新型过氧化氢漂白活化剂4-(2-壬酰氧基乙氧基羰基氧基)苯磺酸钠的合成

研究了以2-壬酰氧基乙基氯甲酸酯和对羟基苯磺酸钠为原料,水为溶剂,氢氧化钠为缚酸剂,合成一种新型过氧化氢漂白活化剂4-(2-壬酰氧基乙氧基羰基氧基)苯磺酸钠的清洁工艺,考察了影响合成反应的主要因素。适宜的工艺条件为:n(2-壬酰氧基乙基氯甲酸酯)∶n(对羟基苯磺酸钠)∶n(氢氧化钠)=2.0∶1∶2.5,水为溶剂,反应温度60℃,反应时间4h,4-(2-壬酰氧基乙氧基羰基氧基)苯磺酸钠的收率高于67.0%。结果表明:该工艺具有操作简单、易控,环境友好等优点。     

一步法合成H2O2漂白活化剂4-壬酰氧基苯磺酸钠的研究

以4-羟基苯磺酸钠和壬酸为原料,亚硫酰氯为酰化剂,甲苯为溶剂,采用一步法合成了4-壬酰氧基苯磺酸钠.考察了影响合成反应的诸多因素.适宜的工艺条件为n(4-羟基苯磺酸钠)∶n(壬酸)∶n(亚硫酰氯)=1∶1∶1.3,反应温度为85℃,反应时间为5h,在此条件下,4-壬酰氧基苯磺酸钠的收率为84.5％,含量为95.8％,用红外光谱、核磁共振验证了目标产物.结果表明,该工艺具有操作简单、易控,产品质量好、收率高,溶剂易回收等优点.     

过氧化氢漂白活化剂壬酰氧基苯磺酸钠的合成研究

研究了以壬酸酐和对羟基苯磺酸钠为原料,丙酮为溶剂,无水碳酸钠为缚酸剂,合成过氧化氢漂白活化剂壬酰氧基苯磺酸钠的清洁工艺,考察了影响合成反应的主要因素。适宜的工艺条件为：n（对羟基苯磺酸钠）：n（壬酰酐）：n（无水碳酸钠）=1：1.3：1.5,反应温度0～5℃,反应时间3h,壬酰氧基苯磺酸钠的收率为90.7%,质量分数为95.5%。结果表明,该工艺具有操作简单、易控,产品质量好、收率高,环境友好等优点。     

离子液体中尼泊金甲酯的合成

研究了离子液体[Hmim]+BF4-中尼泊金甲酯的合成,并通过正交实验获得了反应的最佳条件:反应的摩尔比为n(对羟基苯甲酸)∶n(甲醇)为1∶4 .反应温度为回流,反应时间为4 h ,产率可达88.9%.离子液体[Hmim]+BF4-在尼泊金甲酯的合成中具有良好的催化性能,反应条件温和,无废酸产生,无腐蚀,而且可以重复使用.     

对羟基苯甲酸苄酯合成新方法

介绍了一种在固体超强酸催化作用下,氧化钙作吸水剂,二甲苯作共沸剂,对羟基苯甲酸与苄醇回流脱水直接酯化的新方法。详细探讨了影响酯化反应的各种因素,得出了酯化反应的最佳条件:n(对羟基苯甲酸)∶n(苄醇)∶n(二甲苯)=1∶3∶5,m(对羟基苯甲酸)∶m(SO42-/TiO2-Al2O3)=100∶7,回流反应4h。在此条件下,酯化产率可达90.7%。结果表明,该方法反应时间短,酯化产率高,工艺简单,催化剂活性高。     

SO2-4/MoO3-TiO2催化合成对羟基苯甲酸丁酯

在固体酸SO2-4/MoO3-TiO2的催化下,对羟基苯甲酸与丁醇直接酯化,再经过滤、减压蒸馏制得合格的对羟基苯甲酸二丁酯,其最佳工艺条件为催化剂用量为反应物总质量的1.0%,n(丁醇)n(对羟基苯甲酸)=2.91.0,反应温度150℃,反应时间2.5h,对羟基苯甲酸的转化率为97.2%,催化剂可重复使用.     

对羟基苯甲酸丙酯的强酸性阳离子交换树脂催化合成研究

以对羟基苯甲酸和正丙醇为原料,强酸性阳离子交换树脂为催化剂,经过回流脱水酯化法直接合成对羟基苯甲酸丙酯。探讨了反应温度、反应时间、原料配比、催化剂用量等条件对合成反应的影响。得到的最佳合成工艺条件为：对羟基苯甲酸用量为0.1mol的前提下,反应温度85-90℃、反应时间2.5h、丙醇与对羟基苯甲酸的摩尔比为3.0∶1、催化剂用量为反应物料总质量的2.0%,此时反应的酯化率为97.5%。催化剂不经处理可循环使用多次,而且具有价格低廉、催化活性好、不腐蚀设备、无环境污染等优点。     

纳米稀土复合固体超强酸SO42-/ZrO2-2% Nd2O3催化合成对羟基苯甲酸正丁酯

采用共沉淀法制备稀土复合固体超强酸SO2-4/ZrO2-2%Nd2O3催化剂,电镜分析表明,该催化剂颗粒为纳米级。将其用于对羟基苯甲酸和正丁醇的酯化反应中,考察了影响合成反应的诸多因素。结果显示,催化合成对羟基苯甲酸正丁酯的优化工艺条件为:采用过量的正丁醇作共沸带水剂,回流反应时间为3.0h,催化剂用量为对羟基苯甲酸质量的3.5%,正丁醇与对羟基苯甲酸的物质的量比为3.0∶1.0,在此条件下酯化率可达97.5%。产品经熔点测定、元素分析、液相色谱和红外光谱表征为高纯度的对羟基苯甲酸正丁酯。自制催化剂具有良好的催化活性,并可多次重复再生使用。     

尼泊金十二酯合成工艺研究

对羟基苯甲酸与正十二醇在对甲苯磺酸催化下,以苯为溶剂,直接酯化合成尼泊金十二酯,其最佳的反应条件为:对羟基苯甲酸与正十二醇摩尔比1∶3,反应时间为4h,反应温度为130～140℃,催化剂与对羟基苯甲酸的摩尔比为0.07∶1,产率90.1%。     

尼泊金甲酯的绿色合成

采用对羟基苯甲酸与碳酸二甲酯为原料,以硅胶负载高氯酸为催化剂,加热反应制得尼泊金甲酯,测定所合成的尼泊金甲酯的核磁共振氢谱及熔点并与文献报道值相比较,从而确证所合成的尼泊金甲酯的结构。对影响尼泊金甲酯收率的因素(反应物配比、反应温度、反应时间及催化剂用量)进行研究,确定尼泊金甲酯的适宜合成条件:n(碳酸二甲酯)∶n(对羟基苯甲酸)=2∶1,反应温度为90℃,反应时间为8h,催化剂用量为碳酸二甲酯摩尔量的0.2%,在此条件下尼泊金甲酯的收率达93.1%。与目前合成尼泊金甲酯的方法相比,该法收率高,硅胶负载高氯酸催化剂可以回收利用,无三废排放,绿色环保,适宜规模化生产。     

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.     

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.     

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.     

Announcing a new international peer-reviewed journal:Food Science and Human Wellness now accepting manuscript submission in English

<正>We are pleased to announce the launch of a new international peer-reviewed journal-Food Science and Human Wellness,ISSN 2213-4530,which is an open access journal,produced and hosted by Elsevier B.V.on behalf of Beijing Academy of Food Sciences.Food Science and Human Wellness is an international peer-reviewed English journal that provides a forum for the dissemination of the