液相色谱-电感耦合等离子体质谱法测定大米中无机砷的不确定度评估

目的评估液相色谱-电感耦合等离子体质谱法(liquid chromatography inductively coupled plasma mass spectrometry, LC-ICPMS)测定大米中无机砷的不确定度。方法采用LC-ICPMS测定大米中As~Ⅲ和As~Ⅴ含量,建立数学模型,并从测量重复性、样品称量、提取液移取体积、标准溶液配制、标准曲线拟合等方面进行测量不确定度的计算。结果大米样品中As~Ⅲ、As~Ⅴ、i-As的含量分别为0.180、0.014、0.194 mg/kg,在95%的置信区间下,其扩展不确定度为0.003、0.002、0.028 mg/kg, k=2。结论测量过程中的不确定度主要来源于测量的重复性、标准溶液的配制和曲线拟合,需要在测量过程中加以注意。     

HPLC-ICP-MS法测定毛毛鱼中无机砷的不确定度评定

采用GB 5009.11-2014 《食品安全国家标准食品中总砷及无机砷的测定》中液相色谱-电感耦合等离子体质谱法测定毛毛鱼中的无机砷含量,参照CNAS-GL006《化学分析中不确定度的评估指南》和JJF1059.1-2012《测量不确定度的评定与表示》建立数学模型,对毛毛鱼中As(III)、As(V)的精密度、回收率进行验证,同时对试验过程中带来的不确定度分量进行了来源分析和评定。试验结果表明:当毛毛鱼中无机砷含量为0.096mg/kg时,无机砷i-As在95%的置信区间下扩展不确定度为0.007,测量过程中的不确定度最主要来源为校准曲线拟合和样品加标回收率。     

电感耦合等离子体质谱法测定米豆腐中镉元素的不确定度评价

目的对电感耦合等离子体质谱法测定米豆腐中镉元素的不确定度进行评价。方法样品经微波消解,超纯水定容,用电感耦合等离子体质谱法测定镉含量。分析标准溶液的配制、曲线拟合、样品称量、消解过程、定容体积、仪器测量重复性等影响不确定度的因素,按照JJF 1059.1-2012《测量不确定度评定与表示》中的方法进行合成,计算扩展不确定度。结果扩展不确定度为0.020 mg/kg,不确定度的影响因素从大到小依次为样品消解、样品重复测定、标准溶液配制、标准曲线拟合、样品定容、样品称量。结论本研究为电感耦合等离子体质谱法测量米豆腐中重金属元素的不确定度评价和质量控制提供参考。     

电感耦合等离子体质谱法测定食品包装纸中总砷的不确定度评估

为提高电感耦合等离子体质谱法(ICP-MS)测定食品包装纸中总砷含量结果的准确性,通过建立不确定度数学模型分析该方法评估不确定度的主要来源。结果表明:用该方法测定总砷含量主要包括两类不确定因素:A类不确定因素主要是方法的重复性影响所引起,B类不确定因素主要由样品制备过程中称量、消解、定容和测定过程中的标准溶液配制、曲线拟合等因素引起。     

电感耦合等离子体质谱法测定大米中总砷、镉和铅含量的不确定度评估

摘要：目的 评估电感耦合等离子体质谱法测定大米中总砷、镉和铅含量的不确定度。方法 依据GB 5009.268-2016,利用电感耦合等离子体质谱法（inductively coupled plasma mass spectrometry,ICP-MS）测定大米中总砷、镉和铅含量,按照CANS-GL 006：2018的评估方法,建立测量结果的不确定度评估模型,分析不确定度来源,计算不确定度分量并合成。结果 大米中总砷、镉和铅含量分别为0.0913、0.0793、0.0265 mg/kg,扩展不确定度分别为0.00828、0.00484、0.00322 mg/kg（k=2）。结论 影响总砷、镉和铅不确定度的主要因素为标准曲线拟合,其对总砷、镉和铅结果不确定度贡献率分别为90.2%、78.7%和92.9%;其次为标准溶液配制过程,而重复测定、加标回收和样品制备可忽略不计。     

