Pd/C催化下麦草碱木质素与氢气的还原反应

以钯/炭(Pd/C)为催化剂,以氢气为还原剂与麦草碱木质素进行反应,分析了不同反应条件对催化效果的影响,用化学法测定了反应前后碱木质素官能团的含量,并与环己烯还原法进行了比较。结果表明,在Pd/C催化剂负载量为3%、用量0.1g/g、氢气流速20mL/min、反应温度363K、反应时间3h的条件下,反应后碱木质素的总羟基、酚羟基、醇羟基含量分别为14.39%、4.21%和10.18%,较反应前分别增加了133.68%、27.96%和264.87%。与环己烯法相比,氢气还原法的催化剂用量明显减少,醇羟基数增加较为显著,酚羟基含量基本一致。氢气还原活化效果明显优于环己烯还原效果。     

CuO/C催化还原碱木质素的化学结构特征

用等体积浸渍法制备CuO/C催化剂,采用FTIR、UV、1H-NMR光谱和HPLC色谱,分析了以CuO/C为催化剂,以环己烯为还原剂对麦草碱木质素进行催化,研究了碱木质素的化学结构变化。红外光谱表明,还原碱木质素的总羟基(酚羟基和醇羟基)含量增加,羰基含量减少,芳环稳定;1H-NMR光谱证实,还原碱木质素的羰基质子数呈下降趋势,羰基被还原为羟基;酚羟基和醇羟基质子数增加;高效凝胶渗透色谱分析表明,还原碱木质素的数均分子质量有所增加、重均分子质量减少,活化碱木质素的多分散性小于碱木质素的多分散性。CuO/C催化剂对木质素还原反应具有明显的催化作用,其化学结构发生了改变,活性官能团增加,苯环结构稳定,木质素的反应活性提高。     

钯/炭(Pd/C)催化氢还原碱木质素的抗氧化性能

以工业碱木质素为原料,采用购买和自制两种钯/炭(Pd/C)为催化剂,氢气为还原剂,在高压条件下对其进行还原反应,提高碱木质素的活性,并对其反应前后化学成分和抗氧化性能进行分析。结果表明：经过两种催化剂高压催化活化后,购买催化剂还原碱木质素醇羟基含量为5.01%,酚羟基含量为3.64%。自制催化剂还原碱木质素醇羟基含量为5.35%,酚羟基含量为3.82%。自制Pd/C催化剂催化体系的催化效果优于购买Pd/C催化剂;在抗氧化性能分析实验中,碱木质素原料及两种被还原碱木质素在质量浓度范围为0.025～0.6mg/mL内对DPPH自由基和·OH均有较强的清除能力,且随着木质素质量浓度的增加,清除率逐渐增加,还原力也增强,两种被还原碱木质素DPPH自由基最大清除率分别达到80.91%和82.43%;·OH最大清除率分别达到23.12%和26.21%。     

钯/炭催化剂对碱木质素还原反应的催化作用

采用甲醛还原法制备钯/炭(Pd/C)催化剂,考察了以Pd/C为催化剂,以环己烯为氢给予体的催化体系对麦秆碱木质素还原反应的催化作用,用化学法对反应前后碱木质素官能团进行了定量测定,用FTIR、UV和1H NMR光谱对木质素化学结构进行了分析.结果表明,Pd/C催化剂对碱木质素还原反应具有较高的催化活性,碱木质素总羟基含量增加了46.95%,酚羟基含量增加了33.74%,醇羟基含量增加了63.93%;甲氧基含量降低了17.73%,羧基含量降低了53.41%,总酸性基变化不大,木质素的苯环结构稳定,活性官能团增加,反应活性提高,PdC催化剂对木质素还原活化反应具有良好的催化作用.     

