固相萃取气相色谱-质谱联用法测定牛奶中的雌三醇

通过液液萃取和固相萃取提取、净化牛奶中添加的雌三醇，TMS衍生化试剂BSTFA衍生化。气相色谱-质谱联用（选择离子模式，选择离子为m／z311，m／z345，m／z414，m／zS04）对衍生物检测分析。确定了牛奶中雌三醇的定性、定量分析方法．该法栓出限为0．5μg／L，衍生物的峰面积与样品质量浓度在1—1000μg／L内呈良好的线性关系，线性回归系数为0．999。不同雌三醇加入量的加标回收率分别为78．2％-86．7％，变异系数为3．2％-3．6％。     

液相色谱-电喷雾质谱同时测定肉类中的莱克多巴胺与克伦特罗

建立了液相色谱-质谱法（LC/MS）同时测定肉类中莱克多巴胺与克伦特罗残留的方法。用乙腈-盐酸溶液提取试样中的莱克多巴胺与克伦特罗，旋转蒸干，用甲醇溶解后进行液相色谱-质谱法测定。肉类中莱克多巴胺与克伦特罗的定量检出限均分别为0．2μg／kg与0．5μg／kg。加标回收率分别为82.0％～87.5％与83．6％～89．2％。批内相对标准偏差均小于7．1％。该方法灵敏、定量准确，可广泛应用于肉类中莱克多巴胺与     

面粉中三聚氰胺的高效液相色谱——质谱法测定

建立了面粉中三聚氰胺的高效液相色谱-质谱测定方法。色谱条件：Kromasil C18柱（4．6mm×250mm，5μm），流动相：乙腈-0．1％（体积分数）甲酸（体积比5：95），流速0．4mL／min。采用正离子模式的电喷雾质谱检测，以一级质谱得到的准分子离子m／z127作为母离子，进行碰撞诱导解离二级质谱分析，选择母离子和MS的碎片离子m／z85、109定性确证，提取m／z85、109、127三个离子质量色谱峰面积定量。线性范围为0．01-0．5mg／L，检出限0．01mg／L，回收率为80％～99％。     

GC-MS法测定奶与奶制品中雌二酮残留量的研究

通过液液萃取和固相萃取提取、净化奶与奶制品中添加的雌酮,以TMS衍生化试剂BSTFA衍生化,气相色谱-质谱联用(选择离子模式,选择离子为m/z218、m/z244、m/z257、m/z342)对衍生物检测分析,确定了样品中雌酮的定性、定量分析方法,该法检出限为0.2μg/kg,定量限为0.8μg/kg。衍生物的峰面积与样品质量浓度在0.5～1000μg/L范围内呈良好的线性关系,线性回归系数为0.999。雌酮不同加入量的添加回收率为70.1%～93.6%,变异系数为2.0%～3.7%。该方法可实现对样品进行灵敏、准确的定性定量分析。     

高效液相色谱-电喷雾串联质谱测定尿液中硝西泮代谢物7-氨基硝西泮的研究

采用高效液相色谱．电喷雾串联质谱测定尿液中硝西泮的代谢物7-氨基硝西泮。测定时尿液中加入内标7-氨基氯硝西泮，经过β-葡萄糖醛酸酸苷酶水解，碱性液萃取，过0.45μm的滤膜，反相色谱分离后进行质谱分析，在选择反应监测模式（SRM）下进行特征母．子离子对信号采集。根据保留时间、母离子和特征子离子信息进行定性分析，内标法进行定量。药物检测限（LOD，S／N=3）为0.07μg／L，定量限（LOQ）为0．5μg／L，线性范围为1～50μg／L。在1．0、10．0、25．0、45．0μg／L四个添加水平下，回收率范围为89．0％～95．2％，相对标准偏差（RSD）小于6．4％。结果表明，该法简单、灵敏、重现性强，适用于尿液中7-氨基硝西泮的分析确证。     

