肉品中β-受体激动剂类药物残留检测 技术研究进展

肉品中β-受体激动剂类药物残留问题严重影响着人体健康。近几年来暴露出来的肉品中β-受体激动剂类药物残留事件层出不穷, 为了加强监控, 越来越多的检测方法被建立起来, 极大地提高了肉品中β-受体激动剂类药物残留检测的效率。本文综述了检测肉品中β-受体激动剂类药物残留的色谱法、酶联免疫法、胶体金法和其他一些新方法的研究进展, 以及我国现行的β-受体激动剂类药物残留标准检测方法。对现有的检测方法的优缺点和发展阶段作了归纳总结, 并对β-受体激动剂类药物残留检测方法发展的方向提出了一些展望。未来的发展主要是一些特异性和灵敏度更高的快检方法和样品前处理更加简化的液质色谱联用法。     

食源性动物组织中β-受体激动剂研究进展

β-受体激动剂是一类苯乙醇胺类药物,化学结构和生理功能类似于肾上腺素和去甲肾上腺素,常用于防治人和动物支气管哮喘等疾病。由于β-受体激动剂类药物可促进动物体内蛋白质合成并抑制脂肪沉淀,使动物体内营养成分再分配,所以此类药物常被添加到动物饲养过程中用于提高瘦肉率,继而造成药物在动物体内残留,人类食用后会引发急性中毒而威胁健康。虽然大多数国家已经明令禁止在动物饲养中使用此类药物,但是仍然存在非法使用的情况。为了加强动物源性食品安全,各国已经展开了对β-受体激动剂类药物的研究,已建立多种快速准确的检测方法。本研究主要对β-受体激动剂的结构和性质、在动物源性食品中代谢消除规律和β-受体激动剂检测技术3个方面进行阐述,并对β-受体激动剂药物残留检测的未来研究方向进行展望。     

动物源性食品中β-受体激动剂分类及检测方法研究进展

动物源性食品中的β-受体激动剂兽药残留检出对人体健康存在潜在威胁,对β-受体激动剂残留进行有效监控,建立可靠、灵敏和实用的检测方法至关重要。本文对近10年来β-受体激动剂的常用检测方法进行综述,重点阐述其在色谱-质谱联用技术研究进展,并对未来检测技术的发展方向提出了展望。     

液相色谱-串联质谱法检测猪尿中26种β_2-受体激动剂类药物残留

目的建立了一种在猪尿中检测26种β_2-受体激动剂兽药残留的液相色谱-串联质谱(HPLC-MS/MS)检测方法。方法样品经β-葡萄糖苷酸酶/芳基硫酸酯酶酶解后,用正丁醇及甲基叔丁基醚混合液萃取,过混合阳离子(MCX)固相萃取柱净化。采用0.1%甲酸溶液(A)和0.1%甲酸.乙腈(B)作为流动相进行梯度洗脱,质谱(ESI+)采用多离子检测模式(MRM)对β_2-受体激动剂的定量离子和定性离子进行监测。结果本方法在15 min内完成26种目标化合物的分析,实现高通量检测,可有效地提高β_2-受体激动剂检测效率。26种β_2-受体激动剂在5、10和20μg/kg添加水平的回收率为65.0%~105.3%,相对标准偏差小于11.5%(n=6),方法检出限为0.04~1.02μg/kg。结论该方法快速、准确、灵敏,适合测定猪尿中的β_2-受体激动剂类药物残留。     

液相色谱-串联质谱法检测饲料中26种β2-受体激动剂类药物残留

目的建立一种饲料中26种β2-受体激动剂兽药残留的液相色谱-串联质谱(HPLC-MS/MS)检测方法。方法样品经盐酸甲醇提取液提取,醋酸铅沉淀蛋白后,过混合阳离子(MCX)固相萃取柱净化。采用0.1%甲酸(A)和0.1%甲酸-乙腈(B)作为流动相进行梯度洗脱,质谱(ESI+)采用多离子检测模式(MRM)对β2-受体激动剂的定量离子和定性离子进行监测。结果本方法在15 min内完成26种目标化合物的分离分析。26种β2-受体激动剂在20、50和100μg/L添加水平的回收率为71.9%~102.9%,相对标准偏差小于11.8%(n=6),方法定量限为10μg/kg。结论该方法快速、准确、灵敏,适合测定饲料中的β2-受体激动剂类药物残留。     

