基于可见/近红外光谱和变量选择的脐橙可溶性固形物含量在线检测

为联合可见/近红外光谱技术和变量选择方法在线检测脐橙主要内部品质指标可溶性固形物(SSC),分别选定脐橙校正集和预测集样本141个和47个,脐橙运输速度为0.3m/s,利用USB4000微型光谱仪在线采集脐橙样本的可见/近红外光谱,先分别采用无信息变量消除(UVE)和遗传算法(GA)对650~950nm波段范围的波长变量进行预筛选,再分别利用竞争自适应重加权采样(CARS)及连续投影算法(SPA)对波长变量进一步筛选,并应用偏最小二乘(PLS)方法分别建立脐橙SSC的在线预测模型,并与原始光谱等建立的预测模型进行比较。结果表明,对于脐橙SSC,预筛选方法GA优于UVE方法,变量选择方法CARS优于SPA方法;GA-CARS及GA-SPA联合变量选择方法优于对应的单一变量选择方法CARS及SPA。在上述变量选择方法中,GA-CARS方法获得的结果最优,其所建立的脐橙SSC的PLS模型的校正集和预测集相关系数分别为0.933和0.824,校正集和预测集均方根误差分别为0.429%和0.670%,性能优于原始光谱建立的PLS模型,且建模波长变量数由1 385个下降为78个,仅占原波长变量数的5.63%。由此表明,GA-CARS联合变量选择方法可以有效筛选脐橙SSC的波长变量,提高预测模型的稳定性和预测精度。     

无效变量消除法在油菜籽芥酸近红外无损速测中的应用

探索改善油菜籽芥酸近红外预测模型准确度与精密度的方法,利用无效变量消除法（UVE）,对135个油菜籽样品近红外光谱信号进行筛选,并利用筛选后的光谱对油菜籽芥酸含量进行偏最小二乘法交叉验证。结果表明,UVE法筛选变量后建立的芥酸校正模型对未知样品预测结果的准确度和速度显著优于全波长参与建立的芥酸校正模型。散射校正加一阶导数对光谱预处理,UVE法筛选变量,偏最小二乘法交叉验证建立的校正模型效果最好,其预测值与标准值的相关系数R达到0.92,交叉验证预测均方差为2.2。因此,用UVE进行波长选择后建立的近红外模型,能准确快速地对油菜籽芥酸含量进行定量分析。     

无信息变量消除法在筛选南疆红枣总酸近红外特征波长中的应用

以南疆红枣总酸的快速无损检测为研究对象,利用SPXY(Sample set partitioning based on joint x-y distances)法来划分校正集样本,应用无信息变量消除法(UVE)对南疆红枣总酸近红外光谱(NIRS)特征变量进行筛选,然后用筛选出的变量建立偏最小二乘(PLS)模型,该模型的预测标准偏差(RMSEP)为0.044 7,预测相关系数为Rp为0.877 8,并将UVE筛选的变量建立的PLS模型与全光谱建立PLS模型结果进行比较。结果表明,SPXY法划分的校正集样本合理;UVE优出选全光谱1 557个变量中的420个变量,建立的PLS模型预测效果要好于全光谱建立的PLS模型,UVE能够有效地选取待测成分的特征波长,建立简化的红枣总酸预测模型,降低模型计算量。     

基于CARS-SPA的苹果可溶性固形物可见/近红外光谱在线检测

采用CARS(competitive adaptive reweighted sampling)联合连续投影算法(SPA)方法筛选苹果可见/近红外光谱的特征变量,继而联合多种不同建模方法建立苹果可溶性固形物(SSC)预测模型,并对预测模型进行对比研究。研究结果显示,采用CARS-SPA联合筛选出的31个变量,通过采用PLS建立苹果SSC的可见/近红外光谱在线检测模型性能最稳定,其变量数仅为原始光谱的1.69%,预测集的相关系数和均方根误差分别为0.936和0.351%。研究表明采用CARS-SPA能有效提取苹果SSC的光谱特征变量,能有效简化模型并提高模型精度。     

LS-SVM结合近红外光谱快速检测香梨可溶性糖

利用可见/近红外光谱技术对"库尔勒香梨"内部品质的快速无损检测具有非常重要的研究意义。为了解决光谱数据中由于大量无关信息的存在而导致模型精度降低的问题,探究了基于不同可见/近红外光谱特征波长筛选方法建立模型的效果。分别采用无信息变量消除算法(UVE)、后向偏最小二乘算法(BiPLS)对香梨可溶性糖的特征波长进行筛选,并将其作为输入变量分别建立偏最小二乘(PLS)、最小二乘支持向量机(LS-SVM)模型。结果表明,UVE算法可以有效地减少建模变量,UVE-LS-SVM模型效果明显优于UVE-PLS模型,其决定系数(R~2)为0.976、预测均方根误差(RMSEP)为2.313、预测相对分析误差(RPD)为5.45,验证了UVE-LS-SVM结合近红外光谱分析技术能实现对"库尔勒香梨"可溶性糖含量的快速无损测量。     

