酱香型白酒中氨基甲酸乙酯的快速检测及风险评估

建立了一种液-液萃取-气相色谱串联质谱联用(GC-MS)快速测定酱香型白酒中氨基甲酸乙酯(EC)的方法,并对酱香成品酒中的EC进行风险评估。结果表明,在10~400 ng/mL范围内,该方法线性良好,EC的线性相关系数r²=1.000,检出限为1.2μg/L;加标回收率为92.5%~100.23%,RSD<3.64%,方法准确性良好;不同酒样的EC含量测定结果的RSD<2.91%,方法精密度良好。326份酱香成品酒中EC的检出率为99.4%,平均含量为86.9μg/L,其中10.4%的EC含量超出了国际常用蒸馏酒标准(150μg/L)。采用暴露边界比(MOE)对酱香成品酒中EC进行风险评估,MOE值为35088,致癌风险相对较低。     

黄酒中氨基甲酸乙酯的分析与控制

氨基甲酸乙酯是一种存在于黄酒中的致癌物质。本文采用气质联用法检测了广东市场上42种黄酒样品中氨基甲酸乙酯含量,28个样品中EC含量超过30μg/kg唱,占66．67％,其中7个样品中EC含量超过了100μg/kg（日本清酒中EC的限量标准）,最高的高达1210μg/kg。研究了脲酶对黄酒处理的效果,结果发现,一定条件下添加脲酶能够去除酒里的尿素,破坏产生氨基甲酸乙酯的主要途径,从而控制氨基甲酸乙酯含量不再剧增。并在单因素试验结果的基础上,进行正交实验,得出脲酶最佳的处理条件为酶浓度150mg／L、处理温度为25℃,pH值为3．5,处理时间10d。该条件下进行处理,可使酒中氨基甲酸乙酯含量降低45．83％。     

芝麻香型与浓香型白酒固态发酵过程中氨基甲酸乙酯的形成研究

氨基甲酸乙酯(EC)是一种具有细胞和基因毒性的2A级致癌物质,我国部分白酒中EC检出率和含量居高不下,引起了广泛关注。本文以浓香型和芝麻香型白酒为例,探究了白酒固态发酵过程中EC、前体物质含量与酸度的变化,同时采用模拟发酵分析白酒酒醅固态发酵过程中p H值、尿素与瓜氨酸对EC形成的影响。研究表明:发酵初期的两种酒醅中均检测到超过20μg/kg EC,发酵过程中芝麻香型酒醅中EC形成速率(4.40×10-7μmol/kg·s)和含量(140.55μg/kg)均显著高于浓香型酒醅,且主要积累于发酵2至4周。两种酒醅中乙醇与尿素在发酵前三周含量分别增加了679.31%～181.89%和87.54%～117.87%,发酵三周后瓜氨酸积累更多。尽管芝麻香型酒醅发酵过程中EC与瓜氨酸和尿素含量相关性均不显著,模拟实验发现添加尿素与瓜氨酸后酒醅中EC含量均增加了23.70%～84.82%,且尿素在酒醅发酵过程中形成EC的能力比瓜氨酸更强。此外,酒醅p H值低于4.0有助于发酵初期EC的形成。以上结果可为针对性降低酒醅发酵过程中积累的大量EC提供依据。     

白酒酿造过程酒醅中尿素的控制与减少

尿素是白酒酿造过程酒醅中含有的氨基甲酸乙酯的主要前体之一,对浓香型白酒中氨基甲酸乙酯含量影响较大,通过降低酒醅中尿素含量可以控制或减少白酒中氨基甲酸乙酯的含量。采用产脲酶菌株或其粗酶与酒醅混合,可在发酵过程中降低尿素含量。从大曲中筛选到3株产脲酶的腐生葡萄球菌(Staphylococcus saprophyticus,S.saprophyticus)在酒醅固态发酵中去除尿素效果不显著,产酸性脲酶的罗伊氏乳杆菌(Lactobacillus reuteri,L.reuteri)全细胞及其粗酶对酒醅中尿素均有很好的去除效果。通过与商品脲酶比较,罗伊氏乳杆菌所产脲酶粗酶对酒醅中尿素去除效果更佳,尿素去除率可达100%。当罗伊氏乳杆菌添加量高于10~7CFU/g酒醅时,尿素去除率在97.3%以上,粗酶加入量高于25 U/kg酒醅时,尿素去除率在77.4%以上。罗伊氏乳杆菌能较好地去除白酒酒醅中尿素。     

