应用ICP－MS测定葡萄酒中6种金属元素方法研究

本研究建立了 ICP －MS 在线内标法测定葡萄酒中铁（Fe）、锌（Zn）、铜（Cu）、铬（Cr）、铅（Pb）、锡（Sn）6种重金属元素的方法,采用微波消解对6种元素的前处理方法及ICP－MS工作参数进行了优化。线性范围0～50μg／L 及0～5000μg／L,方法检出限均优于0．2μg／L,回收率在88．6％～109．8％,相对标准偏差RSD均小于6．0％。采用该方法对葡萄酒样品进行了分析,结果表明该方法能够满足重金属痕量检测需求。     

蜂蜜中铅原子荧光光谱测定方法的改进

为改进蜂蜜中的铅的检测方法，用酸性活性炭吸附分离铁氰化钾试剂中铅，以pH计控制消化液的酸度。在最佳的条件下，铅在0．00—40．00μg/L范围内线性良好（r=0．9994）；方法检出限为0．21μg／L；相对标准偏差为4．1％-5．0％；样品加标回收率为93．2％-109．4％。该方法简单，快速，重现性好，灵敏度高，检出限低，结果令人满意。     

氢化物发生-原子荧光光谱法测定酒中痕量铅

为测定酒中的痕量铅建立了痕量铅的断续流动氢化物发生-原子荧光光谱测定方法。采用酸洗活性碳脱铅处理K3Fe（CN）6，使空白值大大下降，改善了方法检出限。对K3Fe（CN）6-KBH4-HCl铅烷发生体系的条件、共存元素的干扰进行了研究，并分别测定了白酒、葡萄酒、啤酒等样品中的痕量铅，加标回收率为98．6％。102．8％，RSD值（n=6）为0．2％-2．9％，方法检出限为0．12μg／L。本法准确、灵敏、简便，完全符合痕量分析要求。     

HPLC同时测定复方丙酸氯倍他索涂膜剂中两组分含量

建立HPLC同时测定复方丙酸氯倍他索涂膜剂中丙酸氯倍他索和水杨酸的含量的方法。方法采用HPLC梯度洗脱色谱分离。色谱柱：Agilent ZORBAX SB-C18柱;流动相4：0．05mol／L磷酸二氢钾（用80％磷酸溶液调节pH2．6）,B：甲醇;流速：1．0mL／mim检测波长：240nm;柱温：室温。结果丙酸氯倍他索、水杨酸的线性范围分别在0．2512-10．048μg／mL（r=0．9999）和10．23～122．76μg／mL（r=0．9999）,平均回收率分别为97．6％,RSD=0．7％（n=6）和96．8％,RSD=0.3％（n=6）。结论该法简单,灵敏,结果准确,可用于复方丙酸氯倍他索涂膜剂的质量控制。     

胶束增溶-流动注射分光光度法测定环境水样中的铜

流动注射胶束增容法测定水环境中的铜，方法简便快速，便于水环境中铜离子的测定。在硼砂盐酸缓冲溶液中，铜与铬天青S以及溴化十六烷基三甲基铵（CTMAB）反应生成黄绿色的络合物，在605nm波长下可以检测。在最佳检测条件下，运用该方法测定铜离子可以得到线性良好且范围广的标准曲线，检测范围为5～40μg／L、40～200μg／L；检测限为0．76μg／L；相对标准偏差为1．59％（n=11）。试验得到的回收率为90．2％～104％。     

流动注射分光光度法测定海水中痕量的镉

建立了在Cd（Ⅱ）-碘化钾-乙基紫高灵敏度显色体系下，采用流动注射分析技术测定海水中痕量镉的新方法，并确定了该方法的最佳条件。线性范围为0．5～12μg／L，相对标准偏差RSD为1.21％（n=11，CCd（Ⅱ）=10μg／L），检出限为0．1μg／L。     

石墨炉原子吸收光谱法测定红葡萄酒中的微量铅

研究了石墨炉原子吸收法测定葡萄酒中微量铅的适宜条件,采用标准加入法和塞曼效应校正背景,铅的线性范围为10μg／L-50μg／L,回收率为90％-110％。并用此法对5种市售红葡萄酒样品进行测定,结果发现铅含量范围为43．50μg／L-91．77μg／L。     

ICP-MS法测定食盐中痕量铅镉砷铬的研究

采用电感耦合等离子体质谱(ICP—MS)法，对食盐中痕量铅镉砷铬进行了分析。对影响其测量的各种因素进行了较为详细的研究，确定了实验的最佳测定条件。结果表明，方法的检出限为：Pb0，003μg／L，Cd0．005μg／L，As0．003μg／L，Cr0．008μg／L，回收率为93．33％-109．52％，RSD小于3.68％。该法准确、快速、简便，应用于食盐中痕量铅镉砷铬的测定，效果满意。     

国外期刊文摘

用在线离子交换富集分光光度流动喷射法测定葡萄酒中的铅Teresal．M．S．LopesetalAnalyst，1996（12）：1047～1050葡萄牙和巴西提出用在线离子交换分光光度法测定葡萄酒中的铅。采用Chelex－100树脂微交换柱（200～400目）富集铅，其色谱反应是基于铅、孔雀绿和碘化物之间生成三元络合物。每小时可处理45个酒样（25～500μg／LPb），结果与用ETAAS法测得的差不多。本法测定精度为RSD＜2．6％，检测限为12pg／L，取样速率为45个／h。（徐小妹，许孙曲）用循环连续液液苹取法测定酒中的酣类化合物E．R．BrhetalAnalyst：1996（121…     

用高效液相色谱法同时测定葡萄酒中4种色素含量方法的研究

为了建立同时测定葡萄酒中喹啉黄、坚牢绿、偶氮玉红（又名酸性红,二蓝光酸性红）和专利蓝等4种色素含量的高效液相色谱方法,采用样品除去乙醇,经水提取和过滤后,使用C18色谱柱（4．6×250mm,5μm）分离,以甲醇和乙酸铵（0．02mol／L）为流动相梯度洗脱,流速为1．0mL／min,二极管阵列检测器检测,波长410nm,柱温30℃。结果显示：4种色素的工作曲线在1．0～50．0μg／mL范围内浓度与峰面积呈良好的线性关系,相关系数r均〉0．999。以S／N=3确定各检出限：喹啉黄为0．23mg／kg,坚牢绿为0．37mg／kg,偶氮玉红为0．29mg／kg,专利蓝为0．15mg／kg。精密度（RSD,n=6）〈3．0％。回收率在91．5％～100．8％。说明该方法干扰小,灵敏度高,分离效果好,操作简便、快速和准确可靠。     

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.