青稞真菌毒素检测分析

采集甘肃、西藏、青海、四川四省共299份青稞样品,采用高效液相色谱串联质谱方法对其13种真菌毒素进行检测分析.结果表明:4个省份青稞样品中13种真菌毒素均未超标,仅检出T-2毒素(T-2 Toxin)、玉米赤霉烯酮(Zearalenone,ZEN).青海部分地区T-2检出率为49.26％;四川部分地区T-2、ZEN,检...     

液相色谱-串联质谱同时测定食用植物油中的多种真菌毒素

基于分步液液提取以及脂质净化柱净化的样品前处理方式,建立同时测定食用植物油中28种真菌毒素的高效液相色谱-串联质谱的测定方法。28种真菌毒素的定量限范围0.07～1.25μg/kg,三水平加标回收率范围60%～120%,峰面积相对标准偏差小于12.5%,均满足国家标准GB/T 27404-2008《实验室质量控制规范食品理化检测》中实验室质量控制规范以及真菌毒素限量标准的要求。应用本方法对市售食用植物油样品进行真菌毒素的风险监测,结果显示:黄曲霉毒素、玉米赤霉烯酮及其衍生物、杂色曲霉素、T-2毒素有不同程度的检出。其中,花生油中主要的真菌毒素种类为黄曲霉毒素、杂色曲霉素以及玉米赤霉烯酮;菜籽油和玉米油中主要的真菌毒素种类为玉米赤霉烯酮及其衍生物。     

免疫亲和层析及其在真菌毒素检测中应用

该文简介免疫亲和层析工作原理,载体要求与选择,免疫亲和柱制备与使用,重点综述免疫亲和层析在黄曲霉毒素,赭曲霉毒素,玉米赤霉烯酮,脱氧雪腐镰刀菌烯醇,伏马毒素,T-2毒素等真菌毒素检测中应用最新进展。     

河北省小麦、玉米及其制品中16种真菌毒素污染水平调查与分析

目的调查分析河北省小麦、玉米及其制品中16种常见真菌毒素污染状况。方法收集河北省37份鲜(冻)玉米/玉米粒、74份玉米、玉米面制品以及240份小麦样品。样品经乙腈:水:甲酸(79:20:1, V:V:V)溶液超声离心提取后,通过同位素内标稀释法处理,采用液相色谱-串联质谱法进行检测。结果伏马毒素小麦检出8份,玉米、玉米面制品检出66份,检出范围为ND~3889.9μg/kg;玉米赤霉烯酮检出小麦检出2份,玉米、玉米面制品检出69份,检出范围为ND~323.2μg/kg;脱氧雪腐镰刀菌烯醇小麦检出122份,玉米、玉米面制品检出68份,检出范围为ND~4183.4μg/kg;3-乙酰基-脱氧雪腐镰刀菌烯醇小麦检出5份,玉米、玉米面制品检出18份;15-乙酰基-脱氧雪腐镰刀菌烯醇小麦检出12份,玉米、玉米面制品检出38份;其他毒素均为未检出。鲜(冻)玉米/玉米粒中16种真菌毒素均未检出。结论伏马毒素、玉米赤霉烯酮和脱氧雪腐镰刀菌烯醇为小麦、玉米及其制品的主要污染物,其污染状况应引起关注。     

烟台市售谷类及其制品中真菌毒素污染状况调查分析

为了解烟台市谷类及其制品中真菌毒素的污染状况,采用随机采样方法,2014年4月~2017年9月在烟台辖区11个监测点采集4类225种样本,按照《国家食品污染物和有害因素风险监测工作手册》规定的真菌毒素标准操作程序,进行15种真菌毒素的检测。结果表明,烟台市玉米及其制品、小麦及其制品普遍存在不同种类真菌毒素污染,而大米、小米均未检出,检出率为52.44%,超标率2.22%。小麦及其制品中主要检出15-乙酰脱氧雪腐镰刀菌烯醇(15-acetyldeoxynivalenol,15-Ac-DON)、脱氧雪腐镰刀菌烯醇(deoxynivalenol,DON)、伏马菌素B1,检出率分别为0.8%、55.2%、0.24%,伏马菌素B1仅存在小麦(原粮)中,15-Ac-DON则仅存在湿面条中。小麦及其制品中DON均有检出,均值73.86μg/kg,馒头、面条(干、湿)、面包中DON的样本检出率100%,小麦粉为40%,小麦(原粮)为20%。玉米及其制品中真菌毒素检出率为53.85%,主要存在伏马菌素(B1、B2、B3)、玉米赤霉烯酮(Zearalenone,ZEN)、DON、15-Ac-DON、赭曲霉毒素A(Ochratoxin A,OTA)、黄曲霉毒素B1(Aflatoxin B1,AFB1)、黄曲霉毒素B2(Aflatoxin B2,AFB2),检出率分别为32.97%、19.78%、26.37%、21.98%、17.58%、13.19%、8.79%、4.40%、2.20%;而T-2毒素、黄曲霉毒素G1(Aflatoxin G1,AFG1)、黄曲霉毒素G2(Aflatoxin G2,AFG2)检出率均为1.10%;玉米油中仅检出ZEN,检出率51.85%,均值126.68μg/kg。小麦及其制品和玉米其制品中均在毒素多重混合污染同一样本状况,2种及以上真菌毒素的多重污染率13.33%,3种毒素多重污染率最高为5.33%,玉米及其制品多重污染水平高于小麦及其制品。     

