发泡餐盒中苯乙烯单体和低聚物的测定及迁移风险评估

目的建立聚苯乙烯发泡餐盒中苯乙烯单体和低聚物的检测方法,并对其向食品的迁移进行风险评估。方法采用二氯甲烷溶解-甲醇沉淀法提取餐盒中的苯乙烯单体和低聚物,采用气相色谱-质谱联用法测定目标物向水、酒精和脂肪食品模拟物的迁移量,通过比较各物质的估计日摄入量和毒理学安全阈值评估迁移风险。结果苯乙烯单体和低聚物在0.02~1.00 μg/mL范围内线性良好（R均大于0.99）,在餐盒及食品模拟物中的加标回收率为80.5%~101.2%,相对标准偏差为1.6%~10.5%;在5%显著性水平下各物质向脂肪食品模拟物的迁移量明显大于向水和酒精食品模拟物的迁移量 ,扩散系数为1.3×10-15~1.4×10-9 cm2/s,迁移活化能为33.5~53.3 kJ/mol;目标分析物的估计日摄入量均未超过毒理学关注阈值。结论该方法简单、可靠, 可用于测定发泡餐盒中苯乙烯单体和低聚物的含量。聚苯乙烯发泡餐盒不适合在高温条件下盛放脂肪食品。     

食品包装的安全隐患及检测

食品包装已经成为食品不可分割的重要组成部分.各类食品包装材料如塑料、玻璃纸还有金属作为食品的"贴身衣物",在零售和家庭厨房中随处可见,其在原材料、辅料、工艺方面的安全性将直接影响食品质量,继而对人体健康产生影响.材料中的聚合物单体和一些添加剂会溶出,并且极少量地转移到食品中.重点介绍各类包装材料存在的迁移隐患和进行食品包装中可迁移物质检测的一般方法.     

焦化及烟熏食品对人体有害吗?

在日常生活中,我们常常可以看到一些食品经过高温煎炸、焙烤或烟熏后,食品表面呈深棕色,形成焦化现象.常食这种焦化及烟熏食品对人体益害如何,这是许多同志关心的问题.据近代毒理学研究:食品在焦化及烟熏过程中,会产生危害人体的化学物质.尽管这些物质含量极微,但对健康的影响却很大.     

塑料食品包装材料中受限物迁移研究进展

塑料食品包装材料为了达到应有的机械强度,韧性,常常需要在包装材料中添加一些加工助剂,但这些加工助剂在包装材料包装食品的过程中,会迁移到食品中,从而对人体产生危害。本文综述了塑料食品包装材料中添加的四大类受限物质,包括增塑剂、抗氧化剂、热稳定剂以及紫外吸收剂,检索了在中国期刊全文数据库CNKI和Web of Science中相关文献的信息,系统地分类分析了查阅到的文献,并且介绍了4类添加剂的作用机制和目前国内国外对4类添加剂发生迁移的研究现状,比较了我国与发达国家关于4类受限物质的法律法规及迁移限量,提出了减少食品中受限物质迁移量的方法措施以及加强我国塑料食品接触材料中受限物质使用与管理的建议。     

食品接触材料中非有意添加物的安全评估

食品接触材料所迁移出的非有意添加物(non intentionally added substance,NIAS)作为影响食品安全的重要因素而日益受到关注。由于这些NIAS来源复杂且相当数量是未知,给食品接触材料的安全评估和监管带来很大的挑战。基于毒理学关注阈值(threshold of toxicological concern,TTC)方法,结合Cramer决策树方法、化学和生物分析技术的使用,可建立一个针对食品接触材料中NIAS的快速筛查和安全评价模型,对缺乏完整毒理学数据且暴露量较低的化学物质进行风险评估。选择Cramer III所对应的1.5μg/kg BW作为NIAS通用安全暴露阈值,通过分步评估手段,可以得出所迁移未知物质是否需要予以安全关注,重点对食品接触材料迁移高于该TTC的物质进行进一步的确证和风险评估,实现对食品接触材料中高关注物的安全评价从基于检测限模式向TTC安全阈值模式的转变,从而避免不必要的动物试验,节约大量人力、物力和时间,有利于加快食品接触材料中低暴露量化学物质的风险评估和提升产品安全管理效能。     