Pd/C催化下碱木质素与环己烯的还原反应

以钯/炭(Pd/C)为催化剂,以环己烯为氢给予体与麦秆碱木质素进行还原反应,分析了不同因素对反应过程的影响,通过正交实验优化了反应参数,用化学法对反应前后碱木质素官能团进行了定量测定,实验结果表明,最佳的Pd/C催化、环己烯还原法活化碱木质素的反应条件为:pH值10,催化剂质量分数7%,反应时间1.5h,碱木质素与环己烯质量比1:4.1,反应后碱木质素的总羟基含量为13.45%,增加了104.72%;羧基含量为1.60%,降低了39.39%;羰基2.96%,降低了50.99%.凝胶渗透色谱(GPC)分析表明,对于反应前后的碱木质素,其相对分子质量主要在1000～10000之间,所占比例分别为63.23%、84.66%,经Pd/C催化还原后碱木质素的多分散系数变小.     

利用H_nXW_(12)O_(40)催化降解碱木质素工艺的研究

利用具有Keggin结构的HnXW12O40（n=3时,X=P;n=4时,X=Si）对工业碱木质素进行催化降解,采用紫外分光光度法和乙酰化结合电位滴定法测定了降解活化后碱木质素的酚羟基和总羟基含量,分别研究了反应温度、反应时间、催化剂用量和溶剂体系等因素对催化降解后碱木质素羟基含量的影响,确定了HnXW12O40降解碱木质素的最佳工艺条件。同时对降解机理进行了初步探讨。     

不同氧化剂对禾草类碱木质素结构变化的影响

研究了禾草类碱木质素在O2、H2O2、O3、O2/H2O2、O3/H2O2等不同氧化剂氧化时其结构的变化规律,为更好地利用禾草类碱木质素提供理论依据和工艺方法。研究结果表明,以O2/H2O2氧化禾草类碱木质素时,高用碱量可促进木质素高分子组分氧化降解,分子质量均一化,酚羟基和羧基增加较多,脱甲氧基反应也较强烈;低用碱量时,木质素氧化降解少,并伴有缩合反应;H2O2可促进碱木质素氧化降解,促进酚羟基、羧基的产生和脱甲氧基反应;在O3氧化适宜条件下,添加H2O2可使O3氧化反应缓和,木质素分子发生缩合并均一化,生成较多的酚羟基、羧基和羰基。     

愈创木基型和紫丁香基型木素小分子的漆酶生物改性

从松柏醇、紫丁香醇模型物的角度人手,通过气相色谱-质谱联用(GC-MS)、凝胶渗透色谱(GPC)、红外光谱和颗粒电荷等测试手段,综合考察了漆酶对松柏醇、紫丁香醇生物改性的机理.松柏醇、紫丁香醇经漆酶处理后,GC-MS检测不到小分子单体的存在,推测两者都参与了化学反应.GPC分析证明,松柏醇和紫丁香醇漆酶处理后分子质量变大,发生了聚合.红外光谱确定了松柏醇漆酶处理过程中反应位点,主要是酚羟基、苯环上的甲氧基、苯环侧链上的双键,β碳、γ碳也有可能参与了反应,紫丁香醇反应位点是酚羟基、苯环上的甲氧基.产物苯环相应吸收峰强度和面积增加,有新的芳基醚键产生,说明苯环以醚键方式连接而聚合.漆酶处理后松柏醇、紫丁香醇阳离子需求量分别下降了88.4%,87.4%.     

酚化改性蔗渣硫酸盐木素制备酚醛树脂胶黏剂

本研究以蔗渣硫酸盐木素(KL)为原料,在酸性条件下对KL进行酚化改性,通过单因素实验和正交实验优化反应条件。以酚化改性硫酸盐木素(P-KL)酚羟基含量为响应值,确定最佳反应条件为:苯酚∶木素(质量比)=4∶1,催化剂(质量分数98%浓硫酸)用量4%,反应时间2. 5 h,反应温度110℃。利用凝胶渗透色谱(GPC)表征硫酸盐木素酚化改性前后相对分子质量的变化,结果表明,与KL相比,P-KL相对分子质量减小、分布变窄,酚羟基含量增加。分别用P-KL和KL代替质量分数60%的苯酚制取木素基酚醛树脂胶黏剂P-KLPF和KLPF。结果表明,P-KLPF中游离甲醛和游离酚含量均小于KLPF胶黏剂。由此可知,酚化改性能显著提高硫酸盐木素与甲醛的反应活性,降低木素基酚醛树脂胶黏剂中游离甲醛及苯酚的释放量。     

