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％。     

固相萃取-高效液相色谱法测定黄酒中氨基甲酸乙酯

建立一种反相高效液相色谱法测定黄酒中氨基甲酸乙酯的方法。样品经固相萃取柱净化后衍生,采用反相C18色谱柱XB—Cfsf4．6mm×250mm,5μm）,以乙腈-0．02moL／L乙酸纳水溶液为流动相进行梯度洗脱,流速为lmL／min;设定荧光检测器中激发波长为233nm,发射波长为600nm,对黄酒中的氨基甲酸乙酯进行检测。结果表明,在50．0-250．0μg／L添加量范围内,平均回收率为92．9％,相对标准偏差为4．5％（n=6）。方法的检出限为10μg／L,线性范围为100～1500μg／L（R=0．9995）,测定结果与标准气相色谱一质谱法基本相同。所建立的方法可以作为黄酒中氨基甲酸乙酯的检测方法。     

固相萃取法在检测饲料中叶酸、VB12的应用

样品用提取液提取,经C18小柱富集、净化后,进行HPLC分离、检测。所使用的色谱柱为UllimatexB—C18,紫外检测波长分别为271nm（叶酸）,365nm（VB12）,流动相为1g／L辛烷磺酸钠＼甲醇,梯度洗脱。该方法回收率为96．7％-97．2％,相对标准偏差（RSD）为1．8％-2．4％（n=6）,线性范围为0．25μg／m-25μg／m,r=0．9999,叶酸检出限为0．1mg／kg,VB12检出限为0．2mg／kg。     

催化动力学光度法测定食品中的痕量钒

基于0．02mol／L的H2SO4介质中，痕量钒（V）对次磷酸钠还原偶氮胂I（AsA I）的褪色反应有明显的阻抑作用，建立了测定痕量钒（V）的动力学光度法。方法检出限为0．052μg／L，线性范围为0～4．0μg／L。用于测定大米、条叶、面粉样品中的痕量钒（V），结果满意。     

溴酸钾氧化二甲基黄动力学光度法测定食品中的痕量硒(Ⅳ)

基于0．004mol／L的HNO3介质中，在乳化剂OP存在时，痕量硒（Ⅳ）催化溴酸钾氧化二甲基黄的褪色反应，建立了测定痕量硒（Ⅳ）的催化光度法。方法检出限为0．015μg／L，线性范围为0～0．8μg／L，加标回收率为98．0％～102．5％，样品测定的相对标准偏差（RSD）为2．6％～7．2％。用于测定食品中的痕量硒（Ⅳ）时，结果满意。     

高效液相色谱荧光法测定营养素补充制剂中维生素K2(MK-7)的含量

建立高效液相色谱荧光法（HPLC-FLD）测定营养素补充制剂中维生素K2（MK-7）的含量。样品用异丙醇超声提取30 min，提取液离心过滤后取样液10 μL注入液相色谱系统中。样液经安捷伦C18色谱柱(4.6 mm×150 mm，5 μm)或其他等效色谱柱分离，柱后采用锌粉还原柱（4.6 mm×50 mm）衍生，使样品中维生素K2（MK-7）具有荧光特性。以甲醇（含5%四氢呋喃，冰乙酸0.03%，乙酸锌1.0 g/L）为流动相，流速1.0 mL/min，检测波长 激发波长243 nm发射波长430 nm。当称取样品1.0 g，定容体积为10 mL时，MK-7的检出限为0.03 μg/g，定量限为0.1 μg/g；MK-7在浓度0~2.176 μg/mL的范围内线性关系良好，线性相关系数为R2=0.9999；重复性实验中RSD%为0.97%；样品加标回收率为93.40%。此方法操作简单，高效，准确，重现性好，可用于营养素补充制剂中维生素K2（MK-7）的含量测定。     

反相高效液相色谱法测定乳制品中核苷酸方法的研究

建立了高效液相色谱法测定乳制品中核苷酸含量的方法。采用紫外检测器，波长为254nm；色谱柱为迪马钻石C18，柱温为25℃，流动相为①0．01mol／L K2HPO4960ml 0．1mol／L K2HPO440mllpH5；测定腺嘌呤核苷(AMP)、鸟嘌呤核苷(GMP)、次黄嘌呤核苷(IMP)。②乙腈：(0．01mol／LKH2PO4 0．005mol／LK2HPO4 1mmol／L四丁基溴化氨，磷酸调pH5．0)=5：95，测定胞嘧啶核苷(CMP)、脲嘧啶核苷(CMP)。流速为1．0ml／min。五种核苷酸组分。标准曲线相关系数r为CMP0．9868；UMP0．9879；GMP0．9792；IMP0．9799；AMP0．9553；回收率为94．6％；8次样品重复测定变异系数为1．79％。     