毒理学关注阈值方法在食品接触材料风险评估中的应用

食品接触材料中包含诸多有意添加的化学助剂,在生产和使用过程中还会引入大量非有意添加物。食品接触材料中的有意和非有意添加物质种类繁多,难以得出所有物质完整的毒理学数据;而且食品接触材料中存在一些低暴露量的物质,它们对人体造成的风险较小而不必要进行传统的风险评估。毒理学关注阈值（threshold oftoxicological concern,TTC）方法作为一种新的风险评估工具,可以对缺乏完整毒理学数据且暴露量较低的化学物质进行风险评估。本文综述TTC方法对食品接触材料中的物质（结构确定和结构未知的物质）进行风险评估的具体应用。对结构已知的物质,可以参照欧洲国际生命科学学会（European International Life Sciences Institute,ILSI）专家组提出的TTC决策树方法;对于未鉴定结构的物质,可以引用一个分步分析的方法,得出未知物质是否需要进行安全关注。本文还指出了TTC方法在食品接触材料风险评估中应用的难点和今后需解决的问题,可为食品接触材料中缺乏毒性数据物质的风险评估提供依据。     

食品中烃类矿物油的污染情况及迁移研究进展

烃类矿物油是石油原油经精馏纯化形成的复杂烃类混合物,食品加工过程中、环境污染以及食品接触材料的迁移等都会导致烃类矿物油进入食品。虽然不同类型矿物油成分对人体的毒性目前还没有统一的界定,但其潜在的危害性已经引起广泛的关注。文中综述了国内外对于烃类矿物油的毒理学特性、食品中烃类矿物油的来源、污染现状及食品接触材料迁移等方面的最新研究进展,总结了目前研究中存在的问题,并对其发展趋势进行了展望。     

食品毒理学的新进展（综述）

食品毒理学的新进展（综述）陈君石中国预防医学科学院营养与食品卫生研究所（１０００５０）食品毒理学的任务是研究与食品有关的毒理学问题。以减少食品中有害物质对人体健康的危害。就其研究对象而言。可以包括凡是与食品的生产、加工、包装、贮藏、运输和销售过程有关...     

邻苯二甲酸酯危害和检测方法的研究进展

邻苯二甲酸酯作为增塑剂广泛应用于塑料工业中,很容易溶出迁移到食品和环境中来,国家质检部门也一直在抽检市场样品进行监测.通过介绍食品中邻苯二甲酸酯产生的来源和对人体的危害以及法规限制,并对检测方法的研究进展进行概述和分析,以期对后续研究做铺垫.     

食品毒理学数据库构建研究

目的 建立食品毒理学数据库（FoodTox）。方法 建立食品毒理学数据库网站,确定数据库优先入库名单,通过文献检索的方式收集相关物质的毒理学资料,利用系统文献综述（SLR）方法整理入库物质的毒理学数据。结果 食品毒理学数据库已收录1 600余种物质,相关数据包括代谢、急性毒性、遗传毒性、生殖发育毒性、亚慢性毒性、慢性毒性和致癌、人群资料、健康指导值等毒理学资料和国内外管理法规、相关食物和症状等,已经向相关领域工作者开放使用。结论 本数据库的建立将为食品毒理学工作者提供第一手的参考资料,为相关优先物质的毒理学安全性评价提供依据,为应急风险评估提供技术支持。     

Development of a Homologous Fluorescence Polarization Immunoassay for Diisobutyl Phthalate in Romaine Lettuce

In this work, three fluorescein-labeled DiBP derivatives (tracers) with different chemical structures and spacer bridges were synthesized and purified by thin-layer chromatography (TLC). Compared with the heterologous tracer, the homologous tracer exhibited more affinity to the antibody. What is more, the tracer concentration and the antibody dilution were further evaluated to improve the sensitivity of fluorescence polarization immunoassay (FPIA). On the basis of sensitive antibody and tracer, a rapid and specific FPIA has been established for the detection of DiBP contamination in the romaine lettuce, which has rarely been reported before. Under the optimal conditions, the developed FPIA showed a good detection range from 8.82 to 2152.84 ng/mL, with a detection limit of 1.77 ng/mL. In addition, the cross-reactivity to several compounds structurally related to DiBP was less than 7.37 %. Therefore, DiBP contamination in spiked romaine lettuce samples was detected by FPIA, with the recovery from 88.28 to 119.11 %. Moreover, when compared with high-performance liquid chromatography (HPLC) and enzyme-linked immunosorbent assay (ELISA), the results analyzed by the developed FPIA shows a strong reliability and a high correlation value of 0.978 and 0.980, respectively. Thus, this data, combined with rapidity and simplicity of the assay, demonstrates that the established FPIA is a suitable method for high throughput screening of DiBP contamination in the romaine lettuce.     

