新型激发态分子内质子转移聚合物的制备与胺类气体的高灵敏检测

目的 基于新的检测机制，构建胺类气体的高灵敏度和高选择性传感器。方法 以2,5-二氨基-1,4-苯二噻吩二盐酸盐、羟基对苯二甲酸和1,10-十二羧酸为原料通过脱水反应制备得到具有激发态分子内质子转移(excited-state intramolecular proton transfer，ESIPT)特性的聚合物，并采用红外光谱对其进行结构表征。通过ESIPT聚合物与胺蒸气的选择性切断乙酰基释放出产生荧光的基团，建立胺蒸气浓度与荧光强度之间的关系，实现食品腐败的高灵敏检测。结果 制备得到ESIPT聚合物具有大的斯托克斯位移(160 nm)。在400 nm光照射下，ESIPT聚合物在542 nm处的荧光强度与胺蒸气浓度之间具有良好的线性关系，相关系数为0.98，检出限为11 mg/L并具有高选择性。相比较于低温保存下的牛肉，储存于25℃下牛肉的ESIPT薄膜荧光强度更强。结论 该传感器利用其轻便性和对胺蒸气的高灵敏度，可通过检测微生物生长产生的挥发性胺来用于食品腐败监测中。     

电化学传感器测定猪肉中的红霉素残留含量

研究了电化学传感器对动物源性食品中红霉素残留的测定。采用电沉积法和共价吸附法将纳米金和壳聚糖/普鲁士蓝/石墨烯复合物修饰到电极表面,构建一种灵敏的电化学免疫传感器。对修饰的电化学传感器进行优化,选取100 ng/m L作为固定抗原的浓度,40 min作为培养时间。对不同浓度红霉素溶液进行检测,得到的线性范围为0.3~1000 mg/m L,检测限为0.15 ng/m L。采用罗红霉素作为干扰物检测电化学传感器的选择性;利用5根电极对同一浓度的红霉素溶液进行测定,其对标准偏差范围为3.8%~5.1%;单支电极连续5次在100 ng/m L的红霉素溶液中测定的标准偏差为4.6%;储存一周后的电化学传感器测定红霉素浓度的标准偏差为4.5%。通过对实际样品(猪肉)的加标测定,回收率范围为86.0%~103.1%。综上所述,该电化学传感器具有很好的选择性、重现性、稳定性和准确性,可以用于猪肉中红霉素残留的检测。     

基于PAMAM树枝状大分子的纳米免疫传感器法快速测定肉类中沙丁胺醇

采用聚酰胺-胺(PAMAM)树枝状大分子材料、羧基化多壁碳纳米管(MC-COOH)和1-丁基-3-甲基咪唑基四氟硼酸盐复合材料修饰玻碳电极,包埋固定沙丁胺醇抗体制备免疫传感器,建立一种新型免疫传感器法快速检测肉类中沙丁胺醇(SAL)。以K3[Fe(CN)6]为探针,利用循环伏安法对该纳米传感器进行电化学表征,优化免疫传感器法测定沙丁胺醇的试验条件,结果:电解质溶液p H 7.0,孵育温度37℃,孵育时间30 min。该传感器的免疫响应电流与电解质溶液中沙丁胺醇的质量浓度在0.1~25 ng/m L范围呈线性关系,其线性方程为IP=-0.2878CSAL+45.865,相关系数R2=0.9946,最低检出限为0.04 ng/m L(S/N=3),加标回收率为95.40%~103.90%;利用该法与高效液相色谱法检测市售猪肉、羊肉中的沙丁胺醇,其检测结果与HPLC法基本一致,该法具有简便快捷、准确等优点,可用于肉类及肉制品中沙丁胺醇的快速检测。     

基于无标记金纳米簇的新型荧光生物传感器在赭曲霉毒素A快速检测中的应用

基于快速合成无标记核酸适配体（aptamer,Apt）模板金纳米簇（gold nanocluster,AuNCs）,并以核酸Apt部分互补的单链DNA修饰的金纳米颗粒（gold nanoparticles,AuNPs）结合,构建新型荧光复合纳米生物传感器。利用检测靶标与核酸Apt之间更强结合力,使已荧光猝灭的Apt-AuNCs@cDNA-AuNPs复合纳米传感器发生荧光共振能量转移,最终体系荧光强度值恢复的特性,用于快速准确检测赭曲霉毒素A（ochratoxin A,OTA）。结果表明,OTA质量浓度在0.01～2.5 ng/mL之间,荧光强度对应峰值（FI）与OTA质量浓度（C）呈现良好的线性关系,回归方程分别为FI=689.84lgC（OTA）＋8 315.31;检出限为0.025 ng/mL（信噪比为3）。该荧光生物传感器具有合成及操作简单、灵敏度高、选择性强、稳定性好及检测下限低的特点,预期在食品中相关有害因子的安全检测等提供一种新的思路和平台。     

