基于HPLC-DAD的多波长指纹图谱构建及其在烟用香精质量评价中的应用

为评价烟用香精质量稳定性，采用240、254、278、330和360 nm 5波长同时监测技术，通过对各单波长下色谱峰选择建立了烟用香精HPLC全时段多波长综合指纹图谱分析方法，同时经与夹角余弦法等4种方法进行对比，探讨了适用于烟用香精指纹图谱相似度评价的算法，并结合感官评价拟定了31种烟用香精质量稳定性判定的相似度阈值。结果表明：(1)全时段多波长综合指纹图谱能够更全面地反映烟用香精的内在质量信息。(2)改进的Nei系数法更适合于烟用香精指纹图谱相似度评价。(3)拟定的31种烟用香精的相似度阈值能够用于各自的质量稳定性判定。该方法准确度高，可用于烟用香精的质量监控。     

咸味香精的气相指纹图谱及质量评价研究

采用固相微萃取法提取香精的挥发性成分,应用气相色谱技术进行分析,研究了咸味香精挥发性组分的气相指纹图谱的分析方法,并同时分析了气相指纹图谱用于咸味香精质量控制的可行性．结果表明：咸味香精挥发性组分指纹图谱稳定性好,相似度高,具有较强的特征性和唯一性．该图谱能综合、准确地反映咸味香精的风味情况,是一种有效的咸味香精质量控...     

主成分分析法在烟用香精质量控制中的应用

为了快速有效地控制不同批次烟用香精的质量,采用同时蒸馏萃取-GC/MS法对同种香精6个不同批次、掺兑不同比例[5%、10%、15%、20%、25%、30%、35%、40%(质量分数)]其他香精、不同比例[5%、10%、15%、20%、25%、30%、35%、40%(质量分数)]乙醇稀释及其他2种不同种类的香精样品的挥发性成分进行了分析,通过计算所有色谱峰的相对保留值和相对峰面积建立了香精样品的指纹图谱,并通过指纹图谱的主成分分析(PCA)和投影分析对样品进行模式识别.结果表明:PCA投影法能区分掺兑5%其他香精或5%乙醇稀释的样品.PCA投影法可以作为烟用香精质量控制的一种有效手段.     

苦瓜皂苷高效液相色谱指纹图谱研究

建立苦瓜皂苷类成分的高效液相色谱法(HPLC)指纹图谱.采用中药色谱指纹图谱相似度评价系统,对不同产地苦瓜中皂苷进行HPLC分析,流动相:乙腈和水梯度洗脱;流速:1.0mL/min;色谱柱:ZorbaxSB-C18柱(150×4.6mm,5 μm);柱温:25℃;检测波长:209 nm;进样量:20 μL;分析时间:65 min.确定8个共有峰作为苦瓜皂苷的特征指纹峰;不同产地苦瓜皂苷指纹图谱与对照指纹图谱(R)的相似度均大于0.85.该方法建立的苦瓜皂苷HPLC指纹图谱,为苦瓜鉴别和品质评价、质量控制、制定质量标准提供参考.     

白芷HPLC指纹图谱的研究

目的建立白芷的高效液相色谱(HPLC)指纹图谱。方法采用HPLC,色谱柱:Agilent C18(250mm×4.6 mm,5μm),梯度洗脱,流动相A为0.01%三氟乙酸水溶液,流动相B为甲醇,流速1.0 ml/min,柱温30℃,检测波长300 nm,建立了21批白芷的HPLC指纹图谱。结果与结论本研究建立的指纹图谱可较好地反映白芷的质量,可为其质量控制提供参考。     

HPLC测定亚麻荠种子中芦丁及指纹图谱研究

为更好地评价亚麻荠种子的质量,采用HPLC测定12批亚麻荠种子的芦丁含量,并建立了亚麻荠种子的HPLC指纹图谱,通过TCMYS指纹图谱软件对不同产地亚麻荠种子指纹图谱进行相似度分析。结果表明,HPLC测定芦丁的标准曲线回归方程线性关系良好（r=0.999）,平均加标回收率为99.37%,12批亚麻荠种子指纹图谱相似度较高,标定16个共有峰。HPLC指纹图谱方法稳定性及重复性良好,可为亚麻荠种子的质量评价及质量控制提供依据。     

山东省道地药材金银花的质量控制研究

利用高效液相色谱和核磁哭振波谱仪测定了金银花提取物的HPLC和^1HNMR图谱，对金银花提取物的HPLC图谱进行了比较，结果表明金银花提取物的HPLC指纹图谱有很好的相似性；对金银花提取物的^1HNMR指纹图谱研究表明，金银花含有其主要有效成分绿原酸的特征峰，同时金银花提取物的^1HNMR指纹图谱也有很好的相似性，并具有很好的重现性和高度的特征性。金银花提取物的HPLC和^1HNMR指纹图谱可以作为金银花鉴定的相对标准图谱和数据，作为金银花质量鉴别的依据。     

川渝地区金银花HPLC指纹图谱的研究

采用HPLC法测定十个不同商品来源的金银花样品,建立川渝地区金银花药材甲醇溶解部分的HPLC指纹图谱,为科学评价与有效控制金银花质量提供新方法。色谱条件为C18柱,甲醇-1%磷酸为流动相进行梯度洗脱,检测波长237nm,体积流量1.0mL/min,柱温30℃。结果表明,该方法能够很好地分离川渝地区金银花的主要成分;不同产地金银花药材指纹图谱相似度较好,建立了含有11个特征指纹峰的川渝地区金银花标准指纹图谱;HPLC标准指纹图谱具有良好的重现性和特征性。     

色谱指纹图谱在烟用香精质量控制中的应用

采用同时蒸馏萃取法提取6批次的烟用HMT-2香精成分,GC/MS分析,建立了该香精的GC/MS指纹图谱。利用夹角余弦法和欧氏距离法计算相似度,并通过掺兑试验考察色谱指纹图谱用于烟用香精质量控制的可行性。结果表明:①6批次的HMT-2香精指纹图谱稳定性好,相似度高,具有很强的特征性和唯一性;②夹角余弦法和欧氏距离法计算简单,易于编程,二者结合能够全面考察香精的质量。色谱指纹图谱能全面、综合、准确地反映烟用香精的质量状况,可以成为烟用香精质量控制的有效手段。     

烟用香精UPLC指纹图谱的夹角余弦、相关系数与欧氏距离评价

以Acquity UPLC TMBEHC C18柱作色谱柱,硝基苯为内标,乙腈-0.1%甲酸水溶液为流动相,检测波长254nm,采用超高效液相色谱(UPLC)法测定了10种烟用香精6批次样品、稀释品和掺兑品,而后采用相对保留值和相对峰面积法对所有成分的保留时间和色谱峰进行处理,建立了烟用香精UPLC指纹图谱,再用夹角余弦、相关系数与欧氏距离法对UPLC指纹图谱进行处理,并通过比较各批次香精样品的夹角余弦、相关系数与欧氏距离接近程度评价这些香精质量的稳定性。结果表明:夹角余弦、相关系数和欧氏距离都能够在一定程度上反映出烟用香精的质量变化,而夹角余弦和相关系数的差异不大,且比较相似,但在小量浓度变化上表现不明显,而欧氏距离则能反映香精浓度和种类的变化。     

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.