Qu ECh ERS EMR-Lipid结合LC-MS/MS测定鸡蛋中磺胺类和喹诺酮类药物残留

采用Qu ECh ERS EMR-Lipid技术处理样品,建立快速检测鸡蛋中14种磺胺类药物和16种喹诺酮类药物残留的液质联用检测方法。将鸡蛋样品用2%甲酸乙腈8 mL提取,再加入0.5 mL pH 7.0、0.1 mol/L的EDTA缓冲液震荡,用Qu ECh ERS EMR-Lipid快速样品提取技术净化,最后用0.2%甲酸溶液(A相)和乙腈溶液(B相)作为流动相进行梯度洗脱,采用电喷雾离子源的动态多反应监测模式(dynamic MRM)对30种磺胺类药物和喹诺酮类药物进行定性和定量分析。结果显示,30种抗生素添加水平在8~32μg/kg的回收率为50.09%~102.11%,相对标准偏差小于15.66%,方法检出限为0.00131~0.09717μg/kg。建立的鸡蛋中磺胺类药物和喹诺酮类药物残留检测的检测方法前处理简单易行,便于操作,方法精密度高,可以满足对鸡蛋中磺胺类药物和喹诺酮类药物快速、准确的检测要求,并适合大批量样品的准确定性和定量分析检测。     

UPLC-MS/MS法同时检测水产品中喹诺酮类药物残留

利用UPLC-MS/MS技术建立一种同时检测水产品中喹诺酮类药物残留的分析方法.对样品进行前处理及分离条件的优化,样品经柠檬酸磷酸盐缓冲液(Mcllvaine)超声提取,采用固相萃取(SPE)方法净化提取液,并对目标物质进行富集,用UPLC-MS/MS法检测.结果表明:依诺沙星、奥索利酸、培氟沙星、帕珠沙星、氟罗沙星含量在3～300 μg/kg 范围,萘啶酸、氟甲喹含量在0.5～50 μg/kg 范围,其余13种喹诺酮类化合物含量在1～100μg/kg范围均具有良好的线性关系,相关系数0.9981～0.9999,定量限(LOQ)0.34～8.13 μg/kg.药物含量在5～150μg/kg范围,除氟甲喹、萘啶酸外,其它喹诺酮的回收率均在63.6%～92.8%之间,相对标准偏差1.51%～11.32%.该方法可满足水产品中喹诺酮类药物多残留检测的要求.     

QuEChERS HPLC-MS/MS法测定禽肉中9种喹诺酮类兽药残留量

建立Qu ECh ERS-液相色谱串联质谱法同时检测禽肉中的丹诺沙星、恩诺沙星、沙拉沙星、环丙沙星、氧氟沙星、诺氟沙星、依诺沙星、培氧沙星、双氟沙星9种喹诺酮类兽药残留量方法。样品以乙腈、EDTA-Mcllvaine和乙酸为提取试剂,无水硫酸钠为脱水剂,C18为吸附剂进行净化,以甲醇-0.1%甲酸水为流动相,反相C18色谱柱分离,正离子多反应监测模式进行质谱分析。9种喹诺酮在1.0μg/kg~200μg/kg范围内具有良好的线性关系,相关系数(r2)均在0.993以上。检出限范围为0.07μg/kg~0.20μg/kg,定量限范围在0.23μg/kg~0.67μg/kg之间。平均回收率介于70.8%~93.0%之间,相对标准偏(RSD)低于8.9%。该方法适合于检测禽肉中的喹诺酮类药物残留量的测定。     

超高效液相色谱-串联质谱测定猪肉中16种喹诺酮药物残留量

建立同时测定猪肉中萘啶酸、恶喹酸、依诺沙星、氟甲喹、诺氟沙星、环丙沙星、洛美沙星、丹诺沙星、恩诺沙星、氧氟沙星、沙拉沙星、二氟沙星、麻保沙星、培氟沙星、司帕沙星、奥比沙星16种喹诺酮类药物残留的超高效液相-串联质谱(ultra performance liquid chromatography-tandem mass spectrophy,UPLC-MS/MS)的检测方法。样品采用乙酸-乙腈(1∶99,V/V)一次性振荡提取,用弱阴离子固相萃取柱净化,内标法定量。结果表明:16种喹诺酮药物的检出限为0.2μg/kg,定量限为0.8μg/kg,空白猪肉中添加2.0、5.0、10.0μg/kg水平,16种喹诺酮的回收率在70%~120%。该方法分析速度快、样品前处理干净、杂质污染少,可用于猪肉样品中喹诺酮类的残留检测。     

