液相色谱-串联质谱法检测火锅底料中罂粟壳

研究建立火锅底料中非法添加罂粟壳的液相色谱-串联质谱测定法。采用水提取,乙腈和无水醋酸钠萃取罂粟壳中的生物碱分,液质联用进行检测,采用色谱柱SHISEIDO CAPCELL PAK CR1∶4(5μm,2.0×150 mm)色谱分离,流动相为乙酸铵:乙腈(50∶50),0.5%甲酸为A相,乙腈为流动相B相。该方法的检出限为1 ng/mL,方法定量下限吗啡为37μg/kg,可待因、罂粟碱、蒂巴因和那可丁为1μg/kg,线性范围为1 ng/m～40 ng/mL,加标回收率64.2%～101.1%。该方法测定火锅底料罂粟碱中吗啡、可待因、罂粟碱、那可丁、蒂巴因5种生物碱的含量快速、准确,适合于火锅调味料食品中罂粟壳的检测。     

超高效液相色谱-串联质谱法测定调味料中吗啡、可待因、蒂巴因、那可丁和罂粟碱残留量

目的：建立超高效液相色谱-串联质谱法测定调味料中吗啡、可待因、蒂巴因、那可丁和罂粟碱残留量的分析方法。方法：样品用水分散、乙腈超声提取，经盐析、低温高速离心分层后，样液于40℃水浴氮吹近干，用10%乙腈溶液(含0.1%甲酸)溶解残渣，再经低温高速离心、过膜上机测定；以Kinetex^? 2.6μm Biphenyl 100?色谱柱(100 mm×3.0 mm)分离，0.1%甲酸-水和0.1%甲酸-甲醇为流动相进行梯度洗脱，电喷雾电离(ESI),正离子模式，多反应监测(MRM)下检测，吗啡、可待因用内标法定量，蒂巴因、那可丁、罂粟碱用外标法定量。结果：吗啡、可待因在0.5～20.0 ng/mL,蒂巴因在0.10～4.0 ng/mL,那可丁、罂粟碱在0.05～2.0 ng/mL范围内均有良好的线性关系，相关系数r均大于0.998。吗啡、可待因的方法检出限为1.0μg/kg,蒂巴因的方法检出限为0.2μg/kg,那可丁、罂粟碱的方法检出限为0.1μg/kg。5种生物碱的加标回收率在75.2%～117.3%之间，相对标准偏差均小于15%。结论：该方法操作简单，具有较高的灵敏...     

亲水作用液相色谱-串联质谱法快速测定食品中罂粟壳的生物碱残留

目的建立亲水作用液相色谱-串联质谱法快速测定食品中的罂粟壳残留生物碱的分析方法。方法样品中的罂粟壳成分采用优化后的Qu ECh ERS方法进行提取,BEH HILIC色谱柱分离(2.1 mm×100 mm,1.7μm),最后采用串联质谱仪对吗啡、可待因、罂粟碱、那可丁及蒂巴因进行检测。结果吗啡、可待因在2.0~100ng/mL范围内线性关系良好,罂粟碱、那可丁、蒂巴因在0.10~5.0 ng/mL范围内线性关系良好。平均加标回收率(n=6)在70%~120%之间,相对标准偏差小于12%。吗啡、可待因、粟碱、那可丁、蒂巴因的检出限分别为10、10、3.8、3.8、7.5μg/kg。结论该方法简便、快速、灵敏,可用于食品中残留罂粟壳成分的检测。     

超高效液相色谱-串联质谱法快速测定调味料中5 种罂粟壳生物碱残留量

建立超高效液相色谱-串联质谱法（UPLC-MS/MS）测定调味料中吗啡、可待因、蒂巴因、罂粟碱、那可丁5种生物碱含量的分析方法。0.2%甲酸的乙腈提取样品,采用QuEChERS方法处理及净化,经乙酸乙酯-环己烷（2∶8,V/V）脱脂,Waters UPLC HSS T3色谱柱（1.7 μm,2.1 mm×100 mm）分离,以含0.1%甲酸10 mmol/L甲酸铵溶液-乙腈为流动相梯度洗脱,电喷雾电离正离子（ESI+）、多反应监测（MRM）模式分析测定,外标法定量。结果表明,5种生物碱5 min内出峰完全,且分离度及各峰型良好。精密度试验结果相对标准偏差（RSD）为0.43%～1.85%,平均回收率为65.7%～108.2%,RSD为1.24%～8.71%。吗啡、可待因的检出限（LOD）和定量限（LOQ）分别为3.0 μg/kg、10.0 μg/kg;蒂巴因、罂粟碱和那可丁的LOD和LOQ分别为0.6 μg/kg、2.0 μg/kg。该方法简单、快捷、准确,可用于调味料等食品中罂粟壳生物碱的定性与定量分析。     

