食品及食品包装材料溶剂残留检测方法研究概况

食品残留溶剂来源于生产加工过程或由食品包装材料带入,对人体健康存在潜在危害,食品中溶剂残留量的测定对于保证食品安全具有重要意义。本文论述了我国食品及食品包装材料溶剂残留的限量规定、检测的现行标准和技术规范。现行国家标准对食品和食品包装材料中残留溶剂的限量规定比较笼统,建议细化具体检测的残留溶剂种类并设定合理的限值。对食品及食品包装材料残留溶剂检测方法的相关文献进行了梳理总结。气相色谱法是分析残留溶剂的常用检测方法,具有专属性强、重现性好、灵敏度高等优点。本文对目前食品及食品包装材料残留溶剂检测存在问题和今后发展方向提出建议,为建立同时检测食品及食品包装材料多种残留溶剂的检测方法提供理论依据和文献参考。     

微波辅助萃取-气相色谱/串联质谱法同时测定皮革及其制品中21种有害有机溶剂的残留量

建立了1个气相色谱/串联质谱方法,对皮革及其制品中21种有害有机溶剂的残留量进行了同时测定,该方法以甲醇为萃取溶剂,微波萃取皮革及其制品中残留的有害有机溶剂,萃取液经硅胶固相萃取柱净化后,直接进行气相色谱/串联质谱分析,外标法定量。结果表明,21种有害有机溶剂的定量下限为15~100μg/kg。在3个加标浓度水平下,方法的加标平均回收率为80.3~94.6%,相对标准偏差为2.5~7.3%。该方法简单快速,灵敏度高,定性准确,定量下限低,定量下限远低于欧盟REACH法规的限量要求,可完全满足皮革及其制品中有害有机溶剂残留量检测工作的需要。应用该方法对市售皮革及其制品中残留的有害有机溶剂含量进行筛查,结果在部分样品中检出了不同含量水平的多种目标分析物。     

QuEChERS结合气相色谱-质谱法同时检测食品包装材料中20种光引发剂

目的 建立同时检测食品包装材料中20种光引发剂含量的检测方法。方法 采用QuEChERS技术结合气相色谱质谱联用法(GC-MS)建立食品包装材料中20种光引发剂同时测定方法。食品包装样品经乙酸乙酯超声辅助提取后，使用无水硫酸镁、N-丙基乙二胺(N-propyl ethylenediamine，PSA)、C18进行净化，再通过GC-MS在选择离子监测(SIM)模式下检测，外标法定量。结果 20种光引发剂在0.05~2.0 mg/L浓度范围内线性关系良好，相关系数均大于0.999；在0.2、0.4、2.0 mg/m2 3个浓度水平的加标回收率在70.6%～112.8%之间；相对标准偏差为1.2%～5.8% (n=6)，检出限为0.01～0.05 mg/m2。结论 该方法简单、灵敏、准确，适用于食品包装材料中20种光引发剂残留量的快速分析检测。     

聚乙烯醇纳米复合膜中残留戊二醛含量的测定

戊二醛作为聚乙烯醇基纳米复合包装材料的交联剂能提高纳米复合材料的综合包装性能,但戊二醛的残留会影响食品包装材料的安全性。对聚乙烯醇纳米复合膜样品采用超声萃取其中残留的戊二醛,并与2,4-二硝基苯肼(DNPH)衍生化后,用高效液相色谱法(HPLC)检测其残留出的戊二醛含量,结果显示:该方法在0.2～5.0mg/L范围内线性相关系数为r2=0.9997,平均回收率达到76.8%～87.3%,相对标准偏差为2.83%～4.08%,最低检测浓度为0.2mg/kg,说明采用的萃取条件及色谱分析方法适合聚乙烯醇基纳米复合膜中戊二醛残留量的测定;待测聚乙烯醇基纳米复合膜中残留戊二醛的含量24.55mg/kg,符合食品包装材料安全限量标准。     

微波萃取-GC/MS-MS测定乙二醇醚类有机溶剂

建立了气相色谱/串联质谱方法,测定纺织品中残留的15种乙二醇醚类有机溶剂。该方法以乙醇为萃取溶剂,100℃下微波萃取纺织品中残留的乙二醇醚类有机溶剂,萃取液直接进行气相色谱/串联质谱分析,外标法定量。在信噪比(S/N)为10的条件下,各组分的定量下限为5~20 mg/kg。在三个加标水平下,平均回收率为81.7%~94.5%,相对标准偏差为2.1%~6.8%。该方法简单快速,可满足纺织品中乙二醇醚类有机溶剂残留量检测的技术要求。     

塑料食品包装材料中溶剂残留的探讨

塑料食品包装材料的安全性对食品安全有着重要影响。简要介绍国内外关于塑料食品包装材料中溶剂残留的相关标准以及检测的方法,分析影响溶剂残留的主要因素,并提出溶剂残留的控制对策。     

食品包装材料中柠檬酸酯类增塑剂GC/MS/SIM分析

为研究食品包装材料中柠檬酸酯类增塑剂的含量,采用超声辅助二氯甲烷萃取,GC/MS/SIM的检测方式,建立食品包装材料中柠檬酸酯类增塑剂含量的检测方法。结果表明,柠檬酸酯类增塑剂含量在0.001~0.1 mg/mL范围内呈良好线性,线性相关系数R~20.99,检出限范围为0.061~0.066μg/g。2种柠檬酸酯类增塑剂的平均回收率为91.46%~107.73%,RSD为1.69%~4.73%(n=6)。运用该方法检测26种食品包装材料,仅有4种包装材料中存在柠檬酸三丁酯和乙酰柠檬酸三丁酯2种增塑剂。     