丝素与一氯均三嗪型活性染料反应性的HPLC研究

用异丙胺、对甲酚和甲醇分别模拟蚕丝丝素上氨基、酚羟基和醇羟基,应用高效液相色谱(HPLC)研究一氯均三嗪型活性染料与蚕丝亲核基团的反应性能。结果表明,一氯均三嗪型活性染料与蚕丝上不同亲核基团的反应性能不同,酚羟基在85℃左右,pH值为8~9的条件下最佳,氨基在95℃,pH值为9左右较好,而醇羟基更适合碱性较强的反应条件。结合亲核基团分布状况及含量可以推断,一氯均三嗪型活性染料适宜在pH值为8~9和85~95℃下对蚕丝染色,在此条件下,一氯均三嗪型活性染料主要与蚕丝上的酚羟基反应,氨基起次要作用,而醇羟基的作用甚微。     

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.     

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.     

低温带皮菜籽粕微粉的不同粒级部分的功能特性

为研究低温带皮菜籽粕微粉的不同粒级部分的功能特性,以经低温脱脂的带皮菜籽粕为原料,经微粉碎后筛分成212~425μm、150~212μm和106~150μm的3个不同粒级的微粉样品,检测这些样品的吸水性、吸油性、乳化性和乳化稳定性、蛋白质体外消化率。结果表明:1 3个不同粒级的微粉样品之间的粗纤维含量存在显著差异,表明三者的结构组成成分有一定差异。23个微粉样品的乳化活性和乳化稳定性随粒度级别的减小而显著增加(P0.01)。33个微粉样品的蛋白质体外消化率随粒度级别的减小而显著增加(P0.01)。4不同粒级带皮菜籽粕微粉样品的吸水性与吸油性受其结构组成物质不同和粒度的双重影响,与粒度的相关性不明显。     

Microbiology of food taints

Fresh and processed foods are often spoilt by the presence of undesirable flavours and odours caused by microbial action. The aim of this paper is to review the current knowledge of microbiologically induced taints that occur in a wide range of foodstuffs, including meats, poultry, fish, crustaceans, milk, dairy products, fruits, vegetables, cereals and cereal products. Examples have been chosen where the compounds responsible for the taint have been identified and sufficient data obtained to demonstrate the involvement of microorganisms. However, in some cases the full identity of the causative organism may not have been elucidated. The types of microorganisms covered by this review include bacteria, fungi, yeasts, actinomycetes and cyanobacteria. Although cyanobacteria do not in general infect foods, their presence in aqueous systems and water supplies can lead to off-flavours in aquatic organisms and processed foodstuffs. Several examples of each of these processes are discussed. Wherever possible, the likely biosynthetic pathway used by the microorganism to produce the offending compound in a foodstuff is indicated.     

Analysis for organic residues from aids to polymerization used to make plastics intended for food contact

Polymers intended for food contact use have been analysed for organic residues which could be attributed to a range of substances employed as polymerization aids (e.g. initiators and catalysts). A wide range of polymers was extracted with solvents and the extracts analysed by gas chromatography-mass spectrometry (GC-MS). The overwhelming majority of substances identified were not derived from aids to polymerization but were oligomers, additives and adventitious contaminants. However, a small number of substances were identified as initiator residues. These included tetramethylsuccinonitrile (TMSN) which was observed in two polymers and it derived from recombination of two azobisisobutyronitrile (AIBN) initiator radicals. Methyl benzoate, benzoic acid, biphenyl and phenyl benzoate were detected in one poly(methyl methacrylate) sample and in two polyvinylchlorides and they are thought to be derived from benzoyl peroxide initiator. TMSN was subsequently targeted for analysis of poly-(methyl methacrylate) plastics using proton nuclear magnetic resonance spectrometry (¹     

