微波辅助消解-固相萃取-氢化物产生-原子荧光光谱联用检测乌龙茶茶叶中无机砷

目的建立微波辅助消解-固相萃取-氢化物产生-原子荧光光谱法测定乌龙茶茶叶中无机砷的分析检测方法。方法以0.06 mol/L HNO_3-3%H_2O_2为消解液,在最大微波功率800 W下,120℃微波消解35 min,提取茶叶中的无机砷,并基于As(Ⅲ)、As(Ⅴ)、一甲基砷(monomethylarsonic acid,MMA)和二甲基砷(dimethylarsinic acid,DMA)解离常数的差异,通过强阴离子交换柱(strong anion exchange cartridge,SAX)实现无机砷和有机砷的有效分离,最后采用氢化物产生-原子荧光光谱法进行无机砷含量测定。结果在0~30μg/L浓度范围内,无机砷的标准曲线方程线性良好(相关性系数r=0.9994),检出限(limit of detection,LOD)为0.208μg/L,样品加标回收率在95.7%~103.6%,相对标准偏差为1.8%~6.8%。结论该方法采用微波辅助消解结合固相萃取提取、分离茶叶中无机砷,具有效率高、成本低、易操作等优点,且可实现乌龙茶茶叶中无机砷高选择性、高灵敏度的分离分析检测。     

聚乙烯亚胺改性硅藻土的制备与表征

采用聚乙烯亚胺(PEI)和十二烷基磺酸钠(SDS),通过浸渍法对硅藻土进行表面改性,研究了硅藻土对PEI的吸附,硅藻土改性后Zeta电位、粒径和形貌特征的变化,以及纸浆中添加改性硅藻土对浆料Zeta电位和滤水性的影响。研究结果表明,PEI能够对硅藻土进行有效改性,与硅藻土相比,PEI改性硅藻土颗粒表面Zeta电位由负电性转变为正电性,粒径增加,当PEI平衡吸附浓度为0.24 mg/m L时,硅藻土颗粒Zeta电位和粒径分别为25.03 m V和14.05μm。PEI改性硅藻土作为造纸填料,可有效提高浆料Zeta电位,并改善浆料滤水性能。     

福建主产乌龙茶中无机砷的分析与风险评价

目的评价乌龙茶中的无机砷含量,并对无机砷的暴露风险进行评估。方法收集春、夏、秋3个季节采摘的8个福建省主栽乌龙茶品种,采用微波辅助消解-固相萃取-氢化物产生原子荧光光谱法(microwave assisted digestion-solid phase extraction-hydride generation-atomic fluorescence spectrometry,MAD-SPE-HG-AFS)测定其无机砷含量并进行无机砷暴露风险评估。结果乌龙茶中无机砷的含量在0.037~0.050 mg/kg之间,平均含量为0.043 mg/kg,其中秋季采摘的武夷水仙茶叶中的无机砷含量最高。方差分析结果表明,不同季节采摘的乌龙茶中无机砷含量差异不显著,而同一季节不同乌龙茶品种中无机砷含量存在显著差异。依据美国环境保护署(United States Environmental Protection Agency,USEPA)规定的每日无机砷摄入限量(reference dose,RfD=0.3μg·(kg·bw)~(-1)·d~(-1))评价表明,人体通过乌龙茶无机砷的每日暴露量(estimated daily intake,EDI)为6.80E-07~9.19E-07 mg/(kg·d),乌龙茶中无机砷含量的危害商值(hazard quotient,HQ)值均小于1。结论福建省主栽乌龙茶品种中无机砷含量低,通过摄入乌龙茶导致消费者无机砷暴露的风险极低。     

高效液相色谱-电感耦合等离子体质谱法测定婴幼儿谷类辅助食品中无机砷及其他砷形态

目的 建立高效液相色谱-电感耦合等离子体质谱法测定婴幼儿谷类辅助食品中无机砷及其他砷形态的分析方法。方法 婴幼儿谷类辅助食品经0.15 mol/L硝酸溶液提取后, 采用阴离子分析柱, 以不同浓度的碳酸铵溶液作为流动相进行梯度洗脱分离, 用高效液相色谱-电感耦合等离子体质谱进行定性和定量分析。 结果 建立的5种砷形态分析方法在0~100 μg/L范围内具有良好的线性关系, 相关系数r>0.999, 加标回收率在89.0%~110.0%, 相对标准偏差(relative standard deviation, RSD)<5%。婴幼儿谷类辅助食品中砷形态以无机砷为主, 在调查的样品中无机砷的含量均远低于国家食品标准的限量。结论 该方法简便、准确, 适用于婴幼儿谷类辅助食品中无机砷及其他砷形态的测定及食品安全的实际监测。     

