冷冻干燥法制备纳米氧化镁条件的研究

较详细地介绍了以卤水和工业氨水为原料，以冷冻干燥法制备纳米氧化镁的方法，对其影响条件作了研究，并对产品作了表征。结果表明，冷冻干燥法能有效地改善凝胶干燥过程中粒子间的团聚性能，制备出的纳米氧化镁粒子的平均粒径为20nm，粒子分布均匀，分散性好。     

白云石制备纳米氧化镁的方法研究

以白云石为原料,采用消化-分散沉淀-超声震荡法处理后,灼烧制得了纳米氧化镁.对前驱体进行热分析(TG-DTG-DTA),确定了合适的煅烧温度为600℃.研究了分散剂种类及用量、沉淀剂种类、溶剂等对纳米氧化镁粒径的影响,并用原子吸收(AAS)、X射线衍射(XRD)、扫描电镜(SEM)等进行了表征.结果表明,该法制备的纳米粒子纯度高、分散性好,晶体粒子分布均匀,纳米颗粒粒径为12.5 nm.     

熊果酸壳聚糖纳米粒子的体外消化特性及稳定性

分别采用冷冻干燥、微波冷冻干燥和喷雾干燥方式制备熊果酸-壳聚糖纳米粒子，研究了熊果酸纳米粒子在光照、不同温度及体外模拟胃肠消化过程中的贮藏稳定性和抗氧化能力。结果表明，胃消化阶段，熊果酸纳米粒子释放率较少；肠消化阶段，冷冻干燥、微波冷冻干燥和喷雾干燥制备的熊果酸纳米粒子释放率分别为59%、55%和50%,说明熊果酸纳米粒子具有缓释特性。体外模拟胃肠消化阶段的1,1-二苯基-2-三硝基苯肼(1,1-diphenyl-2-picrylhydrazyl, DPPH)自由基清除率试验结果表明，熊果酸纳米粒子的抗氧化性高于熊果酸。熊果酸和熊果酸纳米粒子在4℃下稳定性较高，熊果酸保留率均在80%以上。避光室温条件下，冷冻干燥、微波冷冻干燥和喷雾干燥制备的熊果酸纳米粒子保留率分别为66%、64%和60%。其中，冷冻干燥制备的熊果酸纳米粒子在4℃和避光条件下DPPH自由基清除率最高，分别为2.32、2.09 mg/g。研究结果表明，冷冻干燥和微波冷冻干燥制备的熊果酸纳米粒子的光照、温度以及模拟胃肠消化稳定性和抗氧化性均高于熊果酸，熊果酸的稳定性显著提高。     

微通道反应器制备纳米硫酸钡的工艺研究

利用微通道反应器,以硫酸钠和硫化钡为原料反应并进行纳米硫酸钡粒子制备研究,考察了微通道反应器制备纳米硫酸钡粒子的影响因素,并对产品进行激光粒度检测和TEM测试。结果表明,该法可以制备出平均粒径50～80 nm、分布窄的纳米硫酸钡粒子。     

纳米氧化镁制备方法与进展

介绍了用机械粉碎法、流动液面真空蒸发法、固相反应法、直接沉淀法、均匀沉淀法和醇盐水解法、水热法、气相氧化法、溶胶-凝胶法、微乳液/反向胶束法等方法制备纳米氧化镁原理,并对个别方法进行简要评价。针对目前纳米氧化镁研究中存在的问题,提出未来研究方向。     

溶剂置换干燥法制备纳米氧化镁粉体的研究

以MgCl2·6H2O和CO(NH2)2为原料,由均匀沉淀法制备氢氧化镁沉淀,采用溶剂置换直接煅烧法、溶剂置换箱式干燥法、溶剂置换微波干燥法和超临界CO2萃取干燥法除去沉淀中的湿分,再将干燥的氢氧化镁粉体经马弗炉煅烧得到纳米氧化镁粉体,通过透射电子显微镜和X射线衍射仪的表征与分析,研究不同溶剂置换干燥方式对纳米氧化镁粉体形貌、尺寸和团聚行为的影响;讨论了溶剂置换干燥的基本原理和溶剂置换的方法.     