邻苯二甲酸二异丁酯对雄性小鼠空间学习记忆行为的影响

目的观察邻苯二甲酸二异丁酯(DiBP)经口亚慢性暴露,对雄性小鼠空间学习记忆行为的影响。方法每组12只雄性昆明小鼠,空白对照组和阳性对照组给予玉米油溶剂灌胃,各剂量组给予相应剂量的邻苯二甲酸二异丁酯(50、250、500、1000mg/kg BW)玉米油溶液灌胃,连续8周。染毒前后分别对各组动物进行旷场试验和Morris水迷宫试验,其中阳性对照组在染毒结束后进行旷场试验和Morris水迷宫试验前经腹腔注射5mg/kg BW的氢溴酸东莨菪碱。结果试验前各组动物的学习记忆能力一致。8周实验结束后,阳性对照组和1000mg/kg BW剂量组小鼠与空白对照组小鼠相比在旷场中心区域停留时间明显延长(P0.05)。500mg/kg BW剂量组和阳性对照组与空白对照组相比Morris水迷宫训练第一天的逃避潜伏期明显延长(P0.01),1000mg/kg BW剂量组与空白对照组相比逃避潜伏期也明显延长(P0.05)。其他各项指标与空白对照组相比,差异均无统计学意义。结论在本试验条件下,DiBP会降低雄性昆明小鼠的空间学习记忆能力。     

Optimisation of an analytical method and results from the inter-laboratory comparison of the migration of regulated substances from food packaging into the new mandatory European Union simulant for dry foodstuffs

This paper presents the outcome of the development, optimisation and validation at European Union level of an analytical method for using poly(2,6-diphenyl phenylene oxide – PPPO), which is stipulated in Regulation (EU) No. 10/2011, as food simulant E for testing specific migration from plastics into dry foodstuffs. Two methods for fortifying respectively PPPO and a low-density polyethylene (LDPE) film with surrogate substances that are relevant to food contact were developed. A protocol for cleaning the PPPO and an efficient analytical method were developed for the quantification of butylhydroxytoluene (BHT), benzophenone (BP), diisobutylphthalate (DiBP), bis(2-ethylhexyl) adipate (DEHA) and 1,2-cyclohexanedicarboxylic acid, diisononyl ester (DINCH) from PPPO. A protocol for a migration test from plastics using small migration cells was also developed. The method was validated by an inter-laboratory comparison (ILC) with 16 national reference laboratories for food contact materials in the European Union. This allowed for the first time data to be obtained on the precision and laboratory performance of both migration and quantification. The results showed that the validation ILC was successful even when taking into account the complexity of the exercise. The results showed that the method performance was 7–9% repeatability standard deviation (rSD) for most substances (regardless of concentration), with 12% rSD for the high level of BHT and for DiBP at very low levels. The reproducibility standard deviation results for the 16 European Union laboratories were in the range of 20–30% for the quantification from PPPO (for the three levels of concentrations of the five substances) and 15–40% from migration experiments from the fortified plastic at 60°C for 10 days and subsequent quantification. Considering the lack of data previously available in the literature, this work has demonstrated that the validation of a method is possible both for migration from a film and for quantification into a corresponding simulant for specific migration.     

不同温度下邻苯二甲酸酯从塑料包装向鲜肉和食用油中的迁移

以鲜肉和食用油为对象,分别设置80 ℃和4 ℃（鲜肉）、25 ℃和4 ℃（食用油）,研究16 种邻苯二甲酸酯（phthalic acid esters,PAEs）从塑料包装向肉油类食品间的迁移量,分析迁移量与温度、接触时间和塑料包装中PAEs的含量和种类的关系。结果表明：PAEs从塑料包装向肉、油类食品间存在迁移现象,80 ℃、120 min时PAEs向鲜肉中的总迁移量为3.2～5.6 mg/kg,4 ℃,6 d的总迁移量和80 ℃,120 min相当。25 ℃,25 d向食用油中的总迁移量为9.0～10.0 mg/kg,显著高于4 ℃。塑料包装材料中PAEs向肉、油类食品的迁移在接触初期较快,且迁移量随着接触时间的延长而增大。塑料包装材料中PAEs的含量高,向肉、油类食品中的总迁移量也升高,在25 ℃和80 ℃时,总迁移量与包装材料中PAEs的含量呈正相关关系。不同种类的PAEs的迁移存在差异,分子质量大的PAEs迁移速度较慢,其中美国国家环保署优先控制的6 种PAEs均会发生一定的迁移。     

