高效液相色谱法同时测定鳗鱼及其制品中八种磺胺类药物

建立了高效液相色谱测定鳗鱼及其制品中磺胺嘧啶、磺胺甲基嘧啶、磺胺二甲嘧啶、磺胺甲氧嗪、磺胺甲嗯唑、磺胺间甲氧嘧啶、磺胺间二甲氧嘧啶、磺胺喹嗯啉等八种磺胺类药物残留量的方法。研究了鳗鱼及其制品中八种磺胺类药物残留的提取、净化和高效液相色谱条件。样品经二氯甲烷提取、MCX阳离子固相萃取小柱净化，以Cloversil C18柱，甲醇、1％乙酸(V／V)梯度洗脱分离，紫外检测器检测、外标法定量。结果表明，样品添加0．1mg／kg的回收率为80％～93％，定量测定低限为0．02mg／kg。方法已应用于实际样品的测定。     

高效液相色谱法同时测定水产品中13种磺胺类药物残留的研究

建立了一种同时测定水产品(鳗鱼、鮰鱼、龙虾)中13种磺胺类药物残留的高效液相色谱法。样品经乙腈提取,正己烷液-液分配,阳离子固相萃取小柱净化后,采用高效液相色谱分离,紫外检测器检测,外标法定量。13种磺胺类药物在0.1～5.0μg/ml范围内线性关系良好,相关系数R2为0.9997～0.9999,加标回收率为62%～97%,相对标准偏差为2.01%～10.46%。定量测定低限磺胺二甲嘧啶、磺胺甲氧嘧啶、磺胺-6-甲氧嘧啶、磺胺氯哒嗪、磺胺甲基异恶唑、磺胺二甲异恶唑、磺胺间二甲氧嘧啶、磺胺喹恶啉为0.02mg/kg,磺胺嘧啶、磺胺吡啶、磺胺噻唑、磺胺甲基嘧啶、磺胺甲噻二唑为0.05mg/kg。     

牛奶中多种磺胺类抗生素残留的HPLC快速分析

研究了牛奶中磺胺嘧啶、磺胺甲基嘧啶、磺胺二甲基嘧啶、磺胺甲噁唑、磺胺间甲氧嘧啶、磺胺二甲氧嘧啶六种磺胺类抗生素的多残留高效液相色谱(HPLC)分析方法。样品经氯仿-丙酮(2:1,V/V)提取两次,提取液浓缩至干。残渣用流动相甲醇-0.08%乙酸(60:40,V/V)溶解,净化后以反相C18柱,甲醇-0.08%乙酸等度洗脱,紫外检测器检测、外标法定量。结果表明,这六种抗生素在0.01～1.0mg/L浓度范围内呈线性关系,磺胺嘧啶、磺胺甲基嘧啶、磺胺二甲基嘧啶检的检出限为0.010mg/L、磺胺甲噁唑、磺胺间甲氧嘧啶、磺胺间二甲氧嘧啶检出限分别为0.015mg/L。分析的添加回收率为69.4%～123.5%,变异系数为<8%,整体分析时间小于3h。方法具有处理简单、检测快速、准确的特点。     

高效液相色谱-荧光检测法测定水产品中4种磺胺类药物残留量

建立高效液相色谱-荧光检测法测定水产品中4种磺胺类药物残留量的方法。均质后的样品用乙酸乙酯提取,稀盐酸反萃取,正己烷脱脂,荧光胺衍生,反相色谱柱分离,荧光检测器检测,磺胺5-甲氧嘧啶为内标物,内标法定量。4种磺胺类药物磺胺嘧啶、磺胺甲基嘧啶、磺胺二甲基嘧啶和磺胺甲基异噁唑的线性范围为0.01～0.2mg/kg,线性相关系数均大于0.9934;在0.01～0.2mg/kg 范围内四个添加水平范围内的平均回收率为83.0%～91.3%,相对标准偏差为3.89%～8.80%,方法检出限为0.01mg/kg。     

RP-HPLC快速分析牛奶中六种磺胺类抗生素残留

研究了牛奶中磺胺嘧啶、磺胺甲基嘧啶、磺胺二甲基嘧啶、磺胺甲噁唑、磺胺间甲氧嘧啶、磺胺二甲氧嘧啶六种磺胺类抗生素的多残留反相高效液相色谱(RP-HPLC)分析方法.样品经超声波提取两次,提取液浓缩至干.残渣用流动相甲醇-0.08%乙酸(60:40,V/V)溶解,净化后以反相C18柱,甲醇-0.08%乙酸等度洗脱,紫外检测器检测、外标法定量.结果表明,这六种抗生素在0.01～1.0mg·L-1浓度范围内呈线性关系,磺胺嘧啶、磺胺甲基嘧啶、磺胺二甲基嘧啶的栓出限为0.010mg·L-1、磺胺甲噁唑、磺胺间甲氧嘧啶、磺胺间二甲氧嘧啶的检出限为0.015mg·L-1.分析的添加回收率达到80%以上,变异系数＜9.0%,整体分析时间小于3h.方法具有处理简单、检测快速、准确的特点.     

