高效液相色谱法测定蔬菜中异菌脲残留量的不确定度分析

采用高效液相色谱法对蔬菜中异菌脲残留量的不确定度进行评估。根据JJF 1135—2005《化学分析测量不确定度评定》和JJF 1059.1—2012《测量不确定度评定与表示》中的有关规定,建立测定蔬菜中异菌脲残留量不确定度的数学模型,逐层对不确定度来源进行分析。通过对不确定度分量进行量化和合成,得出当蔬菜中异菌脲残留量为5.31 mg/kg时,其扩展不确定度为0.40 mg/kg(k=2)。结果表明,影响检测结果的主要因素为标准溶液配制、标准曲线拟合和测量重复性等。     

水果和蔬菜中抗蚜威残留检测的不确定度评定

对GB/T 19648-2006水果和蔬菜中500种农药及相关化学品残留量的测定气相色谱-质谱法测定蔬菜、水果中抗蚜威的残留量的不确定度进行了评定。通过建立数学模型,分析和评定了标准曲线、试样称量、加标回收率等主要不确定度分量,并计算了测量结果的合成不确定度和扩展不确定度。各不确定度分量中加标回收率、校准曲线和标准溶液的配制对合成不确定度的贡献较大。     

气相色谱-三重四极杆质谱法测定蔬菜中氟虫腈残留量的不确定度评定

目的对气相色谱-三重四极杆质谱法测定蔬菜中氟虫腈残留量的方法进行不确定度评估。方法根据JJF 1059.1-2012《测量不确定度评定与表示》和JJF 1135-2005《化学分析测量不确定度评定》中有关规定,建立了用内标法测定蔬菜中氟虫腈残留量不确定度评估的数学模型,对测定中的不确定度来源进行分析和评估。结果对不确定的分量进行量化和合成,结果表明,当蔬菜中氟虫腈残留量为0.02 mg/kg时,扩展不确定度为0.0096 mg/kg,氟虫腈残留量表示为(0.02±0.0096)mg/kg(k=2)。结论实验过程中的不确定度主要来源于标准溶液的配制和样品的稀释等过程,本评估方法可为气相色谱-三重四极杆质谱法的不确定评估提供依据。     

气相色谱法测定蜂蜜中马拉硫磷残留量的不确定度评定

评定气相色谱法测定蜂蜜中马拉硫磷残留量的不确定度。方法 参照JJF 1059.1-2012《测量不确定度评定与表示》和JJF1135-2005《化学分析测量不确定度评定》, 建立气相色谱法测定蜂蜜中马拉硫磷残留量的不确定度的数学模型, 对测量过程中各测量不确定度分量进行分析和计算。结果 通过对各测量不确定度分量的计算和合成,蜂蜜样品中马拉硫磷的残留量为0.021 mg/kg, 扩展不确定度为0.0037 mg/kg(k=2)。结论 气相色谱法测定蜂蜜中马拉硫磷残留量的不确定度主要来源为标准曲线的拟合, 其次是样品测量重复性和标准溶液, 而回收率与样品前处理影响较小。     

气相色谱-质谱法测定芹菜中甲拌磷残留量的 测量不确定度评定

目的评定气相色谱-质谱法对阳性芹菜样品中甲拌磷残留量测定不确定度。方法参照JJF1135-2005《化学分析测量不确定度评定》和JJF1059.1-2012《测量不确定度评定与表示》,建立气相色谱-质谱法测定芹菜样品中甲拌磷残留量不确定度评定的数学模型,对测定过程中不确定度分量来源进行分析和评定。结果通过对不确定度各分量进行量化和合成,结果表明阳性芹菜样品中甲拌磷的残留量为0.021 mg/kg,扩展不确定度为0.003 mg/kg (k=2)。结论整个测定过程中,标准曲线配制过程所产生的不确定度分量最大,其次为方法重复性和测量重复性产生的分量,这为本实验室内部质量控制提供了依据。     

高效液相色谱法测定食品中桔青霉素的不确定度分析

采用高效液相色谱法对食品中桔青霉素残留量测定的不确定度进行评估。依据JJF 1135-2005《化学分析测量不确定度评定》和JJF 1059.1-2012《测量不确定度评定与表示》规定的测量不确定度的基本方法,建立数学模型,分析食品中桔青霉素的不确定度来源,通过对不确定度分量进行量化和合成,得出当食品中桔青霉素残留量为154μg/kg时,其扩展不确定度为8.6μg/kg(k=2)。评定结果表明,影响检测结果的主要因素为标准曲线拟合、样品前处理过程和测量重复性等。     