液相色谱-串联质谱法检测猪尿中26种β2-受体 激动剂类药物残留

目的 建立了一种猪尿中26种β2-受体激动剂兽药残留的液相色谱-串联质谱（HPLC-MS/MS）检测方法。方法 样品经β-葡萄糖苷酸酶/芳基硫酸酯酶酶解后,用正丁醇及甲基叔丁基醚混合液萃取,过MCX固相萃取柱净化。采用0.1%甲酸(A) 和0.1%甲酸-乙腈(B)作为流动相进行梯度洗脱,质谱(ESI )采用多离子检测模式(MRM)对β2-受体激动剂的定量离子和定性离子进行监测。结果本方法在15 min内完成26种目标化合物的分离分析。26种β2-受体激动剂在5、10和20μg/L添加水平的回收率为65.0%~105.3%,相对标准偏差小于11.5%（n=6）,方法检出限为0.04 μg/ kg ~1.02 μg/kg。结论 该方法快速、准确、灵敏,适合测定猪尿中的β2-受体激动剂类药物残留。     

利用Thermo Scientific全新高分辨台式、四极杆静电场轨道阱Q-Exactive分析19种β-受体激动剂

β-受体激动剂,又称为β-兴奋剂,大家近期所熟知的瘦肉精—克伦特罗,莱克多巴胺等就是这一类兴奋剂。其是一类含氮激素中的苯乙胺类药物,苯乙胺类药物具有苯乙醇胺结构母核,苯环上连接有碱性的β-羟胺侧链。由于发现在饲料中添加β-受体激动剂可以促进营养再分配作用,提高瘦肉率,减少饲料使用,使肉品提早上市,降低成本。因此,β-受体激动剂被人     

高效液相色谱串联飞行时间质谱法 快速检测饲料中多种β-受体激动剂

建立了一种快速筛查饲料样品中11种β-受体激动剂的高效液相色谱-飞行时间质谱的检测方法。样品经过酸性乙腈提取后直接进样分析。结果表明:11种β-受体激动剂得到良好的色谱分离和定性,方法的检测限和定量限分别为2μg/kg和5μg/kg,该方法在β-受体激动剂类药物的靶向和非靶向筛查检测中都有很好的应用前景。     

酶联免疫法检测乳与乳制品中的β-激动剂

β-受体激动剂类药物在动物饲养过程中具有促进动物生长和动物营养再分配的功效,但其易在动物体内及可食性组织中残留,影响动物源性食品安全并危害人体健康.β-受体激动剂类药物在我国和欧盟等国家和地区已被禁止用作动物促生长剂β-激动剂,本方法使用β-激动剂EIA微孔板含12个板条,每个板条8孔.用羊抗兔抗体IgG包被.特异性抗体(兔抗沙丁胺醇和兔抗克伦特罗)、辣根过氧化物酶标记的沙丁胺醇(酶结合物)和沙丁胺醇标准品或样品被加入到微孔后,经过1h孵育,特异性抗体被牢固地结合在板条上的羊抗兔抗体IgG上,与此同时,游离的β-激动剂(存在于标准溶液或样品中)和酶结合物相互竞争与特异性抗体的结合位点结合(即竞争性酶联免疫检测).然后在洗涤过程中除去未结合的酶结合物试剂,加入色原底物(四甲基联苯胺TMB),结合的酶结合物将无色的底物转化为蓝色的产物.滴加终止液(硫酸)终止显色反应,颜色由蓝色变为黄色,在450nm波长下检测吸光度,吸光度值与样品中β-激动剂浓度成反比.本方法为半定量检测,乳及乳制品中β-激动剂灵敏度是0.06ng/mL(ppb),本方法为快速检测方法,检测结果超出标准,必要时,需用国家标准中规定的仲裁方法进行验证.     

分子对接技术研究热休克蛋白27与β受体激动剂的相互作用

利用分子对接技术,研究热休克蛋白27(heat shock protein 27,HSP27)与β受体激动剂类药物的结合能力,探究HSP27用于检测β受体激动剂的可能性。将人工表达的HSP27和β₂肾上腺素受体(β₂ adrenergic receptor,β₂AR)分别与β受体激动剂类药物进行分子对接,比较它们的结合能力的差异性,并对对接结果进行酶联免疫吸附实验(enzyme-linked immunosorbent assay,ELISA)验证。对接结果显示,15种β受体激动剂类药物中有9种药物与HSP27对接的总评分值高于β₂AR。ELISA的结果显示,HSP27可以与HRP-克伦特罗、HRP-非诺特罗和HRP-莱克多巴胺特异性结合,OD值分别为0.685、0525、0.662,这与分子对接结果基本一致。结论:HSP27与β肾上腺素受体激动剂类药物具有较强的结合能力,可以用于检测 β肾上腺素受体激动剂的可能性较大。     

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