高效液相色谱-在线柱后衍生荧光检测法同时测定水产品中14种磺胺类药物残留

建立水产品中14种磺胺类药物的高效液相色谱-柱后衍生荧光检测法。均质后的水产品试样用乙酸乙酯提取、盐酸溶液反萃取、正己烷脱脂、反相色谱柱分离、在线柱后衍生、荧光检测器检测、内标法定量。14种磺胺类药物(磺胺、磺胺嘧啶、磺胺噻唑、磺胺甲基嘧啶、磺胺5-甲氧嘧啶、磺胺二甲基嘧啶、磺胺甲氧哒嗪、磺胺氯哒嗪、磺胺6-甲氧嘧啶、磺胺甲基异噁唑、磺胺多辛、磺胺异噁唑、磺胺二甲氧哒嗪、磺胺喹噁啉)的线性范围为2.5～800μg/L,线性相关系数均大于0.9934;在2.5～200μg/kg三个添加水平范围内的平均回收率为88.9%～98.6%,相对标准偏差均小于6.96%。14种磺胺类药物的定量检出限为2.5～20μg/kg。方法重现性好、灵敏度高,杂质干扰少,广泛适用于水产品中磺胺类药物残留的检测。     

液相色谱-荧光检测法同时测定肠衣中八种磺胺类兽药残留

建立了一种专属性强的高效液相色谱-同时测定肠衣中八种磺胺类药物残留(磺胺嘧啶、磺胺间甲氧嘧啶、磺胺甲基嘧啶、磺胺对甲氧嘧啶、磺胺喹恶啉、磺胺甲基异恶唑、磺胺甲氧嗪和磺胺二甲嘧啶)的检测方法。采用1%乙酸/乙腈对肠衣中的磺胺类药物残留进行提取,用正己烷净化,净化后的样品,经荧光胺衍生,供液相色谱仪测定。实验结果表明,八种磺胺药物在2.00～5.00×102ng/ml浓度范围内,具有良好的线性关系,线性相关系数在0.9982～0.9997,添加浓度为5～50ng/ml时,回收率在63.7%～87.8%之间,该方法的最低检测限为5ng/ml,完全可以达到日常检测要求。     

采用超高效液相色谱串联质谱法检测饲料中3种磺胺类药物

用超高效液相色谱串联质谱法测定饲料中磺胺嘧啶、磺胺甲基嘧啶和磺胺二甲基嘧啶含量.结果显示:磺胺药物浓度与仪器响应值的相关系数0.996 7～0.999 2,方法的检出限为10μg/kg,加标回收率87.67％～100％,相对标准差1.3％～4.3％,精密度相对标准差3.50％～4.40％.表明回收率、相对标准差和精密度符合相关要求,此方法可快速、高效、准确检测饲料中磺胺类药物,同时该方法还可以扩充到其他磺胺类药物的检测.     

高效液相色谱-串联质谱法同时测定鸡脂肪中磺胺嘧啶、甲氧苄啶的残留量

目的建立高效液相色谱-串联质谱法(highperformanceliquidchromatography-tandemmass spectrometry, HPLC-MS/MS)同时测定鸡脂肪中磺胺嘧啶、甲氧苄啶的残留量的方法。方法样品经乙腈2次提取,以乙腈和0.1%甲酸水溶液为流动相进行溶解后,用正己烷2次脱脂,过滤膜后用于液相色谱串联质谱仪测定,基质添加标准溶液外标法定量。结果 0.5～100 ng/mL的浓度范围内磺胺嘧啶、甲氧苄啶色谱峰面积与浓度呈良好线性相关,相关系数均大于0.99;方法定量限为1.0μg/kg;鸡脂肪样品中磺胺嘧啶、甲氧苄啶在1.0～200.0μg/kg添加水平内的平均回收率在66.3%～97.5%之间,批内批间相对标准偏差均小于20%。结论该方法回收率满足残留检测要求,且方法的重现性良好,满足国内外兽药残留相关法规规定。     

乳中磺胺甲基嘧啶残留酶联免疫测定

以BSA为载体合成两种不同摩尔比值（1：13和1：42）磺胺甲基嘧啶抗原,并比较其免疫原性;以OA为载体合成一种包被抗原;用过氧化物酶标以鼠抗免IgG;建立乳中磺胺甲基嘧啶残留酶联免疫测定。抗体亲和常数分别为1．28×107（1：42）和3．21×107（1：13）。ELISA测定磺胺甲基嘧啶工作浓度5～220ng／ml（1．87×10－8～8．2×10－7mol／L）,检测限为2．4ng／ml,回收率为88～118％,与磺胺二甲基嘧啶和磺胺噻唑交叉反应率分别为6．0％和0．84％,与碘胺二甲氧嘧啶和磺胺咪无交叉反应。     

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.