均匀沉淀法制备纳米氧化镁工艺研究

以氯化镁为原料,尿素为沉淀剂,聚乙二醇辛基苯基醚(OP-10)为表面活性剂,采用均匀沉淀法制备了纳米氧化镁。考察了镁离子浓度、反应物配比、反应温度、煅烧温度、煅烧时间对氧化镁粒径的影响。采用热重分析仪对前驱体氢氧化镁进行了表征,采用X射线衍射仪和扫描电镜对氧化镁进行了表征。结果表明,在镁离子的浓度为1.5mol/L;反应物配比为4:1;反应温度为110℃;煅烧温度为500℃;煅烧时间为3h时,所得氧化镁粒径最小,为18nm,且粒径分布均匀,晶型为立方晶系。     

纳米壳聚糖粒子制备工艺优化及抗菌性研究

以壳聚糖和三聚磷酸钠为原材料,采用离子交联法制备壳聚糖纳米粒子。在单因素实验的基础上,采用响应曲面分析法对纳米壳聚糖制备工艺进行优化,并对其抗菌性进行了研究。最佳制备工艺为:壳聚糖质量浓度0.76 mg/mL,三聚磷酸钠质量浓度0.77 mg/mL,壳聚糖与三聚磷酸钠体积比4.11∶1,壳聚糖溶液pH值50。纳米壳聚糖的粒径和Zeta电位的理论预测值分别为122.3 nm和+23.43 mV。验证性实验表明,纳米壳聚糖的粒径为119.2 nm,Zeta电位为+22.8 mV,与理论值偏差分别为2.53%、2.69%,纳米粒子分散均匀。当纳米壳聚糖质量浓度达到0.6 mg/mL时,对大肠杆菌和金黄色葡萄球菌表现出明显抑制作用。该制备工艺为高性能纳米壳聚糖粒子的制备及果蔬保鲜方面的应用提供理论参考。     

细乳液聚合炭黑/乳胶粒纳米复合粒子的制备及其性能

以可聚合分散剂1-烯丙氧基-3-(4-壬基苯酚)-2-丙醇聚氧乙烯(10)醚硫酸铵（DNS-86）为乳化剂,甲基丙烯酸甲酯（MMA）为共聚单体,通过细乳液聚合法制备了炭黑/乳胶粒纳米复合粒子。以炭黑/乳胶粒纳米复合粒子为着色剂对棉织物印花,探讨了粘合剂用量,固色温度和时间对摩擦色牢度的影响。FTIR,TEM及TGA研究结果表明细乳液聚合可以在炭黑表面包覆乳胶粒,制备炭黑/乳胶粒纳米复合粒子。炭黑/乳胶粒纳米复合粒子作为着色剂较佳印花工艺为粘合剂用量15wt%,固色温度180oC,固色时间150s。相同条件下,炭黑/乳胶粒纳米复合粒子印花织物的K/S值、摩擦牢度明显优于超细炭黑。     

纳米纤维素的甲酸制备及其对聚乙烯力学性能的强化

以杨木硫酸盐法漂白浆(卡伯值17.3)为原料制备纳米纤维素。使用甲酸制备纳米纤维素,用光学显微镜观察所制备的纳米纤维素的尺寸,将其冷冻干燥后并计算得率。其次,探索添加纳米纤维素复合材料的性能。物料分析结果如下:加入甲酸的时间越长,所得的纳米纤维素得率越少。甲酸-盐酸工艺比甲酸法纳米纤维素的得率低。加入不同浓度的过氧化氢,则对所得纳米纤维素的影响不大。复合材料的拉伸应力随着纳米纤维含量呈几何增长,在纳米含量为2.5%时复合材料的强度增加了77.28%,复合材料的延展性在纳米含量为2%时达到最大,形变增加97.02%。     

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.