邻苯二甲酸二异丁酯对小鼠主动回避行为及脑组织氧化应激的影响

目的 对邻苯二甲酸二异丁酯(DiBP)影响小鼠主动回避学习记忆行为进行初步研究,并探讨其是否可引起脑组织氧化损伤.方法 将60只昆明小鼠(实验动物房内适应3d)按体重随机分对照组和4个不同剂量的DiBP试验组(4组剂量分别为50、250、500和1 000 mg/kg BW).其中,对照组给予玉米油溶剂灌胃,而各试验组给予相应剂量的DiBP玉米油溶液灌胃,实验连续进行8周,普通饲料喂饲,自由饮水.试验结束后,分别对各组动物进行穿梭箱行为学测试,并测定脑组织超氧化物岐化酶(SOD)、谷胱甘肽过氧化物酶(GSH-Px)的活性及8-羟基脱氧鸟苷(8-OHdG)的含量.结果 500和1 000 mg/kg BW组与对照组比较,条件反射潜伏期(CL)延长,差异均有统计学意义(P＜0.05);1 000 mg/kg BW组与对照组比较,条件反射次数减少,差异有统计学意义(P＜0.01);500和1 000 mg/kg BW组与对照组比较,条件性回避率降低,差异均有统计学意义(P＜0.05).各试验组小鼠脑组织SOD的活性与对照组比较差异无统计学意义(P＞0.05),但GSH-Px活性呈现降低趋势,250和1 000 mg/kg BW组与对照组比较,酶活性差异有统计学意义(P＜0.05);各试验组与对照组相比,8-OHdG含量增加,差异具有统计学意义(P＜0.05).结论 DiBP可损伤实验小鼠主动回避学习记忆能力,并能够导致试验小鼠脑组织发生不同程度的氧化应激损伤.     

塑料食品接触材料中非有意添加物检测方法研究进展

食品接触材料(Food contact materials, FCMs) 与食品安全密切相关。FCMs能有效保护食品,防止其腐败变质,但在生产过程中可能会由于一些原因引发食品安全问题,其中从FCMs中迁移出的非有意添加物(non intentionally added substance,NIAS)成为影响食品安全的重要因素而引起社会各界的广泛关注。由于NIAS非常复杂,且相当数量未知,其检测成为我国乃至全球食品接触材料安全评价的关键点及难点。在这篇综述中,以塑料食品接触材料和NIAS为主,介绍塑料材料中的NIAS来源、种类、国内外相关法律法规、近年来研究现状以及分析方法,最后对NIAS检测以及Orbitrap高分辨质谱检测技术的未来发展方向进行了展望。     

Migration of mineral oil,photoinitiators and plasticisers from recycled paperboard into dry foods: a study under controlled conditions

Migration from recycled paperboard was monitored after 2, 4 and 9 months of storage for six test foods industrially packed in five configurations, four with internal plastic films. After 9 months, the migration of mineral oil saturated hydrocarbons into foods directly packed in the paperboard amounted to 30–52 mg/kg, which corresponded to 65%–80% of those of a volatility up to that of the n-alkane C₂₄ in the paperboard. The concentration of the migrated aromatic hydrocarbons in the foods ranged from 5.5 to 9.4 mg/kg. More than half of this migration occurred in the first 2 months. Differences between the foods amounted to mostly less than a factor of 2 and seemed to be related to porosity or permeability more than fat content. Nine photoinitiators were detected in the paperboard, of which eight migrated into the packed food at up to 24%. Several plasticisers were present in the recycled paperboard, but only butyl phthalates showed significant migration. After 9 months, up to 40% of diisobutyl phthalate and 20% of dibutyl phthalate migrated into the food with direct contact. The internal polyethylene film hardly slowed migration, but the film and the tray absorbed approximately three times more mineral oil than the food, despite constituting merely 4% of the mass of the pack. Oriented polypropylene strongly slowed migration: The highest migration of saturated hydrocarbons measured after 9 months (2.3 mg/kg) corresponded to only 3% of the content in the paperboard and included migrated polyolefin oligomeric saturated hydrocarbons. Coating of polypropylene with an acrylate further slowed the migration, but the migration from the paperboard was still detectable in four of the six samples. Polyethylene terephthalate was a tight barrier.     