毒死蜱等7种农药残留在玉米酿酒加工过程中的 迁移与降解规律

目的开发了多残留检测方法并研究了以玉米为原料发酵加工白酒酿造过程中的几种农药残留变化及残留浓度。方法用改进的QuEChERS方法进行样品前处理,采用气相色谱-质谱法(gas chromatography-mass spectrometry,GC-MS)对毒死蜱等7种农药残留水平及残留浓度进行检测。结果玉米和白酒中7种农药的添加回收率在81%~95%之间,方法检出限均在1~10μg/kg之间,定量限均在3~30μg/kg之间。随着发酵时间的延长,毒死蜱等7种农药的残留水平1~14 d内降低缓慢;蒸馏后的轻组分酒液样品中有痕量农药残留检出。结论发酵并不引起测试的农药残留显著降解,但酿酒过程农药迁移率很低,白酒中农药残留风险不高。     

高效萃取吸管-在线凝胶色谱-气相色谱-质谱法测定淡水鱼中的农药残留量

目的 建立一种在线凝胶色谱-气相色谱-质谱(gel permeation chromatography coupled with gas chromatography-mass spectrometry, GPC-GC/MS)联用法测定淡水鱼中农药残留的检测方法。方法 采用超声辅助技术和高效萃取吸管法对南昌地区淡水鱼样品净化处理, 以乙腈为提取液, 采用氯化钠去除水分后, 经在线GPC-GC-MS系统进样分析, 选择离子检测方式定量检测。结果 25种化合物的质量浓度在一定范围内与其对应的峰面积有良好的线性关系, 相关系数大于0.996, 方法的检出限为9.1×10?5~3.1×10?1 mg/kg。以空白样品为基体进行加标回收实验, 回收率为71.4%~103.2%, 相对标准偏差小于9%。结论 该方法前处理简单快速, 灵敏度高, 有机溶剂使用量少, 适用于淡水鱼中农药残留的检测。     

RP-HPLC法测定织物中残留有机溶剂方法研究

随着多个国家针对纺织品中有机溶剂残留相关限制法规和标准的出台,纺织品中溶剂残留检测已成为生态纺织品检测体系中的一个重要项目。文中采用超纯水机械萃取,反相高效液相法(RPHPLC)同时检测纺织品中N,N-二甲基甲酰胺(DMF)、N,N-二甲基乙酰胺(DMAc)和N-甲基吡咯烷酮(NMP)3种残留溶剂。结果表明,3种残留溶剂均具有良好的线性关系,其相关系数均大于0.999,方法检出限为1.1~2.8 mg/kg。各类纺织品中3种有机溶剂的加标回收率在94.8%~103.0%之间,实际样品测定表明该测试方法能满足织物中3种有机溶剂的日常检测要求。     

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.     

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.     

Analysis for organic residues from aids to polymerization used to make plastics intended for food contact

Polymers intended for food contact use have been analysed for organic residues which could be attributed to a range of substances employed as polymerization aids (e.g. initiators and catalysts). A wide range of polymers was extracted with solvents and the extracts analysed by gas chromatography-mass spectrometry (GC-MS). The overwhelming majority of substances identified were not derived from aids to polymerization but were oligomers, additives and adventitious contaminants. However, a small number of substances were identified as initiator residues. These included tetramethylsuccinonitrile (TMSN) which was observed in two polymers and it derived from recombination of two azobisisobutyronitrile (AIBN) initiator radicals. Methyl benzoate, benzoic acid, biphenyl and phenyl benzoate were detected in one poly(methyl methacrylate) sample and in two polyvinylchlorides and they are thought to be derived from benzoyl peroxide initiator. TMSN was subsequently targeted for analysis of poly-(methyl methacrylate) plastics using proton nuclear magnetic resonance spectrometry (¹     

Tests of potential functional barriers for laminated multilayer food packages. Part II: Medium molecular weight permeants

Experiments were performed to characterize the kinetics of the permeation of different medium molecular weight model permeants: bisphenol A, warfarin and anthracene, from liquid paraffin, through a surrogate potential functional barrier (25 microns-thick orientated polypropylene--OPP) into the food simulants olive oil and 3% (w/v) acetic acid. The characterization of permeation kinetics generally observed the permeation models previously reported to explain the experimental permeation results obtained for a low molecular weight group of model permeants. In general, the model permeants exhibited behaviour consistent with their relative molecular weights with respect to (a) the time taken to attain steady-state permeation into the food simulant in which they were more soluble, (b) their subsequent steady-state permeation rates, and (c) their partition between liquid paraffin and the OPP membrane.     

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.     

The Ministry of Environmental Protection Issued "Feasible Technology Guidelines for Pollution Prevention and Control in Wood Pulping Process of the Paper Industry (Trial)" and Two Other Guiding Technical Documents

On December 27t＂, 2013, the Ministry of Environmenta Protection announced that, in order to implement ＂The Environmental Protection Law of the People＇ s Republic of China＂, improve the working system in environmenta protection technologies, and promote technologica advancement in pollution prevention, the Ministry of Environmental Protection sponsored the formulation of three guiding technical documents including ＂Feasible Technology Guidelines for Pollution Prevention and Contro n Wood Pulping Process of the Paper Industry （Trial）＂     

1~(st) Intelli-Tissue~ EcoEc Tissue Machine Supplied by PMP Group Successfully Put into Operation in China

正On April 29th,2014,Intelli-Tissue EcoEc tissue machine supplied by PMP Group successfully put into operation at Hebei Xuesong Paper Co.,Ltd.,this is the first such kind of paper machine of PMP Group in China.