杂多酸离子液体催化制备生物柴油研究

制备了3种杂多酸离子液体催化剂[PyPS]H_2PW_(12)O_(40)、[PyPS]_2HPW_(12)O_(40)和[PyPS]3PW_(12)O_(40),用于催化酯交换制备生物柴油,其中杂多酸离子液体[PyPS]H_2PW_(12)O_(40)的催化活性最高。采用单因素试验,考察了[PyPS]H_2PW_(12)O_(40)催化酯交换制备生物柴油时,醇油摩尔比、催化剂[PyPS]H_2PW_(12)O_(40)用量、反应温度和时间对生物柴油收率的影响,结果表明,当醇油摩尔比(甲醇/大豆油)为12,催化剂[PyPS]H_2PW_(12)O_(40)用量为6%,反应温度为100℃,反应时间为6 h时,生物柴油收率94.8%。重复使用性能试验表明,杂多酸离子液体[PyPS]H_2PW_(12)O_(40)重复使用6次后,生物柴油收率仍可达90.5%。     

微波辅助酸性离子液体催化大豆油制备生物柴油

设计合成了3种酸性离子液体[BSO3HMIM]HSO4、[BSO3HMIM][PTSA]、[BMIM]HSO4,考察酸性离子液体对大豆油和甲醇酯交换制备生物柴油的催化效果。以筛选出的酸性离子液体[BSO3HMIM]HSO4为催化剂,在微波辅助下,考察了醇油摩尔比、催化剂用量、反应温度和反应时间对生物柴油收率的影响。结果表明:当醇油摩尔比为10∶1,催化剂用量为8%,反应温度为120℃,反应时间为60 min,微波功率为320 W时,生物柴油收率可达95.8%;离子液体[BSO3HMIM]HSO4循环使用6次后,生物柴油收率没有明显降低,保持在90%以上。     

微波辐射下离子液体[Bmim]HSO4催化葵花籽油制备生物柴油

生物柴油是绿色可再生能源。研究了微波辐射下离子液体[Bmim]HSO4催化葵花籽油与甲醇通过酯交换反应制备生物柴油,考察了催化剂用量、微波功率、醇油摩尔比和反应时间对酯交换反应的影响。试验结果表明,当醇油摩尔比为12：1、催化剂用量（催化剂与油的质量比）为7%、微波功率为300W、反应时间为35min时,生物柴油的收率可以达到98.9%。     

碱性离子液体[Bmim]OH催化菜籽油制备生物柴油

研究合成了具有碱性功能的离子液体[Bmim]OH,并用其催化菜籽油酯交换反应制备生物柴油,考察了醇油摩尔比、反应温度、反应时间和离子液体用量对酯交换反应的影响及离子液体的稳定性。结果表明:在n(甲醇)∶n(菜籽油)=16∶1,反应温度150℃,反应时间4 h和离子液体用量为菜籽油质量6%的条件下,生物柴油收率可达96.2%,并且该离子液体的稳定性良好,循环使用5次催化性能没有明显降低。     

碱性离子液体催化棉籽油制备生物柴油的工艺研究

应用碱性离子液体[Emim]OH催化棉籽油制备生物柴油,考察了醇油比、催化剂用量、反应温度、反应时间对生物柴油收率的影响;正交试验确定[Emim]OH催化工艺条件为：醇油摩尔比6∶1、催化剂用量3.5%、反应时间50 min、反应温度55℃。在该优化条件下,甲酯混合物收率高于90%,催化剂[Emim]OH重复使用6次没有明显消耗,催化性能稳定。     