气相色谱法测定核糖核酸中乙醇含量的研究

通过蒸馏法分离提取核糖核酸中乙醇，采用气相色谱法测定乙醇含量，确定了有关测定方法参数。该方法样品最低捡测浓度为0．007g／kg，回收率为95％～104％，相关系数为r=0．9997，线性范围为（0．02～2．00）g／kg，相对标准偏差RSD为1．74％（n=6）。该方法快速、准确、灵敏度高、线性好，回收率高，可为核糖核酸中乙醇含量的监测提供灵敏、准确的分析方法。     

超高效液相色谱法快速检测乳粉中维生素A方法的研究

本文建立了超高效液相色谱法快速测定乳粉中维生素A的方法。采用紫外检测器,Waters公司的T3柱,以甲醇-水（97：3,V／V）为流动相,流速0．2mL／min,波长为325nm,测定一个样品只需2min。结果表明：该方法的回收率为：94．0—101.2％。RSD（n=6）为：2．94％。标准曲线相关系数R为0．9999。检出限为：0．1ug／100g。     

石墨炉原子吸收绝对分析法测定葡萄酒中的铜、铅

为探讨葡萄酒中铜、铅实现绝对分析的可行性，使用日本日立Z-5000原子吸收分光光度计，在不同时间检测葡萄酒中铜、铅两元素的“特征质量m0”值。石墨管使用次数与不同原子化温度对特征质量m0影响不大；铜特征质量（3．50≤m0≤3．70，RSD％=7．5）；铅特征质量（8．09≤m0≤8．42，RSD％=10．2）；不同实验室同型仪器比对（铜：RSD％=3．2，铅：RSD％=7．6）；用绝对分析法按测m0值的相同条件测定茶叶与西红柿叶标准样品，其实测值与标准值基本一致；用绝对分析法对葡萄酒中铜、铅进行不同时间的加标回收测定，其回收率分别为：铜（91．2％～102．6％）；铅（91．9％-101．3％）。检出限（铜：0．042μg，L；铅：0．075μg／L）；测量范围（铜：0．10～30．00μg／L；铅：0．10—50．00μ／L）。该方法对葡萄酒中铜、铅两元素实现绝对分析是可行的。     

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.     

An internet compendium of analytical methods and spectroscopic information for monomers and additives used in food packaging plastics

An internet website (http://cpf.jrc.it/smt/) has been produced as a means of dissemination of methods of analysis and supporting spectroscopic information on monomers and additives used for food contact materials (principally packaging). The site which is aimed primarily at assisting food control laboratories in the European Union contains analytical information on monomers, starting substances and additives used in the manufacture of plastics materials. A searchable index is provided giving PM and CAS numbers for each of 255 substances. For each substance a data sheet gives regulatory information, chemical structures, physico-chemical information and background information on the use of the substance in particular plastics, and the food packaging applications. For monomers and starting substances (155 compounds) the infra-red and mass spectra are provided, and for additives (100 compounds); additionally proton NMR are available for about 50% of the entries. Where analytical methods have been developed for determining these substances as residual amounts in plastics or as trace amounts in food simulants these methods are also on the website. All information is provided in portable document file (PDF) format which means that high quality copies can be readily printed, using freely available Adobe Acrobat Reader software. The website will in future be maintained and up-dated by the European Commission's Joint Research Centre (JRC) as new substances are authorized for use by the European Commission (DG-ENTR formerly DGIII). Where analytical laboratories (food control or other) require reference substances these can be obtained free-ofcharge from a reference collection housed at the JRC and maintained in conjunction with this website compendium.     

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.     

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 of benzo[a]pyrene in spiked fatty foods by second derivative synchronous spectrofluorimetry after microwave-assisted treatment of samples

A simple, rapid and inexpensive method has been developed for the determination of benzo[a     

The development of reference materials for paralytic shellfish poisoning toxins in lyophilized mussel. II: Certification study

This paper describes the second part of a project undertaken to develop certified mussel reference materials for paralytic shellfish poisoning toxins. In the first part two interlaboratory studies were undertaken to investigate the performance of the analytical methodology for several PSP toxins, in particular saxitoxin and decarbamoyl-saxitoxin in lyophilized mussels, and to set criteria for the acceptance of results to be applied during the certification exercise. Fifteen laboratories participated in this certification study and were asked to measure saxitoxin and decarbamoyl-saxitoxin in rehydrated lyophilized mussel material and in a saxitoxin-enriched mussel material. The participants were allowed to use a method of their choice but with an extraction procedure to be strictly followed. The study included extra experiments to verify the detection limits for both saxitoxin and decarbamoyl-saxitoxin. Most participants (13 of 15) were able to meet all the criteria set for the certification study. Results for saxitoxin.2HCl yielded a certified mass fraction of <0.07 mg/kg in the rehydrated lyophilized mussels. Results obtained for decarbamoyl-saxitoxin.2HCl yielded a certified mass fraction of 1.59+/-0.20 mg/kg. The results for saxitoxin.2HCl in enriched blank mussel yielded a certified mass fraction of 0.48 +/- 0.06 mg/kg. These certified reference materials for paralytic shellfish poisoning toxins in lyophilized mussel material are the first available for laboratories to test their method for accuracy and performance.     

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.