强化淀粉类食品中7 种水溶性维生素的快速测定

建立高效液相色谱-二极管阵列-荧光联用法同时检测营养强化淀粉类食品中7 种水溶性维生素含量的方法。样品经淀粉酶60 ℃酶解45 min,调pH值提取后,经十二烷基硫酸钠（5 mmol/L,加入0.1%磷酸,三乙胺调pH 3.0）-乙腈梯度洗脱,VB1、烟酸、烟酰胺在不同波长下进行检测,VB2、吡哆醛、吡哆醇、吡哆胺采用目标物出峰时间段转变激发、发射波长检测。7 种维生素在各自线性范围内线性关系良好,相关系数r2为0.999 6～0.999 9,加标回收率为90.5%～102.5%,检出限为0.01～0.08 mg/100 g,定量限为0.025～0.26 mg/100 g。方法快速、高效,适用于大批量强化淀粉类食品中7 种水溶性维生素的同时测定。     

UPLC-MS/MS分析运动饮料中水溶性维生素

建立一种超高效液相色谱-串联质谱分析运动饮料中VB1、VB2、VB5、VB6、VB7、VB9、VB12、烟酸、烟酰胺、VC10种水溶性维生素的方法。样品前处理用10%乙醇沉淀提取后,采用Waters Atalantis T3色谱柱(2.1 mm×150 mm,3μm)分离,以0.1%甲酸-10.0%甲醇为流动相的梯度洗脱模式下,10种水溶性维生素在10.0 ng/mL~1 000.0 ng/mL浓度范围内线性良好,相关系数r2为0.999 3~0.999 9,检出限范围为0.10μg/kg~11.5μg/kg,定量限范围为0.35μg/kg~38.0μg/kg,加标回收率为90.3%~99.5%,相对标准偏差(RSD)为2.0%~3.6%。     

反相高效液相色谱法测定果醋中的8 种维生素

建立梯度洗脱反相高效液相色谱法同时检测果醋中VC、VB1、VB2、VB3、VB6、VB12、叶酸和烟酰胺8种水溶性维生素的分析方法。考察柱温、缓冲液浓度、pH值以及梯度洗脱程序对各组分分离的影响。最终采用0.1mol/L醋酸钠溶液(pH4.25)和甲醇作为流动相进行梯度洗脱,流速为1.00mL/min,柱温为30℃,8种水溶性维生素在14.2min内达到基线分离;紫外检测波长为266nm和280nm;线性范围：VB2、叶酸为0.05～12.5μg/mL;VC、VB1、VB3、烟酰胺为0.1～25μg/mL;VB6、VB12为0.15～37.5μg/mL,相关系数均在0.999以上,其最低检出限为0.47～3.46ng/mL。该法被成功地用于定量果醋中的维生素,平均加标回收率为92.4%～105.2%,相对标准偏差为0.08%～1.54%。     

鸡胚蛋中水溶性维生素的测定及其孵化期间的变化

对鸡胚蛋中水溶性维生素的色谱测定方法进行优化和验证,5种维生素的加标回收率均在90%以上,且在0.1～50μg/mL具有良好的线性相关性;采用RP-HPLC对不同胚龄(即入孵的第0、2、4、6、8、10、12、14、16和18天)肉鸡胚胎发育过程中的5种水溶性维生素(核黄素、烟酸、烟酰胺、吡哆醇和叶酸)进行测定与分析,并与鲜蛋进行对比。结果表明,随着孵化时间的延长,维生素B2、烟酸和叶酸3种维生素均有不同程度的增加,其中烟酸增加3.2倍,维生素B2增加31%;叶酸在12d达到最高,比鲜蛋约增加1倍;未能检测出维生素B6和烟酰胺。     

反相高效液相色谱 -增敏化学发光测定VB6

基于维生素B6对于鲁米诺(Luminol)和高碘酸钾(KIO4)化学发光反应的增敏作用原理,建立了反相高效液相色谱(RP-HPLC)分离柱后化学发光检测VB6的新方法,并成功运用于饮料中VB6的测定。其中在鲁米诺中加入KBr可以大大增敏该反应。该方法测定VB6的线性范围为5.0×10-7～5.0×10-4g/mL,检测限为2.0×10-8g/mL。对1.0×10-5g/mL的VB6进行连续5次测定的相对标准偏差分别为2.8%,回归方程为Y=954.472X 1.488。     