冷却方式和NaCl浓度对猪肉匀浆物凝胶特性的影响

目的研究3种冷却方式和不同NaCl浓度对冷鲜猪肉匀浆物凝胶特性的影响。方法以冷鲜猪肉为原料,分析测定不同冷却方式和NaCl浓度对猪肉匀浆物蛋白质溶解度、凝胶脱水率,凝胶持水力、凝胶强度和凝胶硬度的影响。结果 NaCl浓度为0.42mol/L时,常规冷却的猪肉匀浆物蛋白质溶解度为18.25mg/m L、凝胶持水力为49.66%、凝胶强度为40.65 g、硬度为52.38 g,均大于快速冷却和浸没冷却; NaCl浓度为0.60 mol/L时,快速冷却的猪肉匀浆物蛋白质溶解度为20.74mg/m L、凝胶强度72.27g、凝胶持水力为74.02%,均大于常规冷却和浸没冷却。结论在较高的NaCl浓度(0.60mol/L)下,快速冷却的猪肉匀浆物凝胶特性相对较好;在较低的NaCl浓度(0.42 mol/L)下,常规冷却的猪肉匀浆物凝胶特性相对较好。     

棉纺织品中几种常用荧光增白剂的检测

研究高效液相色谱法测定纺织品中11种荧光增白剂残留量的检测效果。将样品在50℃温度下经70%二甲基甲酰胺水溶液超声提取40 min,提取液以Inertsil Ph-3色谱柱(4.6 mm×250 mm,5μm)作为固定相,甲醇、乙腈和水作为流动相进行梯度洗脱,有效分离了11种目标物质。试验结果表明:11种荧光增白剂检出限在0.2 mg/kg~14 mg/kg之间,定量低限在1.0 mg/kg~70 mg/kg之间,在0.01μg/m L~70μg/m L范围内峰强度与质量浓度的线性关系良好(r0.999 0),方法的平均回收率在83.23%~101.51%之间。认为:该方法简单快速,稳定准确,灵敏度高,可适合于大批量检测纺织品样品。     

基于激发态分子内质子转移机理的荧光分析法测定茶叶中的铜含量

基于激发态分子内质子转移机理,合成荧光猝灭型铜离子荧光探针(CFP)。通过优化铜离子的检测条件,构建一种简单、快速、灵敏的荧光分析法检测茶叶中的铜含量。试验结果显示:在p H 7.0的4-羟乙基哌嗪乙磺酸缓冲溶液中,铜离子质量浓度C在0.1~0.9μg/m L范围与CFP 500 nm处的相对荧光强度△F呈良好的线性关系,线性回归方程△F=641.9524C-65.3323,相关系数R2=0.9869,方法检出限为0.04μg/m L。该方法应用于实际茶叶样品中铜离子的快速测定,相对标准偏差小于4.5%,回收率在94%~106%之间,结果令人满意。     

基于二氧化锰纳米片和核酸外切酶I构建荧光适配体传感器检测氯霉素

为创建食品中氯霉素的新型快速检测方法,以二氧化锰纳米片淬灭适配体的荧光,核酸外切酶I酶切放大荧光信号,构建了检测氯霉素的适配体传感器。结果表明:在适配体浓度50nmol/L,二氧化锰质量浓度0.05mg/mL,核酸外切酶用量0.4U/μL,酶切时间50min的最佳荧光检测条件下,线性范围为0.1~80.0nmol/L,检出限为0.08nmol/L。构建的检测方法具有操作简单,检测灵敏度高的优点,并实现了在食品样品中的准确检测。     

基于2,7-二（4-吡啶基）吖啶的荧光探针灵敏检测烟草农药残留抑芽丹

为实现烟草农药残留抑芽丹的快速定量检测，利用实验室自行设计合成的有机小分子荧光探针2,7-二（4-吡啶基）吖啶与抑芽丹分子间存在荧光作用机制，建立了烟草中抑芽丹的快速检测方法。结果表明：(1)抑芽丹在0.5～100.0μmol/L范围内线性关系良好，检出限为0.1μmol/L(0.11 mg/kg)。(2)该方法荧光响应时间为1 min，测定快速。(3)10倍浓度的其他农药对待测液的荧光强度影响不大，方法选择性好；将其用于烟草中农药残留抑芽丹检测，加标回收率介于91.0%～106.7%之间，相对标准偏差为1.4%～4.8%。该方法适用于烟草中农药残留抑芽丹的快速定量检测。     