基于变量筛选的温州蜜桔品质的光谱快速检测

目的利用可见/近红外光谱技术结合变量筛选算法建立预测模型。方法采集7个不同批次蜜桔样本的漫透射光谱,预处理优化后,以无信息变量消除法(uninformative variable elimination,UVE)、竞争性自适应重加权法(competitive adaptive reweighting sampling,CARS)及其组合(UVE-CARS)共3种策略来进行光谱有效波段的筛选,建立蜜桔可溶性固形物含量(soluble solid content,SSC)的偏最小二乘预测模型(partial least square,PLS)。结果比较全变量模型和3个特征变量模型的预测性能,UVE-CARS-PLS模型取得了最优的检测效果,相比全变量模型,建模变量数减少了96.5%,其预测集相关系数R_P提升至0.732,预测集均方根误差(root-mean-square error,RMSEP)下降至0.873~0Brix。结论结合多重变量选择算法,可以进一步压缩建模变量数,简化模型,提高模型预测精度,实现区域蜜桔品质的光谱快速检测。     

基于可见/近红外光谱和变量优选的南水梨糖度在线检测

利用可见/近红外光谱技术对南水梨糖度进行在线检测研究。南水梨样本以0.3m/s速度传输,并采用USB4000光谱仪在470~1 150nm波段范围内采集南水梨样本的光谱。然后,利用3种变量选择方法对波长变量进行筛选,应用偏最小二乘(PLS)方法分别建立南水梨糖度的在线预测模型,并分析预测模型性能的优劣。结果表明:可见/近红外光谱技术结合变量选择方法在线检测南水梨的糖度是可行的;竞争自适应重加权采样(CARS)方法优于无信息变量消除(UVE)及连续投影算法(SPA);CARS方法可以有效简化预测模型并提高预测模型的性能;南水梨全光谱PLS及CARS—PLS糖度预测模型的预测集相关系数和预测均方根误差(RMSEP)分别为0.940,0.951和0.467%,0.420%。     

基于特征波长提取的哈密大枣可溶性固形物的高光谱预测

本文利用高光谱图像技术对干制后的哈密大枣可溶性固形物含量(SSC)进行预测研究。使用多种预处理方法对原始光谱进行处理,并对原始光谱和预处理后的光谱分别建立PLS模型,对比分析得出均值中心化(MC)处理效果最佳。对MC处理后的光谱经联合区间偏最小二乘算法(si-PLS)筛选后,再结合遗传算法(GA)和竞争性自适应重加权算法(CARS)提取哈密大枣SSC的特征波长,将提取的波长变量建立哈密大枣SSC的PLS预测模型。结果显示:利用MC-CARS-GA-si-PLS方法提取的16个关键波长变量(仅占全光谱变量的2%)所建立的PLS模型性能优于全光谱PLS模型。该模型的预测集相关系数(Rp)、预测均方根误差(RMSEP)和预测(RPD)分别为0.93、0.48和2.721。该方法提取的波长变量所建立的预测模型,不仅使模型简化,而且增强了模型的预测能力,为高光谱图像技术对水果及其干制品的定量分析研究提供了参考。     

虾样品不同采集状态对近红外光谱PLS模型的影响

研究了不同采集状态的虾样品对近红外光谱PLS模型的影响。利用DA7200近红外光谱仪,采集南美白对虾完整虾和虾糜的近红外光谱曲线。采用Unscrambler10.3软件选择最佳光谱预处理方法和最优波段,建立了完整虾和虾糜与挥发性盐基氮(TVB-N)值、菌落总数(TBC)值关联的偏最小二乘(PLS)模型,并对模型进行评价和验证。结果表明:定标集虾糜模型中的校正相关系数rc,校正决定系数Rc2,交叉验证相关系数rv,交叉验证决定系数Rv2,均高于完整虾模型;校正均方根误差RMSEC,校正标准误差SEC,交叉验证均方根误差RMSECV,交叉验证标准误差SECV均低于完整虾模型。验证模型中虾糜预测模型中相关系数r均大于完整虾预测模型,预测均方根误差RMSEP,预测标准误差SEP均低于完整虾预测模型,且虾糜预测模型对TVB-N、TBC值预测值更为准确,表明以虾糜作为近红外光谱采集状态优于完整虾。     

基于近红外光谱对桃果实低温贮藏品质的定量检测

采用近红外光谱法结合化学计量学方法对桃果实的可溶性固形物(SSC)含量、总酸(TA)含量、糖酸比和硬度等4种品质进行快速检测,研究不同光谱预处理算法对模型的影响,建立偏最小二乘法(PLS)预测模型。建模前,采用方差分析和Pearson相关性分析研究几种指标的关系。桃果实贮藏期的SSC含量、TA含量、糖酸比和硬度最优PLS模型的校正集相关系数分别为0.93,0.69,0.74和0.97;验证集相关系数分别为0.79,0.69,0.68和0.95。交互验证均方根误差(RMSECV)为0.56,0.11,4.24和8.81,预测集均方根误差(RMSEP)为0.89,0.10,6.02和16.22。试验结果表明,近红外光谱对桃果实SSC含量和硬度的快速检测是可行性的,TA含量和糖酸比的预测算法需进一步优化。本研究为实际生产中近红外光谱对桃果实低温贮藏品质无损检测与质量控制提供技术参考。     

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.     

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.     

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.     

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.     

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.     

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.