青藏高原白刺、枸杞和沙棘果粉中水溶性维生素含量比较分析

采用高效液相色谱(HPLC)法对青藏高原白刺、枸杞、沙棘果粉中的7 种水溶性维生素进行分析测定。结果表明：一次提取、分离可同测定7 种水溶性维生素的含量,加标回收率在88.0%～113.4% 之间,相对标准偏差在1.1%～9.0% 之间;3 种果粉的VC、VB1、VB2 含量差异显著,VC 含量高低顺序为沙棘果粉＞白刺果粉＞枸杞果粉,沙棘、白刺果粉VC 含量丰富,分别高达(18266.4 ± 201.1)、(1468.5 ± 24.6)mg/kg;VB1 含量高低顺序为枸杞果粉＞白刺果粉＞沙棘果粉;VB2 含量高低顺序为白刺果粉＞枸杞果粉,而沙棘果粉未检出VB2;VB6、VB12、烟酸、叶酸均没有检出。     

钛胶RP-HPLC法同时测定5 种维生素

采用钛胶反相色谱柱,建立高效液相色谱法同时测定5 种维生素：烟酸、生物素、烟酰胺、叶酸和钴胺素含量的检测方法。研究5 种维生素的保留行为与磷酸缓冲盐pH值、缓冲盐类型及浓度、柱温和流速的关系,得出了最优色谱条件：于波长210 nm处检测生物素和钴胺素,于波长270 nm处检测烟酸、烟酰胺和叶酸,磷酸盐pH 7.0,浓度5.0 mmol/L,柱温50 ℃,流速0.8 mL/min。分析5 种维生素保留的热力学参数焓、熵和吉布斯自由能。烟酸、生物素、烟酰胺、叶酸和钴胺素标准曲线线性良好（R2＞0.999 0）;烟酸、生物素、烟酰胺、叶酸和钴胺素的检出限分别为6、10、20、22、8 ng/mL;5 种物质的相对标准偏差均低于1.36%;加标回收率范围为92.30%～107.20%。方法的精密度和准确度均可满足高效液相色谱法的测定要求。     

HPLC法同时测定婴幼儿配方奶粉中5种水溶性维生素

建立了同时测定婴幼儿配方奶粉中烟酸、烟酰胺、泛酸、维生素B2、维生素B6(包括吡哆醇、吡哆醛和吡哆胺)等5种水溶性维生素的高效液相色谱测定法.采用Zorbax SB-C8(5um,4.6 mm×250mm i.d)反相色谱柱,以质量浓度为1 g/L辛烷磺酸钠:甲醇(95:5,体积比,调pH值为3.0)+乙腈为流动相(梯度洗脱),流速为1.0 mL/min,进样量20μL.方法定量限0.5～5.0 mg/kg,加标回收率91.2%～104.2%,相对标准偏差为0.31%～3.07%.该法具有样品预处理简单,灵敏度高,分析时间短等优点,适用于婴幼儿配方奶粉中上述5种水溶性维生素的同时测定.     

高效液相色谱法测定蔬菜中B族维生素

建立一种使用高效液相色谱与光电二极管阵列检测器(PDA)联用测定蔬菜中七种B族维生素的方法.色谱柱为ZORBAX SB-C18,以甲醇与缓冲溶液(庚烷磺酸钠、冰乙酸、三乙胺、EDTA、异丙醇)作为流动相进行梯度洗脱,设定267nm为检测波长.结果表明:VB1、VB2、VB6、VB12、叶酸、烟酸、烟酰胺的线性范围较宽,平均回收率为92.55%～116.71%,相对标准偏差在0.003%～0.013%,最低检出限能达到mg/kg级.本方法简单、实用,为测定蔬菜中水溶性B族维生素的含量提供了可靠依据.     

HPLC检测黑皮鸡枞菌中的水溶性维生素

研究建立一种简单、快速、可同时检测新鲜黑皮鸡枞菌和菌粉中7种水溶性维生素(维生素C、维生素B_1、维生素B_2、维生素B_6、维生素B_(12)、烟酸和叶酸)的高效液相色谱(high performance liquid chromatographic,HPLC)方法,为黑皮鸡枞菌的深度开发和加工提供科学依据。采用Inertsil ODS-SP(5μm,4.6 mm×250 mm)色谱柱,流动相A为0.05 mol/L的KH_2PO_4溶液(pH=6.0),流动相B为甲醇,流速0.8 mL/min,柱温为室温,检测波长为268 nm,梯度洗脱,反相高效液相色谱,紫外检测器。7种维生素标准曲线的线性相关系数R2在0.999 6～1.000 0之间,相对标准偏差RSD在0.31%～2.17%之间,加标回收率在88.07%～106.01%之间,最低检出限为0.15μg/mL～1.52μg/mL,定量限为0.49μg/mL～5.08μg/mL。利用所建方法检测出新鲜黑皮鸡枞菌中含有4种水溶性维生素,菌粉中含有5种水溶性维生素且都以维生素C和烟酸为主,水溶性维生素总量分别达到22.25μg/g和242.41μg/g。     

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.