溶剂法制备戊二酸淀粉酯及其性质研究

以玉米淀粉为原料,戊二酸酐为酯化剂,探讨了在乙醇溶剂中制备戊二酸淀粉酯的过程中淀粉乳初始浓度、反应时间、反应温度和体系p H值对产物取代度的影响,得到制备戊二酸淀粉酯的工艺条件:淀粉乳浓度35%(质量分数,下同),反应时间3 h,反应温度35℃,体系p H为8.5。采用傅里叶变换红外光谱(FT-IR)、扫描电子显微镜(SEM)、X射线衍射仪(XRD)及差示扫描量热仪(DSC)对产物进行了表征。结果表明:戊二酸淀粉酯中新出现了1733 cm-1处C=O的伸缩振动吸收峰,1555 cm-1处游离的-COO-的反对称伸缩振动吸收峰,说明淀粉分子酯化成功;改性淀粉颗粒表面出现了不同程度的凹陷和破裂;XRD分析显示淀粉改性后仍属于A型晶体结构,表明了反应主要发生在无定形区。DSC热分析说明改性后的淀粉糊化温度及糊化焓值均降低;布拉班德粘度分析则表明了改性后的淀粉峰值粘度有很大的提升。     

戊二酸蜡质玉米淀粉酯的制备及理化性质研究

以原蜡质玉米淀粉为原料,戊二酸酐为酯化剂,乙醇为反应溶剂制备戊二酸淀粉酯(EGAS)。采用傅里叶变换红外光谱（FT-IR）、扫描电子显微镜（SEM）、X射线衍射仪（XRD）及布拉班德粘度仪等对样品进行表征及理化性能分析。结果表明：FT-IR显示戊二酸淀粉酯在1730 cm-1处和1565 cm-1处出现了新的吸收峰,其中1730 cm-1处为C=O的伸缩振动吸收峰,1565 cm-1处为游离的-COO-的反对称伸缩振动吸收峰,表明了淀粉分子中成功接入了戊二酸基团;改性前后淀粉的表观形貌变化,证实了反应不仅发生在淀粉颗粒表面,也发生在淀粉颗粒内部;XRD分析显示改性后的淀粉仍属于A型结晶结构,表明了反应主要发生在无定形区;布拉班德粘度分析则表明了改性后的淀粉（DS=0.0450）峰值粘度提高了2.33倍;EGAS的冻融稳定性和抗剪切力均强于原淀粉,糊的透明度得到改善。     

羟丙基戊二酸酯复合改性木薯淀粉的性质分析

以木薯淀粉为原料,利用乙醇溶剂法先进行羟丙基醚化改性,再采用戊二酸酐作酯化剂进行处理而制得复合改性淀粉。采用傅里叶变换红外谱仪（FT-IR）、扫描电镜（SEM）和DV-I Prime旋转粘度仪等对样品的微观结构进行表征及其性能分析。红外分析表明改性淀粉在1287 cm-1处出现羟丙基的吸收峰,羟丙基戊二酸复合改性淀粉在1733 cm-1处和1555 cm-1处出现新的酯化吸收峰,说明原淀粉已接入了羟丙基和戊二酸基团。复合变性前后淀粉的表观形貌变化,证实了反应不仅发生在淀粉颗粒表面,也发生在淀粉颗粒内部。旋转粘度仪分析则表明了复合改性后的羟丙基戊二酸酯淀粉的粘度和抗流变性有很大的提升,当DS为0.0362时,淀粉糊的粘度为12100 mPa?s,比羟丙基木薯的粘度提高了6.72倍（羟丙基木薯淀粉的粘度为1800 mPa?s）。     

离子液体介质中木薯淀粉琥珀酸酯的均相合成

以离子液体(ILs)1-烯丙基-3-甲基咪唑氯盐(AMIMCl)为反应介质,研究无催化剂条件下木薯淀粉琥珀酸酯的均相合成。实验结果表明,将木薯淀粉在105℃的AMIMCl介质中预处理30 min,可使淀粉溶解,表明可利用这种预处理方法将淀粉均相化,作为后续化学改性的反应介质。通过浊度法测定结果表明,木薯淀粉在105℃的离子液体AMIMCl介质中的溶解度为10.2%。在离子液体AMIMCl介质中,通过探讨反应条件对木薯淀粉酯化产物取代度的影响,得到最佳反应条件为:琥珀酸酐与脱水葡萄糖单元(AGU)的摩尔比4:1,反应温度110℃,反应时间3 h,在此条件下,最大取代度为0.518。FT-IR结果显示在1733 cm-1出现了琥珀酸酐的伸缩振动峰,表明淀粉与琥珀酸酐发生了酯化反应,SEM结果表明,所合成的淀粉琥珀酸酯不存在原淀粉的完整颗粒结构,较高取代度的木薯淀粉琥珀酸酯的XRD曲线在2θ为8°处出现弥散峰,表明形成了新的结晶型式。     