羊奶及奶粉中27种β-受体激动剂类药物残留UPLC-MS/MS检测方法

采用超高效液相色谱串联质谱建立羊奶及奶粉中吡布特罗、丙卡特罗、瑞普特罗、克伦普罗、奥达特罗等27种β-受体激动剂类药物残留检测方法。样品经过1%甲酸乙腈提取、Oasis PRi ME HLB柱净化后,经Acquity UPLC BEH C18(100 mm×2.1 mm,1.7μm)分离,以甲醇和0.1%甲酸水溶液为流动相进行梯度洗脱,多通道MRM信号采集模式,27种β-受体激动剂类药物能在10.5 min内出峰完好,在1.0~100.0μg/L浓度范围内,27种β-受体激动剂类药物线性良好,相关系数均在0.993以上;羊奶中最低定量限均低于0.5μg/kg,通过0.5、2.5、5.0μg/kg三个浓度的加标回收实验表明,回收率为65.7%~119%,批内变异系数为0.79%~10.4%,批间变异系数为2.13%~15.7%。奶粉中最低定量限均低于2.0μg/kg,通过2.0、10.0、20.0μg/kg三个浓度的加标回收实验表明,回收率为60.5%~109%,批内变异系数为1.91%~12.4%,批间变异系数为3.06%~17.2%。所建立方法为一种高通量检测羊奶及奶粉中β-受体激动剂类药物残留确证分析方法。     

同位素内标-超高效液相色谱串联质谱法测定禽类食品中喹诺酮与四环素残留量

摘 要：目的 建立测定禽类食品中11种喹诺酮与4种四环素兽药残留的超高效液相色谱-串联质谱(ultra performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)分析方法。方法 鸡肉和鸡蛋样品经Mcllvaine-Na2EDTA缓冲液提取,7%钨酸钠溶液沉淀蛋白,HLB柱净化后,喹诺酮类药物采用10 mmol/L乙酸铵(含0.1%甲酸,v/v)与甲醇为流动相,四环素类药物采用0.1%甲酸与乙腈为流动相。两种类型药物均采用电喷雾电离,正离子扫描,多离子反应监测模式,基质匹配同位素内标,标准曲线法定量。结果 15种兽药残留在0.1~50.0 μg/L的浓度范围内线性良好,相关系数r2均大于0.9927,检出限范围为0.05~0.20 μg/kg,平均回收率为60.6％~117.9％,相对标准偏差范围为0.51%~15.3%。采用建立的方法检测安徽省市售2016~2018年的鸡肉和鸡蛋样品中喹诺酮与四环素残留,检测结果通过食品安全指数(international foundation for science ,IFS)评估,发现鸡肉和鸡蛋中喹诺酮类IFS均值分别为0.00048 μg/kg?bw?d与0.000097 μg/kg?bw?d,四环素类IFS均值分别为0.00073 μg/kg?bw?d与0.00098μg/kg?bw?d,均小于1,说明其膳食暴露风险较低。结论 该方法的样品前处理沉淀蛋白完全,净化效果好,减少了基质效应的影响,适用于大批量禽类食品中喹诺酮与四环素兽药残留量的快速测定。     

UHPLC-MS/MS同位素内标法测定豆制品中16种喹诺酮类药物残留

建立了同时测定豆制品中16种喹诺酮类药物(依诺沙星、氟罗沙星、诺氟沙星、氧氟沙星、培氟沙星、环丙沙星、洛美沙星、达氟沙星、恩诺沙星、奥比沙星、沙拉沙星、双氟沙星、司帕沙星、恶喹酸、萘啶酸、氟甲喹)残留的同位素内标结合超高效液相色谱-串联质谱法检测方法。样品用0.1mol/L EDTAMcllvaine缓冲溶液提取,经HLB固相小柱净化,氮吹定容后,采用超高压反相C18色谱柱分离,质谱分析采用电喷雾电离,正离子扫描,多反应监测模式,内标法定量。在优化条件下,16种喹诺酮类药物在0.50～50.00ng/mL的质量浓度范围内线性良好,相关系数R2均在0.99以上,检出限(LOD)为0.5μg/kg,在检出限的1倍、2倍和10倍添加浓度下,16种喹诺酮类药物平均回收率在80.7%～107.1%之间,相对标准偏差(RSD,n=6)在1.5%～10.6%之间。该方法前处理简便快速,选择性好,灵敏度、回收率和精密度高,适用于豆制品中喹诺酮类药物残留的定性定量检测。     

