鸡肉糜样中金刚烷胺检测能力验证研究

目的设计鸡肉糜样中金刚烷胺残留检测能力验证研究(proficiency testing,PT)项目,评价实验室对鸡肉中金刚烷胺残留量的检测能力。方法采用单因素方差分析和t检验对样品均匀性和稳定性进行分析。对能力验证结果进行稳健统计分析,通过Z比分数评价实验室检测能力。结果在P为0.05显著水平,制备100包样品均匀性符合要求且在整个能力验证计划周期内保持稳定,满足能力验证计划要求;17个省、市的42家实验室参加了本次能力验证,其中35家结果为满意,满意率为83.3%。结论参加能力验证的绝大多数实验室可以准确检测金刚烷胺,表明鸡肉中金刚烷胺残留量检测水平总体良好。     

肉鸡中金刚烷胺残留测定及其残留代谢规律研究

目的 建立液相色谱-串联质谱测定肉鸡中金刚烷胺残留量的分析方法, 探究鸡肉和鸡肝中的残留代谢规律。方法 样品用乙腈-乙酸-1%三氯乙酸(70:2:30, V:V:V)溶液提取, 固相萃取小柱净化后, 用液相色谱-串联质谱仪进行测定, 利用金刚烷胺-D6为内标定量。结果 金刚烷胺在0~10 μg/kg范围内线性良好, 相关系数(r2)为0.9995, 方法检测限为1 μg/kg。在添加质量浓度1~10 μg/kg范围内回收率为90.1%~95.7%, 相对标准偏差为1.17%~1.62%(n=6)。药物饲喂实验结果表明, 金刚烷胺在肉鸡中吸收快、分布广, 鸡肉中的残留明显高于鸡肝中残留含量, 鸡肉更容易产生药物蓄积。在停药13 d后, 鸡肉中金刚烷胺仍有药物蓄积, 而鸡肝中的金刚烷胺残留量为未检出。结论 该方法操作简单、灵敏度高、稳定性好, 适用于肉鸡中金刚烷胺残留的测定, 揭示金刚烷胺在肉鸡中残留代谢规律。     

鸡肉中金刚烷胺和利巴韦林残留基体标准物质的研制

目的建立含金刚烷胺和利巴韦林多残留鸡肉糜样自然基体标准样品的研制和定值方法。方法通过添加金刚烷胺和利巴韦林饲养白羽肉鸡获得阳性样本,然后经过取样、均质、包装、辐照灭菌、均匀性检验、稳定性检验、协同定值等过程,制备预期目标含量水平的含金刚烷胺和利巴韦林的多残留鸡肉糜样自然基体标准样品。结果经10家实验室采用液相色谱-串联质谱法进行协同定值,金刚烷胺和利巴韦林的特性值分别为10.1±1.0μg/kg(k=2),11.3±1.6μg/kg(k=2)。结论研究表明获得的样品均匀性良好,稳定性达到10个月,能够用于兽药残留检测的质量控制。     

我国畜禽内脏食用安全指标检测分析

目的了解我国食用畜禽内脏的重金属污染和药物残留情况。方法随机抽检全国29个省/市/自治区/兵团市场上销售的772份畜禽内脏样品,并采用国家标准检测方法对重金属污染物(铅、镉、总汞、总砷和铜)和违禁药物(克伦特罗、莱克多巴胺、沙丁胺醇、金刚烷胺和硝基呋喃类)残留情况进行检测分析,同时根据评价标准进行判定。结果 327份猪肝脏样品中,镉、铅、总汞、总砷、铜的超标率分别为2.14%、0.61%、3.98%、1.22%、6.12%,克伦特罗和沙丁胺醇的检出率分别为0.61%和0.31%;84份猪心脏样品中,镉、铅和总汞的超标率分别为3.57%、2.38%和5.95%;88份猪肾脏样品中总汞超标率为11.36%;43份猪肠、32份猪胃中镉超标率分别为2.33%和3.13%。71份鸡肫中镉、总汞和总砷的超标率分别为5.63%、7.04%、21.13%;69份鸡肝脏、31份鸡心脏中总汞超标率分别为11.59%、22.58%;鸭肫的重金属含量与药物残留情况均未发现不合格样品。结论我国畜禽内脏制品重金属污染比例相对较高,存在一定的食品安全风险。     

金刚烷胺残留化学发光酶免疫法的建立

建立金刚烷胺残留的化学发光酶免疫方法。对酶标抗原与磁标抗体的最佳稀释倍数、反应时间、底物发光时间进行优化,建立标准曲线,同时对方法的检测限、准确度和精密度进行评价。结果表明:50%抑制浓度(IC₅₀)为0.481 μg/L,线性范围是0.085~2.729 μg/L;在动物组织、兽药、饲料中的检测限为0.1 μg/kg,样本添加回收率为80.2%~94.5%,批内、批间相对标准偏差均<10%。该方法灵敏度高、操作简便,可广泛用于动物组织、兽药、饲料中金刚烷胺残留量的测定。     