高活性离子液体杂多酸催化大豆油制备生物柴油工艺的研究

以氯球为载体,经氨基化、磺化等制备的系列氯球固载化离子液体杂多酸为催化剂,大豆油与甲醇为原料进行酯交换反应制备生物柴油工艺研究,考察了醇油摩尔比、催化剂量、反应温度及反应时间等因素对生物柴油产率的影响,并通过响应面法优化制备工艺。研究表明,[CPPI-SO3H]2.0H1.0PW12O40催化剂具有最好的催化酯交换反应活性,催化剂强的Br?nsted酸性及“假液相”特性是其具有高活性的原因。利用响应面法优化的最佳生物柴油制备工艺条件为：醇油摩尔比25.5: 1,催化剂用量为大豆油质量的5.2%,反应时间20 h,反应温度119 ℃,此条件下,生物柴油的产率为97.3%,该结果与模型预测值基本相符。实验结果对以植物油为原料制备生物柴油研究提供参考。     

微波协同功能化酸性离子液体催化制备生物柴油工艺研究

通过两步法合成了功能化酸性离子液体[HSO_3-pPy]HSO_4,在微波协同条件下,以其作为酯交换反应的催化剂,催化制备生物柴油研究。采用单因素试验,考察了微波功率、醇油摩尔比、离子液体[HSO_3-pPy]HSO_4用量、反应温度和时间对生物柴油收率的影响。结果表明,生物柴油的最佳制备工艺条件为微波功率400 W、醇油摩尔比12∶1、催化剂[HSO_3-pPy]HSO_4用量5%、反应温度70℃、反应时间45 min,在最佳制备工艺条件下,生物柴油收率可达95.1%。同时,考察了催化剂[HSO_3-pPy]HSO_4的重复使用性能,重复使用6次后,催化剂的催化活性没有明显降低。     

双核酸性离子液体[DABCO-PS][HSO_4]催化蓖麻油制备生物柴油研究

研究合成了双核酸性离子液体[DABCO-PS][HSO_4],并将其用于催化蓖麻油酯交换制备生物柴油。优化后得离子液体前体[DABCO-PS]合成最佳条件为n(1,3-丙烷磺酸内酯)∶n(三乙烯二胺)=2∶1、反应温度60℃、反应时间3 h,在此条件下离子液体前体收率达93.4%。采用红外光谱、核磁共振和质谱对[DABCO-PS][HSO_4]进行表征,确定产物为目标离子液体。优化得到[DABCO-PS][HSO_4]催化蓖麻油制备生物柴油的最佳条件为n(甲醇)∶n(蓖麻油)=12∶1、离子液体用量4%(以蓖麻油质量计)、反应温度50℃、反应时间1 h,在此条件下生物柴油收率达90%。采用气相色谱确定生物柴油主要成分是棕榈酸甲酯、亚油酸甲酯、油酸甲酯、亚麻酸甲酯、硬脂酸甲酯和蓖麻油酸甲酯,且脂肪酸甲酯占生物柴油的90%以上。     

微波辐射离子液体[Bpy]HSO_4催化葵花籽油制备生物柴油

生物柴油是一种绿色可再生能源。该文报道微波辐射下离子液体[Bpy]HSO4催化葵花籽油与甲醇通过酯交换反应制备生物柴油,以正交法对制备工艺条件进行优化,考察醇油物质量比、催化剂用量、微波功率和反应时间对酯交换反应影响。实验结果表明,当醇油物质量比为10∶1、催化剂用量(催化剂与油质量比)为5%、微波功率为400W、反应时间为45min时,生物柴油转化率可达96.2%;与传统加热方式相比,采用微波辐射加热方式,反应时间明显缩短,能耗减少。     

响应面法优化吡咯烷酮离子液体[HNMP]CH3SO3催化菜籽油酯交换制备生物柴油的工艺研究

合成了酸性离子液体[HNMP]CH3SO3,并用于催化菜籽油酯交换制备生物柴油。采用响应面法对离子液体[HNMP]CH3SO3催化菜籽油酯交换制备生物柴油的工艺参数进行优化,获得的最佳反应条件为:反应温度100℃,醇油摩尔比9∶1,催化剂用量10%,反应时间12 h。在最佳条件下,生物柴油转化率为84. 8%。该离子液体有较好的稳定性,循环使用4次后生物柴油转化率仍可达到79. 6%。     

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