-1,3,5,9-四烯十一烷基膦酸二乙酯(9);以E-2-丁烯-1,4-二膦酸二乙酯(2)与4,4-二甲氧基-2-丁酮(3)通过Wittig-Horner反应和水解反应合成化合物3,8-二甲基-3,5,7-辛三烯-1,10-二醛(5),2,6,10-三甲基-1,3,5,9-四烯十一烷基膦酸二乙酯(9)与3,8-二甲基-3,5,7-辛三烯-1,10-二醛(5)通过Wittig-Horner反应得到目标产物番茄红素(10),并采用核磁共振(NMR)、质谱(HRMS/GC-MS)和红外光谱(IR)进行结构验证。结果表明,合成的番茄红素总产率为16.7%。     

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.     

Analysis on Economic Indicators from 62 Enterprises in Printing Machinery Industry in Q1 2014

Operation of printing machine industry was still unsatisfactory in the first quarter of 2014.Analysis on operation of printing machine industry.a.Market demand was not strong;sales of product undulated and declined.According to the statistics,the total industrial output value fell by 19.28% in the first quarter of 2014 than the average quarter value in 2013; industrial added value decreased by 4.16%; sales revenue dropped by 22.83%. h. Business operation of enterprises was in poor condition. c. R＆D of new products is an important transformation guarantee for enterprises. d. To take self explore new ways upgrading advantages,and explore new ways.