LC-MS/MS法测定人血浆中曲司氯铵的浓度

目的建立测定人血浆中曲司氯铵浓度的LC—MS／MS方法。方法血浆样品经液-液提取后，以甲醇（含0．1％乙酸）：水（含0．1％乙酸＋2．5mmol／L酸铵）（80：20）为流动相，使用Agilent1100VL型离子阱质谱仪，电喷雾离子源正离子模式，采用多反应离子监测方式测定曲司氯铵（MRM，m／z392→164＋182）。结果血浆中曲司氯铵线性范围为0．1～10．0ng／mL，定量下限为0．1ng／mL，准确度85％～115％，日内、日间精密度（RSD）±15％。结论该方法准确，专属性强，可用于曲司氯铵药动学研究。     

碳酸饮料中微量铜的测定

研究在酸性条件下用吡咯烷二硫代甲酸铵和二乙氨基二硫代甲酸钠及甲基异丁酮（APDC＋DDTC—MIBK）体系萃取富集碳酸饮料消化液中铜离子，再用石墨炉原子吸收法测定铜离子含量的检测方法。并对实验条件进行优化，确定最佳消化体系：HNO3-HClO4（5＋2），方法检出限为0．2653μg／L，特征灵敏度为0．2122μg／L。线性范围为1．5μg/L～10μg/L，相关系数为0．9993，加标回收率为95，79％-100．74％，相对标准偏差为3．13％～5．06％。     

HS-SPME-GC-MS法测定纺织品游离甲醛

建立了纺织品游离甲醛的衍生．萃取．气质联用测定方法：试样剪碎后置于饱和NaCl溶液中，60℃超声波超声处理30min，用五氟苯盐酸氢胺衍生化后，采用顶空固相微萃取和色质联用技术（HS-SPME-GC-MS），选择离子（m/z181）进行定量。该方法适用于各类单层或多层纤维织物中甲醛的测定，加标回收率94．9％-98．7％，相对标准偏差2．97％-4．59％；方法检出限为0．02mg／kg。     

气相色谱-质谱法测定动物性食品中三种β-激动剂的残留量

建立了用气相色谱-质谱同时测定动物性食品中克伦特罗、沙丁胺醇和莱克多巴胺残留量的检测方法。样品用乙酸胺缓冲液匀浆,加入β-葡萄糖苷酸酶水解,用异丙醇-乙酸乙酯(40:60)萃取,有机相浓缩,经LC-SCX固相萃取柱进行分离,用4%氨化甲醇洗脱,洗脱液氮气吹干后,经N、O-双三甲基硅烷三氟乙酰胺(BSTFA)衍生后于气质联用仪上进行测定。检测采用选择性离子监控模式(SIM),以特征离子克伦特罗(86,262,243)、沙丁胺醇(86,369,440)和莱克多巴胺(250,267,502)定性,以试样峰(m/z86,m/z369,m/z250)的峰面积外标法定量。本方法检出限为克伦特罗和沙丁胺醇0.5ug/kg,莱克多巴胺2ug/kg;3种组分的线性相关系数均大于0.99。该方法的回收率为75%-98%,相对标准偏差为5%-14%。     

高效液相色谱-串联质谱法测定家禽组织中硝基呋喃类抗生素代谢物残留的研究

本文建立了用高效液相色谱-串联质谱（LC-MS-MS）测定禽肉组织中3-氨基-2-唑烷基酮（AOZ）、5-甲基吗啉-3-氨基-2-唑烷基酮（AMOZ）、氨基脲（SEM）和1-氨基-2-内酰脲（AHD）4种硝基呋喃类抗生素代谢物的方法。0．2mol／L盐酸水解禽肉组织中与蛋白结合的硝基呋喃代谢物，用2-硝基苯甲醛（2-NBA）37℃衍生16h。上清液调pH=7．4后，用LiChrolut EN固相萃取柱净化，乙酸乙酯洗脱，流动相定容。采用电喷雾电离，正离了扫描，多反应监测（MRM）模式检测，标准曲线用空白禽肉样品添加标准与样品同步操作获得并用其进行外标定量。在添加浓度0．5～10μg／kg范围内，四种代澍物的平均回收率在70．2％～89．1％，检出限AMOZ、AOZ为0．1μg／kg，SEM、AHD为0．2μg／kg。10次测定结果相对标准偏差在5．59％～10．10％之间。     

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.