电感耦合等离子体质谱法测定辣椒镉含量中不确定度的评估

摘要：目的 采用电感耦合等离子体质谱法(ICP-MS)测定辣椒中镉（Cd）含量,及评估测定过程产生的不确定度,以提高定量分析结果的可靠性。方法 建立数学模型,分析识别试样称量、试样定容、标准物质、标准溶液的配制、标准曲线的拟合、重复测量、回收试验等不确定度来源,量化各不确定度分量,计算合成标准不确定度。结果 辣椒中镉含量不确定度测定结果为：。结论 测定过程不确定度主要来源于标准溶液配制和标准曲线拟合。电感耦合等离子体质谱法测定辣椒中镉含量准确度高,重复性好,建立的不确定度评估能保证分析结果的质量。     

电感耦合等离子体质谱法测定荷花花粉和油菜花粉中镉含量的不确定度评定

目的评定荷花花粉和油菜花粉样品中镉含量可能产生的不确定度,以提高测量结果的准确性。方法采用NexIon 350X型电感耦合等离子体质谱仪对2种蜂花粉中镉的含量进行测定,建立实验过程的数学模型,对主要影响测量不确定度的样品称量、标准溶液的配制、标准曲线的拟合、测量的重复性等因素进行分析,并对各不确定度分量、合成标准不确定度以及扩展不确定度进行计算。结果荷花花粉中镉含量测定结果不确定度为:U=(0.166±0.010) mg/kg, k=2;油菜花粉中镉含量测定结果不确定度为:U=(0.0599±0.0033) mg/kg, k=2。结论影响测定荷花花粉和油菜花粉中镉含量的不确定度的主要来源为标准溶液稀释和样品重复性试验。电感耦合等离子体质谱法测定荷花花粉和油菜花粉中镉含量是可靠的。     

肠衣中12种磺胺类药物残留量测定的 不确定度分析

目的为保证实验室测试结果的准确性和可靠性,采用液相色谱-串联质谱法对肠衣中12种磺胺类药物残留量测定的不确定度进行评估。方法按照《测量不确定度评定与表示》的要求,对GB/T 20759-2006《畜禽肉中十六种磺胺类药物残留量的测定液相色谱-串联质谱法》进行肠衣中12种磺胺类药物测定的不确定度分析。结果建立了相应的数学模型,对测量结果的不确定度来源,如标准物质、标准溶液配制、样品称量、样品定容、样品回收率及结果的重复性等进行了量化分析。结论标准溶液的配制及稀释、样品回收率对样品的合成不确定度贡献较大。     

电感耦合等离子体质谱法测定肉制品中总砷的不确定度评定

目的评定电感耦合等离子体质谱法(inductively coupled plasma mass spectrometry,ICP-MS)测定肉制品中总砷含量的不确定度。方法依据CNAS-GL06:2006《化学分析中不确定度的评估指南》和JJF1135-2005《化学分析测量不确定度评定》,通过建立不确定度数学模型,采用微波消解-ICP-MS测定肉制品中的总砷含量,分析该方法测量不确定度的主要来源,并评定各标准不确定度的分量。结果在肉制品的总砷含量测定中,当样品的总砷含量为0.120 mg/kg,其扩展不确定度为0.008 mg/kg(k=2),结果表示为(0.120±0.008)mg/kg。结论用ICP-MS进行测量时,主要不确定度来源于样品的重复性测定、标准物质及配制、标准曲线拟合,通过降低可控不确定度来提高测量结果的准确度,该质量控制手段可用于合理地体现测定结果的可靠程度。     

ICP－MS法测定饮用水中铅砷镉的不确定度评定的研究

利用电感耦合等离子体质谱对饮用水中的Pb、As、Cd三种重金属测定不确定度进行分析,通过考察准溶液的配制、曲线拟合以及仪器测量重复性等因素对于待测元素不确定度的影响,标准溶液配制是ICP-MS测定饮用水中铅砷镉不确定度的主要影响因子,仪器重复性影响最小。     

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.