卷烟主流烟气中无机态As(Ⅲ)和As(Ⅴ)的形态分析

为更全面深入地评价卷烟烟气中砷的危害,建立了一种砷形态分离测定方法。用超声溶剂提取剑桥滤片捕集的卷烟主流烟气中的砷,AB-8 大孔吸附树脂分离有机态和无机态砷,717 强碱阴离子交换树脂进一步分离无机态中的As(Ⅲ) 和As(Ⅴ)。对影响As(Ⅲ) 和As(Ⅴ) 分离的实验条件进行了研究,并确定了较佳分离条件。考察了分离方法的精密度和回收率,结果表明:该方法相对标准偏差(RSD,n=6)3.5%-4.7%,无机态砷加标回收率90.6%-102.4%。检出限和定量限分别为0.013μg/L 和0.043μg/L。该方法准确、可靠,可有效地用于卷烟主流烟气中砷的形态分析。      

聚电解质层间自组装对OCC浆强度及纤维表面性能的影响

研究CPAM/CMC两种聚电解质层间自组装对废旧瓦楞纸(OCC)浆强度性能的影响,对层间自组装过程中浆料的Zeta电位变化进行了测试,并借助扫描电镜(SEM)和傅里叶红外光谱(FT-IR)对吸附聚电解质的OCC纤维表面进行了分析。结果表明,CPAM/CMC自组装对纸页的增强效果较好,裂断长、耐折度及环压指数分别提高了82.82%、550.00%、92.88%,浆料滤水时间减少,滤水性能明显改善。浆料Zeta电位随聚电解质自组装层数的增加而不断变化,表明纤维表面自组装过程源于阳离子和阴离子聚电解质的静电作用力。SEM、FT-IR表征显示,纤维表面确实吸附有聚电解质复合物。     

pH值、无机电解质对PAE和CMC在纤维上吸附量的影响

通过测量纸浆Zeta电位以及聚合电解质的吸附量等方法,研究了pH值和无机电解质对阳离子聚酰胺-环氧氯丙烷树脂(PAE)和阴离子羧甲基纤维素(CMC)在纤维表面吸附量的影响。实验结果证明吸附量随纸浆悬浮液中无机电解质浓度的升高先增大后减小;随pH值的升高而增大。     

L-半胱氨酸修饰的Au／Fe_3O_4磁性复合粒子的制备及其对牛血清蛋白的吸附性能

采用L-半胱氨酸在Fe_3O_4表面键接Au纳米粒子的方法,制备了L-半胱氨酸修饰的Au／Fe_3O_4磁性复合粒子（LC—Au／Fe_3O_4）,并将其用于吸附牛血清蛋白（BSA）．通过紫外可见分光光度计、x-射线衍射仪、傅里叶红外光谱仪、扫描电镜、透射电子显微镜、Zeta电位仪对样品的光学性质、结构形貌、稳定性进行表征,结果表明：复合粒子中的Fe_3O_4具有尖晶石结构,粒径在200nm左右,稳定性较好．对BSA的吸附实验结果表明：LC—Au／Fe304的BSA单位吸附量达到161．5mg／g．     

高效液相色谱-电感耦合等离子体质谱法测定大米中无机砷

摘要：目的 建立高效液相串联电感耦合等离子体质谱法测定大米中无机砷的分析方法。方法 样品经0.15mol/L硝酸溶液提取,以100 mmol/L (NH4)2CO3为流动相,使用AS7 阴离子交换柱(250 mm×4.0 mm, 10 μm)分离,进入质谱进行检测。结果 As（Ⅲ）和As（Ⅴ）在浓度0~100ng/mL范围内线性相关性良好,精密度RSD均小于5%,检出限为0.234ng/mL~0.904ng/mL,加标回收率在89.7%~108.0%之间,能力验证和质控样结果较好。结论 此方法适用于大米中无机砷的快速检测。     

