油脂及其制品中BHA、BHT、PG和TBHQ快速测定方法的研究

研究了采用高效液相色谱仪同时测定油脂及食品中BHA、BHT、PG、TBHQ的检测方法。样品经甲醇提取、过滤后即可直接测定。检测波长 ,2 80nm ;流动相 ,V(甲醇 )∶V(质量分数 1%乙酸 ) =40∶60 ;梯度 ,40 %～ 10 0 %甲醇 /7 5min ,10 0 %甲醇保持 4 5min。 4种组分的回收率在 85 8%～ 10 1 5 %之间 ,相对标准偏差 (RSD) <5 5 4%。该法简单、快速、准确 ,可用于油脂及其制品中BHA、BHT、PG和TBHQ的日常检测。     

抗氧化剂的超高效液相色谱-串联质谱法测定

研究了油炸食品中化学合成酚类抗氧化剂--丁基羟基茴香醚(BHA)、二叔丁基对甲酚(BHT)、没食子酸丙酯(PG)、特丁基对苯二酚(TBHQ)的检测,采用超高效液相色谱-串联质谱法测定,以反相C18为分离柱,乙腈-甲醇水体系为流动相进行梯度洗脱,采用负离子检测模式,外标法定量。4种抗氧化剂呈良好线性关系(R2=0.9953~0.9998),PG方法检出限为2.0μg/kg,BHA、TBHQ检出限为200μg/kg,BHT检出限为500μg/kg。回收率为79%~96%,相对标准偏差为0.9%~5.3%,方法准确、灵敏、重现性好,可用于油炸食品中抗氧化剂的检测。     

油炸薯条中酚类抗氧化剂的高效液相色谱法测定

采用反相高效液相色谱法测定油炸薯条中PG、TBHQ、BHA、4HR、BHT、2246.其中PG、TBHQ用50%甲醇(体积分数1%的冰醋酸)作流动相,BHA、4HR、BHT、2246用80%的甲醇作流动相,检测波长为280nm,用纯甲醇提取样品中的PG、TBHQ;用甲醇∶二氯甲烷=9∶ 1(V/V)提取BHA、4HR、BHT、2246.相关系数在0.9983～0.9996之间,检出限为1.0～2.0μg/g ,标准偏差在0.21%～5.30%之间,平均回收率均在85%以上.     

PG、TBHQ、BHA和BHT4种常见抗氧化剂部分稳定性的研究

研究PG、TBHQ、BHA和BHT 4种常见抗氧化剂在不同溶荆、酸碱中稳定性为检测工作者及科研工作者在试验过程中储存或者提取时提供参考依据。采用高效液相色谱法(HPLc),以4种抗氧化剂的保留率为指标,考察4种抗氧化剂的稳定性。从试验结果来看:PG、TBHQ、BHA和BHT在甲醇以及酸性条件下具有较好的稳定性。     

油脂、食品中BHT、BHA、PG的薄层色谱测定及油脂中BHT、BHA的气相色谱测定

<正> BHT、BHA、PG是人工合成的酚类油溶性抗氧化剂,被添加到油脂及高脂肪食品中防止脂肪氧化,保证食品质量。油脂及食品中抗氧化剂的测定方法文献报道很多,本方法参考文献加以改进用甲醇作溶剂直接提取豆油,花生油、菜籽油、芝麻油及猪油中的BHT、BHA、PG后,(一)用薄层色谱法定性以及根据其在薄层板上显示的最低检出量与标准品最低检出量比较而概略定量;(二)用气相色谱分离BHT,BHA并测定含量。对高脂肪食     

高效液相色谱法同时测定食用油中9种抗氧化剂

采用乙腈提取食用油脂中的抗氧化剂PG、THBP、TBHQ、NDGA、BHA、OG、IONOX-100、DG、BHT,浓缩后用乙腈-水淋洗的反相高效色谱法测定其中的抗氧化剂的含量,方法最低检测限:PG、THBP、NDGA、OG、DG为0.5μg/g,TBHQ、BHA、IONOX-100、BHT为1μg/g,相对标准偏差为1.01%～6.89%,回收率为88.85%～102.57%。该方法简便、快速,稳定可靠。     

肉制品中合成抗氧化剂含量的高效液相色谱法测定

建立用高效液相色谱法同时测定肉制品中的合成抗氧化剂叔丁基羟基茴香醚(BHA)、2,6-二叔丁基对甲酚(BHT)、叔丁基对苯二酚(TBHQ)、没食子酸丙酯(PG)含量的方法.将试样中的抗氧化剂用甲醇提取,经0.5μm滤膜过滤,进行色谱分析.方法栓出限BHA为5 mg/kg,BHT、TBHQ、PC为2 mg/kg.3个不同加标水平样品中4个目标化合物的回收率为85%～101%,RSD为3.6%～6.1%(n=6).该方法前处理方法快速、简单,检测结果准确.实现了用高效液相色谱对肉制品中合成抗氧化剂的定量分析.     

HPLC法测定花生酱中BHA、BHT和TBHQ

采用甲醇浸提花生酱中的抗氧化剂BHA、BHT和TBHQ,浓缩后用甲醇-水淋洗的反相高效液相色谱法测定其中的抗氧化剂含量,检测波长为280nm;流动相甲醇∶水=20∶80;梯度:20%～80%甲醇/5～20min,80%甲醇保持5min。3种抗氧化剂的回收率在85.25%～103.91%,变异系数为2.07%～3.80%,该方法简便、快速、准确,适用于花生酱中BHA、BHT和TBHQ的检测。     

毛细管气相色谱法测定食品中的酚类抗氧化剂

建立了同时测定食品中BHA、BHr、TBHQ和PG等四种酚类抗氧化剂的测定方法.采用HP-1毛细管色谱柱分离,氢火焰离子化检测器外标法定量,样品加标回收率为96.3%～104.2%,相对标准偏差为0.63%～1.53%,检出限分别为BHA为0.72mg/L、BHT为0.62mg/L、TB-HQ为0.68mg/L、PG为1.2mg/L.该方法具有快速、灵敏度高、重现性好、预处理简单等优点.     

液相色谱法同时快速测定植物油中TBHQ、BHA、BHT探讨

采用NY/T 1602-2008液相色谱条件分析TBHQ、BHA和BHT时,结果发现色谱图基线不稳,有杂峰干扰结果准确定量,导致BHT不能建立良好线性标准工作曲线。为建立同时快速测定该三种抗氧化剂方法,该研究采用甲醇―水(体积比85∶15)进行等梯度洗脱,对比三种标准物质色谱图;结果表明,荧光检测器(FLD)更适于定量检测TBHQ和BHA;紫外检测器(VWD)更适于定量检测BHT;色谱图均基线平稳、峰形良好,无杂峰干扰,TBHQ、BHA和BHT均能建立良好线性标准工作曲线,相关系数分别为0.99999、0.99963和0.99999;TBHQ、BHA和BHT平均加标回收率分别为102.68%、110.97%和102.39%;相对标准偏差分别为3.87%、2.46%和1.98%(n=10)。该法前处理简单、定量快速准确、方法回收率高、精密度好,适于同时快速测定植物油中TBHO、BHA、BHT三种抗氧化剂。     

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.     

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.     

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.     

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.