Determination of Phthalates into Vegetable Oils by Isotopic Dilution Gas Chromatography Mass Spectrometry

The presented method for the determination of a number of phthalic acid esters into oily media is based on their extraction by acetonitrile with precipitation under freezing and subsequent solid-phase extraction using alumina. This technique was checked as the best procedure to separate lipophilic phthalates from fatty media achieving elimination of contamination by excess use of solvents. Extracted phthalates are determined in acetonitrile solutions with gas chromatography in conjunction to isotopic dilution mass spectrometry using D4 isotopic labeled derivatives. Full validation of the method was carried out and background effect was examined. Method calibration for extraction from oil resulted in limit of detection (LOD) of 7–10 ng g^?1 and limit of quantification (LOQ) of 20–50 ng g^?1 for DMP, DEP, DiBP, DBP, DEHP, and BBP and in LOD 500 ng g^?1 and LOQ of 1,500 ng g^?1 for DiNP and DiDP. Real samples of virgin olive oil from olive press establishments from three different areas were analyzed and the phthalates content was below detection limit for all phthalic esters under consideration for nonindustrial areas and in measurable concentrations for industrial areas specifically with regard to DiBP.     

Determination of phthalic acid diesters in human milk at low ppb levels

Phthalic acid diesters (PAE) are omnipresent in the human environment and food is a major contributor to the overall human exposure towards these chemicals. Due to developmental effects, PAE infants’ exposure via human milk has been subjected to a number of analytical studies. These previous studies, however, revealed that normal laboratory blank values are in the range of or even higher than human milk levels due to the presence of PAE in laboratory environments. In order to provide more reliable data on PAE exposure via human milk, the aim of this study was to develop and validate a robust and sensitive analytical method. This should be capable of removing matrix components efficiently and guarantee limits of quantification in the low ppb range. The method development took into account liquid–liquid extraction and selective pressurised fluid extraction (sPFE) as well as chromatography-based clean-up steps. The final method consisted of a liquid–liquid extraction followed by an automated chromatographic clean-up by an sPFE device. After volume reduction the cleaned extracts were analysed by quadrupole GC/MS. Quantification was based on internal standards. An extensive quality assurance and method test programme demonstrated conservatively determined limits of detection and quantification from 0.3 to 10?ng?g^?1 in human milk, with recoveries of internal standards from 50% to 101%. Thus, the method allowed the quality-assured detection of di-isobutyl phthalate (DiBP), di-n-butyl phthalate (DBP), di-2-ethylhexyl phthalate (DEHP), di-allyl phthalate (DAP), benzylbutyl phthalate (BBP) and di-cyclohexyl phthalate (DcHP) in 30 human milk samples provided by 30 volunteers from southern Germany. DiBP, DBP and DEHP were the most commonly detected PAE, with median levels of 1.0, 0.6 and 2.3?ng?g^?1, respectively.     

Model studies of migration from paper and board into fruit and vegetables and into Tenax™ as a food simulant

Four samples of paper and board (P/B) of a type used for packaging dry foods were subjected to migration tests using mushrooms, apples, potatoes and bananas, and using the polymeric powder Tenax? as a food simulant. The P/B samples contained only low levels of diisopropylnaphthalene (DiPN) and diisobutyl phthalate (DiBP) and so the experiments were conducted after impregnating the P/B with added model substances. These were o-xylene, acetophenone, dodecane, benzophenone, DiPN and DiBP. Migration levels depended strongly on the nature of the substance and on the nature of the food and much less on the characteristics of the P/B, except insofar as they affected the contact area – flexible papers giving more extensive contact with the food than thick rigid board. Migration into Tenax? was at least a factor of 10 higher than migration into the fresh fruit and vegetables. The food samples were placed in contact with the P/B and then overwrapped loosely with aluminium foil and so this correction factor will tend to be conservative compared with a more open storage of the packed foods. Washing, peeling or cooking the fruits and vegetables after contact with the P/B had a surprisingly small effect on contaminant levels in general, and no one processing step was effective in giving a significant reduction of all the types of chemicals studied. This was because either they had penetrated into the food (so resisting peeling), or were not freely water-soluble (so resisting washing) or were not particularly volatile (so resisting loss by evaporation during cooking).