云南地区茶叶中总砷及无机砷含量调查分析

目的为云南茶叶的开发利用提供数据支持。方法利用国家标准方法对云南省110份茶叶样品的总砷和无机砷含量进行测试,并就产地、包装、流通环节等进行调查分析。结果经对采集的110个茶叶样品进行总砷检测,最高0.152 mg/kg,均值0.0325 mg/kg,仅1件检出无机砷,检测值为0.0591 mg/kg,均符合国家相关标准要求。总砷残留量在生熟茶和包装形态上的分布存在统计学差异,但不同原料来源地和不同品种上总砷残留量分布无统计学差异。总砷和无机砷残留量在分布上无相关性。结论云南省茶叶中总砷和无机砷含量属于较低水平,说明云南省茶叶生产有环境优势,砷含量整体控制在安全水平。     

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.     

Chlorohydrins of bisphenol A diglycidyl ether (BADGE) and of bisphenol F diglycidyl ether (BFDGE) in canned foods and ready-to-drink coffees from the Japanese market

BADGE.2HCl and BFDGE.2HCl were determined in 28 samples of ready-to-drink canned coffee and 18 samples of canned vegetables (10 corn, 5 tomatoes and 3 others), all from the Japanese market. HPLC was used as the principal analytical method and GCMS for confirmation of relevant LC fractions. BADGE.2HCl was found to be present in one canned coffee and five samples of corn, BFDGE.2HCl in four samples of canned tomatoes and in one canned corn. No sample was found which exceeded the 1mg/kg limit of the EU for the BADGE chlorohydrins. However the highest concentration was found for the sum of BFDGE.2HCl and BFDGE.HCl.H₂O at a level of 1.5mg/kg. A Beilstein test confirmed that all cans containing foods contaminated with BADGE.2HCl or BFDGE.2HCl had at lest one part coated with a PVC organosol.     

European priorities for research to support legislation in the area of food contact materials and articles

A strong science base is required to underpin the planning and decision-making process involved in determining future European community legislation on materials and articles in contact with food. Significant progress has been made in the past 5 years in European funded work in this area, with many developments contributing to a much better understanding of the migration process, and better and simpler approaches to food control. In this paper this progress is reviewed against previously identified work-areas (identified in 1994) and conclusions are reached about future requirements for R&D to support legislation on food contact materials and articles over the next 5 or so years.     

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.     

Influence des ions sur le pouvoir hydratant de l'ure e: e tude sur peau de porc ex vivo

This study deals with the influence of ions (NaCl and MgSO4) in a W/O emulsion containing 10% urea. Moisturization kinetics are assessed by corneometry on pig skin ex vivo. The formula's influence on urea penetration is measured by infrared spectrometry with an ATR device and the stripping method. Corneometry and spectroscopy were chosen to record simultaneously the hydratation levels and urea localization into superficial cell layers. Urea crystallization after evaporation of emulsions and aqueous solutions is described. Results show that urea does not hydrate nor penetrate when applied to the skin through an aqueous gel. In a W/O emulsion, sodium chloride increases the ability of urea to moisturize without improving penetration. In vitro urea crystallization is disturbed by sodium chloride or magnesium sulphate for solutions and emulsions. This stabilization by ions is correlated with good moisturization values. The stabilization of urea in the solute state provided by ions increases its water epidermal binding capacity without enhancing penetration.     

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 on Economic Indicators from 62 Enterprises in Printing Machinery Industry in Q1 2014

Operation of printing machine industry was still unsatisfactory in the first quarter of 2014.Analysis on operation of printing machine industry.a.Market demand was not strong;sales of product undulated and declined.According to the statistics,the total industrial output value fell by 19.28% in the first quarter of 2014 than the average quarter value in 2013; industrial added value decreased by 4.16%; sales revenue dropped by 22.83%. h. Business operation of enterprises was in poor condition. c. R＆D of new products is an important transformation guarantee for enterprises. d. To take self explore new ways upgrading advantages,and explore new ways.