液相色谱-串联质谱法检测蜂蜜中15种喹诺酮类和17种磺胺类药物残留

目的建立同时测定蜂蜜中15种喹诺酮和17种磺胺类药物残留的液相色谱-串联质谱(liquid chromatography-tandem mass spectrometry,HPLC-MS/MS)检测方法。方法样品经过磷酸盐缓冲溶液(pH=8)提取,过HLB(hydrophile-lipophile balance)固相萃取柱净化。以CORTECS C18色谱柱(2.1 mm×100 mm,1.6μm)分离,以5 mmol乙酸铵、0.1%甲酸水(A)和0.1%甲酸-乙腈(B)作为流动相进行梯度洗脱。质谱分析以电喷雾为离子源(electrospray ionization,ESI+),采用多反应监测(multiple reaction monitoring,MRM)。结果本方法在15 min内完成32种目标化合物的分离。15种喹诺酮和17种磺胺类药物在1.0、5.0和10.0μg/kg添加水平的回收率为54.9%~122.5%,相对标准偏差(relative standard deviation,RSD)小于18.7%(n=6),方法检出限为0.4μg/kg,定量限为1.0μg/kg。结论该方法快速、准确、灵敏,适合测定蜂蜜中喹诺酮和磺胺类药物残留。     

QuEChERS-超高效液相色谱-串联质谱法同时测定畜禽肉中11 种喹诺酮类兽药残留

建立一种超高效液相色谱-串联质谱法测定畜禽肉中恩诺沙星、环丙沙星、氧氟沙星、培氟沙星、诺氟沙星、洛美沙星、沙拉沙星、双氟沙星、司帕沙星、氟罗沙星和达氟沙星共11 种喹诺酮类兽药残留的检测方法。畜禽肉样品经2%甲酸-乙腈均质提取,离心沉淀后上清液经QuEChERS净化剂净化后,经快速溶剂蒸发系统浓缩,采用Waters BEH C18色谱柱（2.1 mm×50 mm,1.7 μm）分离,以0.1%甲酸-水和0.1%甲酸-乙腈为流动相进行梯度洗脱,电喷雾离子源电离,多反应监测模式采集信号,内标法定量。结果表明：11 种喹诺酮类兽药在2～80 ng/mL质量浓度范围内线性关系良好（R2＞0.99）,方法的检出限和定量限分别为0.5～2.0 μg/kg和1.5～6.0 μg/kg;空白样品加标量为10、25、50 μg/kg 3 个水平时,11 种喹诺酮类兽药的平均加标回收率为74.52%～106.83%,相对标准偏差为1.8%～8.7%（n=6）。该方法检测过程简单快捷、准确度好、灵敏度高,适用于畜禽肉中喹诺酮类兽药残留的检测。     

液相色谱-串联质谱法测定猪肉中13种磺胺类药物残留

利用液相色谱-电喷雾串联质谱建立猪肉中13种磺胺类药物残留的同时、快速分析方法.猪肉样品中的残留药物用1%乙酸-乙腈均质提取,浓缩后用0.1%甲酸-乙腈定容,并用正己烷液-液分配除脂后,用Kinetex C18色谱柱(100mm×2.1mm,2.6μm)分离,以0.1%甲酸-乙腈作为流动相梯度洗脱,采用电喷雾正离子电离,多反应监测模式检测,基质匹配外标法定量.13种磺胺类药物在1~300μg/kg范围内线性关系良好,定量限均小于10μg/kg.在1、2μg/kg和10μg/kg这3个添加水平下,回收率在60.0%~78.1%之间,相对标准偏差(RSD)在0.24%~8.88%之间.此方法操作简便,灵敏度、准确度、精密度均满足残留分析的要求.     

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）＂     

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