白酒中塑化剂(DBP)处理的实践应用

针对塑化剂含量较高的基酒进行活性炭处理,减少在勾兑成品酒时由于不具备检测能力而反复送检的次数。通过对指标的检测和感官品评选择出最适用的活性炭型号、用量和搅拌方案,最后进行大样验证。结果表明JT-207活性炭可以较好去除塑化剂并保持原酒风味,当原酒DBP含量在3mg/kg以上时,最适活性炭用量为4‰,而当DBP含量在3mg/kg以下时,最适活性炭用量为3‰;最佳搅拌方案为B方案。407吨大样实验结果表明活性炭处理方案可行,DBP降低到国家规定标准,且勾兑组合的23个成品酒样DBP检测合格率为100%。     

黄酒中氨基甲酸乙酯直接减除技术的研究

黄酒中含有微量氨基甲酸乙酯(Ethyl Carbamate),简称EC,直接降低黄酒中的EC含量,具有重要的现实意义。在各种吸附性材料中,优选得特异性功能树脂材料L2、L3,复配后以合适的添加量体积分数10%处理酒样,对黄酒中的EC能较有效减除,去除率在60%以上,基本达到EC限量要求,同时对酒体风味的保持较好。材料对EC的减除为吸热过程,实际应用中需保证作用温度大于20℃。面向中国黄酒中EC含量的直接降低,提供了一个实用、便捷的全新途径。     

减少麦曲用量对黄酒中尿素含量及质量的影响

试验了适当减少麦曲用量对黄酒中尿素含量、黄酒理化指标及感官指标的影响。结果表明减少麦曲用量1％，可降低约29％左右的尿素；减少麦曲用量2％，可降低约33％左右的尿素。同时减少麦曲用量1％的酒样其理化指标、感官指标与对照样比较差距不大，可以作为实际生产中降低尿素含量的途径之一加以使用。     

葡萄酒贮存过程中氨基甲酸乙酯含量的变化

为探讨葡萄酒贮存过程中氨基甲酸乙酯(EC)含量的动态变化情况,通过外加反应底物(尿素与瓜氨酸),在葡萄酒体系中研究EC的生成规律,分析了贮存温度、初试尿素和瓜氨酸含量、pH值对贮酒过程中EC含量的影响。结果表明,贮存过程中葡萄酒中尿素和瓜氨酸含量呈下降趋势,而EC的含量逐渐上升;贮存温度、初试尿素和管氨酸含量越高,贮存一段时间后葡萄酒中EC含量也越高;对葡萄酒进行热处理能够显著促进EC的形成,但pH值对EC含量的影响不明显。     

慕萨莱思酒发酵过程中氨基甲酸乙酯含量的变化研究

氨基甲酸乙酯（EC）是发酵食品中存在的一种致癌物质,该研究以新疆阿瓦提慕萨莱思酒为研究对象,检测发酵过程中不同阶段EC含量、尿素含量、酒精体积分数,探究EC的形成与尿素、酒精含量的关系。结果显示,发酵结束后EC含量为25.6 μg/L,尿素与酒精含量越高,EC生成速率越快,慕萨莱思酒中EC含量越高,温度对EC的生成影响较大。     

绍兴黄酒氨基甲酸乙酯的检测与控制

2007年国际癌症研究总署(IARC)将氨基甲酸乙酯(EC)归为人类可能致癌物质(2A类).在黄酒中含量较高.应用GC/MS方法对绍兴黄酒EC含量进行研究,对煎酒前后进行氨基甲酸乙酯监测分析,发现煎酒前和煎酒后EC平均含量分别为16.1μg/kg、63.7μg/kg、其中在煎酒过程中EC增加了47.6μg/kg.在贮存过程中,对年份加饭酒分析,发现EC含量在不断地增加.第一年增加量最多,但后几年平均增加量大约每年15μg/kg左右.所以需加强对黄酒生产工艺和贮存条件的管理和改进,以减少EC的产生,确保绍兴黄酒的竞争性及安全.     

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.