Tests of potential functional barriers for laminated multilayer food packages. Part II: Medium molecular weight permeants

Experiments were performed to characterize the kinetics of the permeation of different medium molecular weight model permeants: bisphenol A, warfarin and anthracene, from liquid paraffin, through a surrogate potential functional barrier (25 microns-thick orientated polypropylene--OPP) into the food simulants olive oil and 3% (w/v) acetic acid. The characterization of permeation kinetics generally observed the permeation models previously reported to explain the experimental permeation results obtained for a low molecular weight group of model permeants. In general, the model permeants exhibited behaviour consistent with their relative molecular weights with respect to (a) the time taken to attain steady-state permeation into the food simulant in which they were more soluble, (b) their subsequent steady-state permeation rates, and (c) their partition between liquid paraffin and the OPP membrane.     

The development of reference materials for paralytic shellfish poisoning toxins in lyophilized mussel. I: Interlaboratory studies of methods of analysis

This paper describes the first part of a project undertaken to develop mussel reference materials for Paralytic Shellfish Poisoning (PSP) toxins. Two interlaboratory studies were undertaken to investigate the performance of the analytical methodology for several PSP toxins, in particular saxitoxin (STX) and decarbamoyl-saxitoxin (dc-STX) in lyophilized mussels, and to set criteria for the acceptance of results to be applied during the second part of the project: the certification exercise. In the first study, 18 laboratories were asked to measure STX and dc-STX in rehydrated lyophilized mussel material and to identify as many other PSP toxins as possible with a method of their choice. In the second interlaboratory study, 15 laboratories were additionally asked to determine quantitatively STX and dc-STX in rehydrated lyophilized mussel and in a saxitoxin-enriched mussel material. The first study revealed that three out of four postcolumn derivatization methods and one pre-column derivatization method sufficed in principle to determine STX and dc-STX. Most participants (13 of 18) obtained acceptable calibration curves and recoveries. Saxitoxin was hardly detected in the rehydrated lyophilized mussels and results obtained for dc-STX yielded a CV of 58% at a mass fraction of 1.86 mg/kg. Most participants (14 out of 18) identified gonyautoxin-5 (GTX-5) in a hydrolysed extract provided. The first study led to provisional criteria for linearity, recovery and separation. The second study revealed that 6 out of 15 laboratories were able to meet these criteria. Results obtained for dc-STX yielded a CV of 19% at a mass fraction of 3.49mg/kg. Results obtained for STX in the saxitoxin-enriched material yielded a CV of 19% at a mass fraction of 0.34mg/kg. Saxitoxin could not be detected in the PSP-positive material. Hydrolysis was useful to confirm the identity of GTX5 and provided indicative information about C1 and C2 toxins in the PSP-positive material. The methods used in the second interlaboratory study showed sufficiently consistent analysis results to undertake a certification exercise to assign certified values for STX and dc-STX in lyophilized mussel.     

The Ministry of Environmental Protection Issued "Feasible Technology Guidelines for Pollution Prevention and Control in Wood Pulping Process of the Paper Industry (Trial)" and Two Other Guiding Technical Documents

On December 27t＂, 2013, the Ministry of Environmenta Protection announced that, in order to implement ＂The Environmental Protection Law of the People＇ s Republic of China＂, improve the working system in environmenta protection technologies, and promote technologica advancement in pollution prevention, the Ministry of Environmental Protection sponsored the formulation of three guiding technical documents including ＂Feasible Technology Guidelines for Pollution Prevention and Contro n Wood Pulping Process of the Paper Industry （Trial）＂     

1~(st) Intelli-Tissue~ EcoEc Tissue Machine Supplied by PMP Group Successfully Put into Operation in China

正On April 29th,2014,Intelli-Tissue EcoEc tissue machine supplied by PMP Group successfully put into operation at Hebei Xuesong Paper Co.,Ltd.,this is the first such kind of paper machine of PMP Group in China.