间接竞争化学发光酶联免疫分析方法检测禽肉中金刚烷胺和氯霉素残留

为快速检测禽肉中残留的金刚烷胺和氯霉素,结合高效的前处理方法,建立检测金刚烷胺和氯霉素的间接竞争化学发光酶联免疫分析方法（indirect competitive chemiluminescence enzyme-linked immunosorbent assay,ic-CLEIA）。对包被原与抗体的最佳稀释倍数、竞争时间、酶标二抗稀释倍数进行优化。结果表明：金刚烷胺的IC50为0.33 μg/L,线性范围为0.06～1.77 μg/L;氯霉素的IC50为0.039 μg/L,线性范围为0.010～0.179 μg/L。样品经乙酸乙酯和碳酸钾溶液提取后,取上清液用氮气吹干,净化后进行检测。金刚烷胺和氯霉素的加标回收率分别为92.55%～105.14%和92.00%～112.50%,变异系数均低于10.48%,且实际样品检测结果与仪器方法相关性良好（R2＞0.98）,表明建立的ic-CLEIA方法具有良好的准确度和可靠性。该方法将为涉及多种药物残留的免疫快速检测方法及相应的前处理技术提供技术依据。     

嘉兴市畜禽肉中盐酸克伦特罗残留情况调查

为了解嘉兴市畜禽肉中盐酸克伦特罗的残留情况，嘉兴市卫生监督所和嘉兴市疾病预防控制中心于2001年2～10月进行了调查，选择3个城区，1个县区作为调查点，随机抽取32家畜禽养殖户，32家屠宰场，140家农贸市场肉禽店（摊），40家用肉单位（饭店，食堂，粽子厂等）进行调查和检测，调查结果显示，只有1户屠宰公司进行宰前盐酸克伦特罗残留检测，抽检畜禽组织309份，60份盐酸克伦特罗阳性，占19.42%，平均残留量为34.7μg/kg；检测生猪尿液36份，4份阳性，占11.11%，检测饲料及水23份，未检出。猪，鸡，牛组织中的残留检出情况分别为猪57份(21.35%），鸡2份（7.41%），牛1份（6.67%），就猪组织而言，肺，肝，肾的阳性率高于肉。调查结果表明酸盐克伦特罗残留情况严重，应加强监督管理。     

2016年云南省部分地区鸡蛋中兽药及禁用药物残留监测结果分析

目的 了解云南省部分地区鸡蛋中兽药及禁用药物残留水平, 为监督执法的提供技术支撑。方法 采集云南省昆明等部分地区超市、农贸市场销售的鸡蛋67份, 按照国家标准方法和《2016年国家食品污染和有害因素风险监测工作手册》对鸡蛋中氯霉素、五氯酚钠、金刚烷胺、利巴韦林、甲硝唑、喹诺酮类抗菌药11项、四环素类抗菌药4项残留检测, 检测结果依据2002年农业部235号公告《动物性食品中兽药最高残留限量》等进行评价。结果 氯霉素、金刚烷胺、五氯酚钠未检出, 利巴韦林检出率1.49(1/67), 甲硝唑检出率为32.84%(22/67), 四环素类检出率为37.31%(25/67), 喹诺酮类检出率为4.48%(3/67)。结论 云南省部分地区鸡蛋中甲硝唑残留情况较严重, 应该引起相关部门重视。     

同位素稀释-超高效液相色谱-串联质谱法测定禽类食品中利巴韦林和金刚烷胺类化合物残留量

目的建立同位素稀释-超高效液相色谱-串联质谱(UPLC-MS/MS)法检测禽类食品中利巴韦林和金刚烷胺类化合物(金刚烷胺、金刚烷甲胺、金刚烷乙胺、3,5-二甲基金刚胺)的残留量。方法样品经酶解,三氯乙酸沉淀蛋白,低温高速离心,上清液调节pH值后经PBA/PCX复合固相萃取柱净化,Agilent ZORBAX SB-Aq柱(3.0 mm×100 mm,1.8μm)分析利巴韦林,Waters BEH C_(18)色谱柱(2.1 mm×100 mm,1.7μm)分析金刚烷胺类化合物,串联质谱测定,同位素内标法定量。结果利巴韦林在1.0～100 ng/mL、金刚烷胺类化合物在0.2～20 ng/mL范围内呈良好的线性关系,相关系数(r)均为0.999。利巴韦林的检出限和定量限分别为0.5和1.5μg/kg;金刚烷胺类化合物的检出限和定量限分别为0.1和0.3μg/kg。利巴韦林(1.5～15μg/kg)和金刚烷胺类化合物(0.3～3.0μg/kg)添加3个浓度的检测结果显示,利巴韦林的回收率为91.4%～103.7%,金刚烷胺类化合物的回收率为94.3%～108.2%,相对标准偏差(RSD)均小于10%。结论本方法具有简便快捷、灵敏度高、定性准确等特点。     

2006-2007年福建省地产茶叶中有机氯农药残留调查

目的了解福建省地产茶叶中有机氯农药残留现状。方法2006-2007年在福建省主要产茶地随机抽取不同品种茶叶共72份,参照GB/T5009.19—2003《食品中六六六、滴滴涕残留量的测定方法》,采用毛细管气相色谱法进行检测。结果所测72份茶叶中,六六六残留量合格率为95.8%;滴滴涕残留量合格率为63.9%。六六六的主要残留成分为γ-HCH,滴滴涕的主要残留成分为p,p′-DDE。闽南地区的有机氯农药残留远高于闽北地区。结论福建省地产茶叶中有机氯农药残留状况不容乐观,应引起重视,加强监管。     

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.