豆腐皮中乌洛托品残留量的测定不确定度评估

目的评定液相色谱-质谱法测定豆腐皮中乌洛托品留量的不确定度。方法运用JJF 1059.1-2012《测量不确定度评定与表示》分析豆腐皮中的乌洛托品残留量测量过程中的不确定度来源,通过建立数学模型量化不确定度分量,计算合成不确定度和扩展不确定度。结果本方法的不确定度主要来源于液相色谱质谱仪设备。当豆腐皮中乌洛托品残留量为0.523 mg/kg,扩展不确定度为0.018 mg/kg,乌洛托品残留量表示为(0.523±0.018)mg/kg(k=2)。结论该评定方法可为液相色谱-质谱法测定豆腐皮中乌洛托品残留量的结果和方法的可靠性提供科学依据。     

气相色谱-串联质谱法测定果汁中毒死蜱残留量的不确定度评定

目的评定气相色谱-串联质谱法测定果汁中毒死蜱残留量的不确定度。方法依据国家计量技术规范JJF 1059.1-2012《测量不确定度评定与表示》对毒死蜱测定中的不确定度来源进行分析,通过建立数学模型量化不确定度分量,计算合成不确定度和扩展不确定度。结果本方法的不确定度主要来源于标准曲线的配制和样品的稀释过程。当果汁中毒死蜱残留量为41.1μg/kg,扩展不确定度为9.8μg/kg,毒死蜱残留量表示为(41.1±9.8)μg/kg(k=2)。结论该评定方法可用于气相色谱-串联质谱法对果汁中毒死蜱残留量的不确定分析。     

顶空-气相色谱法测定橄榄油中六号溶剂残留量的不确定度评定

目的评定顶空气相色谱法测定橄榄油中六号溶剂残留量的不确定度。方法运用JJF 1059.1-2012《测量不确定度评定与表示》分析橄榄油中六号溶剂残留量测量过程中的不确定度来源,通过建立数学模型量化不确定度分量,计算合成不确定度和扩展不确定度。结果本方法的不确定度主要来源于标准溶液的配制。当橄榄油中六号溶剂残留量为123.6 mg/kg,扩展不确定度为8.8 mg/kg,六号溶剂残留量表示为(123.6±8.8)mg/kg(k=2)。结论该评定方法可为顶空气相色谱法对橄榄油中六号溶剂残留量的测量结果和方法的可靠性提供科学依据。     

高效液相色谱法测定鲜虾中4-己基间苯二酚残留量的不确定度分析

采用高效液相色谱法对鲜虾中4-己基间苯二酚残留量测定的不确定度进行评估。根据JJF1135-2005《化学分析测量不确定度评定》和JJF1059.1-2012《测量不确定度评定与表示》规定的测量不确定度的基本方法,建立数学模型,分析鲜虾中4-己基间苯二酚残留量测定的不确定度的来源,并对各不确定度分量进行量化和合成,得到当鲜虾中的检测结果为1.01 mg/kg时,其扩展不确定度为0.094mg/kg(k=2)。通过评定比较各影响分量可知,影响检测结果的不确定度的主要因素为待测物浓度和回收率,重复性测定次之,样品称量、试样定容引入的不确定度较小。     

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.     

Focus on China's Paper Industry

In the English section of this issue, 〈China Paper Newsletters〉 will introduce ＂National Development and Reform Commission Issued Announcement for Selection of Major Preliminary Research Projects for the ＇13th Five-Year Plan＇＂, ＂2013 Annual Report of China＇s Paper Industry＂, and news of projects and other policies.     

Listen to downstream & search for innovation

正Nowadays,textile enterprises are all taking efforts in transformation and upgrading,like improving producing capacity and optimizing production structure to face market downturn.It claimed a higher request to the standard of textile equipments.In the upcoming of ITMA ASIA+CITME 2014exhibition,this magazine have interviewed several branch associations and a series of relative enterprises,to summarize industrial developing status