辛烯基琥珀酸糊精酯的制备及其乳化性的研究

研究了辛烯基琥珀酸糊精酯的合成工艺以及其乳化性能,并以产品的取代度(DS)为指标,对该酯化工艺的影响因素进行了单因素实验。实验结果表明在OSA添加量为糊精干基3%的条件下,最佳的工艺条件为:麦芽糊精乳质量分数40%,反应体系pH值8.5,反应温度35℃,反应时间5 h;经红外光谱扫描后,产品在1725 cm-1处有C=O伸缩振动吸收峰,在1574 cm-1处有C=C伸缩振动吸收峰;糊精酯可以作为乳化剂应用于饮料乳液的制备,随着DE值的增大,其乳化油滴的能力降低。     

辛烯基琥珀酸大蒜多糖酯的制备

为拓宽大蒜多糖的应用范围,以自制大蒜多糖为原料,与辛烯基琥珀酸酐进行酯化反应后,经纯化获得了辛烯基琥珀酸大蒜多糖酯产品.经其取代度测定和红外光谱鉴定,辛烯基琥珀酸大蒜多糖酯的取代度为0.005,在1 724.05 cm-1处有C=O伸缩振动吸收峰,在2 856.11 cm-1处有饱和亚甲基的对称伸缩振动峰,在1 118.39 cm-1和1 061.41 cm-1处有C-O-C的不对称伸缩振动峰,结果表明,用辛烯基琥珀酸酐酯化大蒜多糖是成功的.     

硬脂酸木薯微晶淀粉酯性质研究及结构表征

采用微晶化和干法酯化制备硬脂酸木薯微晶淀粉酯,研究不同低取代度硬脂酸木薯微晶淀粉酯理化性质,并应用红外光谱和X-射线进行结构表征。结果表明,淀粉经复合改性后,糊粘度明显降低,凝沉性变小,透明度增加,淀粉溶解性、乳化性和乳化稳定性得到较大改善;硬脂酸木薯微晶淀粉酯在3,000～3,700cm-1处羟基伸缩振动吸收峰强度减弱,酯化反应主要发生在淀粉分子结构无定型区。     

甘薯淀粉辛烯基琥珀酸酯物化性质的研究

以甘薯淀粉为参照,采用扫描电镜分析、红外光谱、差示扫描量热分析、快速粘度分析等现代仪器分析方法对甘薯淀粉辛烯基琥珀酸酯的颗粒形貌、结构特征、热力学特性、黏度特性等物化性质进行了测定和研究。结果表明,甘薯淀粉经辛烯基琥珀酸酐酯化后,其颗粒表面出现不同程度的凹陷和破裂,说明酯化反应发生在淀粉颗粒表面;产品的红外光谱在1718 cm-1和1554 cm-1处出现新的吸收峰,其中1718 cm-1处的吸收峰表明酯羰基的存在,说明分子中引入了新的官能团,1554 cm-1处出现的特征峰是缘于RCOO-不对称的伸缩振动;产品的起始糊化温度、峰值糊化温度、糊化结束温度和糊化热焓值降低,说明淀粉结晶结构的致密程度下降;随着产品取代度的增加,淀粉糊峰值粘度升高,出峰时间提前,糊化温度降低。     

微溶剂体系酶法合成松香酸淀粉酯

以松香和木薯淀粉为原料,叔戊醇为溶剂,研究了微溶剂体系下采用酶催化酯化法合成松香酸淀粉酯。通过单因素实验考察了松香与淀粉质量比、反应时间、反应温度、固定化脂肪酶用量对松香酸淀粉酯取代度的影响,确定最适反应条件为:松香与淀粉的质量比为4∶1,反应温度为55℃,反应时间为10 h,固定化脂肪酶用量为4%(以淀粉质量计)。通过红外光谱分析产物的结构发现,产物在1 725 cm-1处出现了酯羰基C=O的伸缩振动吸收峰,表明松香与淀粉发生了酯化反应合成了松香酸淀粉酯;通过X射线衍射分析和扫描电镜分析产物的结构发现,酯化反应没有破坏淀粉原有的晶体型貌和结构。对产物的亲油性能进行研究,结果表明,与原淀粉相比酯化产物在正辛烷中对橄榄油的吸附能力增加了166.67%。微溶剂体系的反应大大降低了成本,提高了产物的量。     

辛烯基琥珀酸芋艿淀粉酯制备及性质研究

以芋艿淀粉为原料,采用湿法制备辛烯基琥珀酸芋艿淀粉酯。以辛烯基琥珀酸淀粉酯取代度(DS)为指标,研究芋艿淀粉浓度、辛烯基琥珀酸酐用量、反应温度、反应时间对辛烯基琥珀酸芋艿淀粉酯制备的影响。在单因素试验的基础上,通过正交试验优化辛烯基琥珀酸淀粉酯制备工艺。结果表明:辛烯基琥珀酸芋艿淀粉酯制备的适宜工艺条件:淀粉质量分数40%、辛烯基琥珀酸酐用量为2.0%芋艿淀粉干重、反应温度40℃、反应时间3 h。在该工艺条件下,制得的辛烯基琥珀酸芋艿淀粉酯颗粒结构发生变化,糊化温度由原淀粉的最高温度85.49℃变为82.15℃,红外光谱图中1 710~1 740 cm-1,1 550~1 610 cm-1区间分别出现酯羰基(C=O)伸缩振动吸收和RCOO-特征吸收,可断定辛烯基琥珀酸与淀粉酯化生成辛烯基琥珀酸淀粉酯。     

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.