免疫亲和柱净化-HPLC法同时测定玉米制品中的赭曲霉毒素A和玉米赤霉烯酮

建立了同时测定玉米制品中赭曲霉毒素A和玉米赤霉烯酮的免疫亲和柱净化高效液相色谱方法。试样经乙腈-水溶液(体积比80?20)提取,复合免疫亲和柱富集和净化后,采用Syncronis C18色谱柱(250 mm×4.6 mm,5μm)固定相,以0.5%冰乙酸-乙腈-甲醇(体积比10?45?45)为流动相,等度洗脱,荧光检测器检测(Ex:333 nm,Em:470 nm)。结果表明:赭曲霉毒素A和玉米赤霉烯酮检出限分别为5.65×10-2μg/kg和4.53×10-1-μg/kg;标准曲线的线性范围分别为1~50 ng/mL(r=0.9999)和10~500 ng/mL(r=0.9999);3个不同水平的加标平均回收率为95.81%~98.31%,RSD值为1.24%~1.65%。20批试样中赭曲霉毒素A和玉米赤霉烯酮测定值分别为0.59~0.69μg/kg和3.84~5.22μg/kg,均无过量残留。该方法具有操作简便、灵敏度高、重现性佳等优点,适用于同时检测玉米制品中赭曲霉毒素A和玉米赤霉烯酮。     

肉制品中真菌毒素污染现状与控制研究进展

简要介绍了肉制品中常见真菌毒素(黄曲霉毒素、赭曲霉毒素、脱氧雪腐镰刀菌烯醇、玉米赤霉烯酮、展青霉素、桔霉素)的来源及其危害,重点介绍了肉制品中常见真菌毒素的污染现状及其控制方法,并展望了肉制品中真菌毒素未来的研究方向。     

高效液相色谱法同时测定谷物中的赭曲霉毒素和玉米赤霉烯酮

采用反相高效液相色谱法同时测定谷物中的赭曲霉毒素和玉米赤霉烯酮.以ODS C18(250mmx4.6mm,5μm)为色谱柱,乙腈-2%乙酸(两者体积比40:60)为流动相,荧光检测器检测, Ex 325nm, Em 455 nm.赭曲霉毒素A和玉米赤霉烯酮的线性范围分别为1～100μg/L和10～100)μg/L,检出限分别为0.025 ng和0.26 ng.5种样品的检测中两种生物毒素的加标回收率在75%～110%之间.该方法灵敏、准确,适用于谷物中赭曲霉毒素和玉米赤霉烯酮的栓测.     

白酒酒醅中真菌毒素的检测

该实验建立了白酒生产原料酒醅中31种真菌毒素的液相色谱-串联质谱检测方法。样品使用乙腈与1%的甲酸水混合溶液（85∶15,V/V）提取,经QuEChERS法净化后,采用多反应监测模式（MRM）检测,可同时对31种真菌毒素进行定性定量分析。结果表明,该方法的相关系数R2为0.991～0.999,线性关系良好,检出限和定量限分别为0.1～5.0 μg/kg和0.4～16.5 μg/kg,平均回收率为83.1%～108.7%,回收率实验结果的相对标准偏差（RSD）为2.5%～9.6%。对10个随机抽取的酒醅样品进行检测,检出的真菌毒素分别有：黄曲霉毒素、脱氧雪腐镰刀菌烯醇及其衍生物、T-2毒素、新茄病镰刀菌烯醇、玉米赤霉烯酮、赭曲霉毒素、杂色曲霉素。该方法的灵敏度、准确度和精密度良好,可满足白酒生产原料中31种真菌毒素的检测。     

大米中16种真菌毒素同时检测分析

目的建立大米中黄曲霉毒素、伏马毒素、雪腐镰刀菌烯醇、脱氧雪腐镰刀菌烯醇类毒素、玉米赤霉烯酮、赭曲霉毒素A、T-2毒素、HT-2毒素以及杂色曲霉毒素等16种真菌毒素便捷准确的液相色谱-串联质谱法。方法大米样品经粉碎均质后采用70%甲醇水溶液浸泡提取,通过PriboFastRM226多功能净化柱净化,利用液相色谱串联质谱的多反应监测模式进行测定分析,采用内标法定量。结果 16种真菌毒素均具有良好的线性关系(r0.99),3个加标水平回收率为85.2%～102.8%,相对标准偏差范围为2.05%～4.75%。在61件大米检测中,共有5件样品检出真菌毒素,检测到的真菌毒素有5种,其中雪腐镰刀菌烯醇、伏马毒素B_1、伏马毒素B_2、15-乙酰基脱氧雪腐镰刀菌烯醇各有1件样品检出,黄曲霉毒素B_1有3件检出,检出率为8.33%,检出的5种真菌毒素含量在0.69～71.47μg/kg,均未超过国家食品安全标准规定的真菌毒素限量标准。结论大米中真菌毒素的检出率低,含量符合国家标准要求,该检测方法准确、可靠、便捷,可适用于大米中多种真菌毒素的检测。     

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.