利用分子马达技术检测霍乱弧菌

利用载色体chromatophore上的F0F1-ATPase分子马达生物传感器,建立了应用在食品检测中的快速检测方法。首先在ATP合酶的ε亚基上连接ε亚基抗体-生物素-链霉亲和素-生物素-ompW探针,将待测霍乱弧菌和阴性对照分别与此生物传感器结合,比较其催化ATP合成30 min后的ATP产生量,进而对霍乱弧菌的DNA进行检测。ATP合成的量可以通过环境H+的量进行测定,H+的量通过F-DHPE所体现的荧光强度大小标定。结果表明,Chro ompW的浓度在0.078 mg/mL,单核增生李斯特菌DNA浓度在40 ng/mL为最适检测条件。通过与实际检测样品的传统检测方法及PCR检测方法对照,具有良好的检测符合性。     

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.     

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.     

低温带皮菜籽粕微粉的不同粒级部分的功能特性

为研究低温带皮菜籽粕微粉的不同粒级部分的功能特性,以经低温脱脂的带皮菜籽粕为原料,经微粉碎后筛分成212~425μm、150~212μm和106~150μm的3个不同粒级的微粉样品,检测这些样品的吸水性、吸油性、乳化性和乳化稳定性、蛋白质体外消化率。结果表明:1 3个不同粒级的微粉样品之间的粗纤维含量存在显著差异,表明三者的结构组成成分有一定差异。23个微粉样品的乳化活性和乳化稳定性随粒度级别的减小而显著增加(P0.01)。33个微粉样品的蛋白质体外消化率随粒度级别的减小而显著增加(P0.01)。4不同粒级带皮菜籽粕微粉样品的吸水性与吸油性受其结构组成物质不同和粒度的双重影响,与粒度的相关性不明显。     

Microbiology of food taints

Fresh and processed foods are often spoilt by the presence of undesirable flavours and odours caused by microbial action. The aim of this paper is to review the current knowledge of microbiologically induced taints that occur in a wide range of foodstuffs, including meats, poultry, fish, crustaceans, milk, dairy products, fruits, vegetables, cereals and cereal products. Examples have been chosen where the compounds responsible for the taint have been identified and sufficient data obtained to demonstrate the involvement of microorganisms. However, in some cases the full identity of the causative organism may not have been elucidated. The types of microorganisms covered by this review include bacteria, fungi, yeasts, actinomycetes and cyanobacteria. Although cyanobacteria do not in general infect foods, their presence in aqueous systems and water supplies can lead to off-flavours in aquatic organisms and processed foodstuffs. Several examples of each of these processes are discussed. Wherever possible, the likely biosynthetic pathway used by the microorganism to produce the offending compound in a foodstuff is indicated.     

The development of reference materials for paralytic shellfish poisoning toxins in lyophilized mussel. I: Interlaboratory studies of methods of analysis

This paper describes the first part of a project undertaken to develop mussel reference materials for Paralytic Shellfish Poisoning (PSP) toxins. Two interlaboratory studies were undertaken to investigate the performance of the analytical methodology for several PSP toxins, in particular saxitoxin (STX) and decarbamoyl-saxitoxin (dc-STX) in lyophilized mussels, and to set criteria for the acceptance of results to be applied during the second part of the project: the certification exercise. In the first study, 18 laboratories were asked to measure STX and dc-STX in rehydrated lyophilized mussel material and to identify as many other PSP toxins as possible with a method of their choice. In the second interlaboratory study, 15 laboratories were additionally asked to determine quantitatively STX and dc-STX in rehydrated lyophilized mussel and in a saxitoxin-enriched mussel material. The first study revealed that three out of four postcolumn derivatization methods and one pre-column derivatization method sufficed in principle to determine STX and dc-STX. Most participants (13 of 18) obtained acceptable calibration curves and recoveries. Saxitoxin was hardly detected in the rehydrated lyophilized mussels and results obtained for dc-STX yielded a CV of 58% at a mass fraction of 1.86 mg/kg. Most participants (14 out of 18) identified gonyautoxin-5 (GTX-5) in a hydrolysed extract provided. The first study led to provisional criteria for linearity, recovery and separation. The second study revealed that 6 out of 15 laboratories were able to meet these criteria. Results obtained for dc-STX yielded a CV of 19% at a mass fraction of 3.49mg/kg. Results obtained for STX in the saxitoxin-enriched material yielded a CV of 19% at a mass fraction of 0.34mg/kg. Saxitoxin could not be detected in the PSP-positive material. Hydrolysis was useful to confirm the identity of GTX5 and provided indicative information about C1 and C2 toxins in the PSP-positive material. The methods used in the second interlaboratory study showed sufficiently consistent analysis results to undertake a certification exercise to assign certified values for STX and dc-STX in lyophilized mussel.