高效液相色谱-串联质谱法测定药酒中5种罂粟壳生物碱

目的 建立高效液相色谱-串联质谱法测定药酒中非法添加吗啡、可待因、蒂巴因、罂粟碱和那可丁５种罂粟壳生物碱的分析方法。方法 药酒在60 ℃水浴锅上挥去乙醇, 再加入含0.2%(V/V)甲酸的乙腈溶液提取, 最后用分散固相萃取(dispersive solid phase extraction, d-SPE)纯化管净化待测。以乙腈和10 mmol/L乙酸铵溶液（含0.1%甲酸）作为流动相进行梯度洗脱, 选用色谱柱为Xtimate TM C18柱, 在0.4 mL/min流速下, 质谱采用电喷雾电离源正离子扫描, 多反应监测模式检测。结果 吗啡和可待因线性范围为5.0~250.0 ng/mL, 蒂巴因、罂粟碱、那可丁的线性范围为1.0~50.0 ng/mL, 相关系数均在0.997以上。5种生物碱的方法检出限和定量限分别为0.02～0.80 μg/L 和 0.07～3.00 μg/L, 回收率范围为80.3%～101.5%, 相对标准偏差(relative standard deviation, RSD)在3.2%～8.1%之间(n=6)。结论 该方法简便、快速、准确可靠, 可用于药酒中罂粟壳生物碱含量的检测。     

QuEChERS-UPLC-MS/MS-内标法测定肉制餐饮食品中5种罂粟壳生物碱

建立改进的QuEChERS（quick, easy, cheap, effective, rugged, safe）方法,以内标法结合超高效液相色谱-串联质谱法（ultra high performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS）测定肉制餐饮食品中吗啡、可待因、那可丁、罂粟碱、蒂巴因5 种罂粟壳生物碱。样品经乙腈-体积分数0.1%氨水提取,净化包（2 g无水硫酸镁、50 mg N-丙基乙二胺,100 mg C18E）净化,选择含10 mmol/L甲酸铵的体积分数0.1%甲酸-水溶液和体积分数0.1%甲酸-乙腈溶液作为流动相,采用等度洗脱,使净化液中5 种罂粟壳生物碱经HILIC Core-shell色谱柱（50.0 mm×2.1 mm,1.7 μm）分离,在多反应监测模式下利用电喷雾电离源正离子模式扫描获得质谱数据,内标法定量。结果表明：5 种罂粟壳生物碱可在8 min内有效分离,且罂粟碱、那可丁、蒂巴因在0.2～20.0 ng/mL质量浓度范围内线性良好,吗啡、可待因在1.0～100.0 ng/mL范围内线性良好,r均大于0.999,方法检出限为0.3～2.5 ng/mL,定量限为1.0～7.5 ng/mL,5 种罂粟壳生物碱的平均回收率为85.8%～107.4%,相对标准偏差为0.5%～4.7%。该方法操作简单、净化效果好、检测效率高,适用于餐饮肉制食品中5 种罂粟壳生物碱的快速检测。     

超高效液相色谱-串联质谱法检测汤料食品中罂粟壳成分

目的建立超高效液相色谱-串联质谱法(ultra performance liquid chromatography tandem mass spectrometry, UPLC-MS/MS)定性定量检测市售麻辣烫、火锅底料及牛肉汤等汤料食品中罂粟碱、吗啡、可待因、那可丁和蒂巴因的分析方法。方法样品经0.1 mol/L HCl提取、混合阳离子(mixed-cation, MCX)固相萃取柱净化。选用Waters BEH HILIC(2.1 mm×100 mm, 1.7μm)色谱柱进行分离,以0.1%(V/V)甲酸-乙腈和0.1%甲酸-10mmol/L甲酸铵溶液为流动相,进行梯度洗脱。采用正离子源模式(positive electrospray ionization, ESI+)和多反应检测(multi reaction monitor, MRM)模式进行检测,内标法定量。结果在0.1～20μg/L(吗啡和可待因)以及0.1～4.0μg/L(蒂巴因、那可丁和罂粟碱)的浓度范围内, 5种罂粟壳物质线性良好,相关系数均大于0.995,检出限为0.1～0.5μg/L,方法回收率的范围在77.9%～95.5%之间,相对标准偏差1.75%～9.49%(n=6)。结论方法简单易行可操作,且精密度及准确度均较高,适用于汤料食品中罂粟壳的检测。     

液相色谱-质谱联用法(HPLC-MS/MS)快速测定凉茶中的5种罂粟壳类生物碱

目的:建立液相色谱-质谱联用法(HPLC-MS/MS)快速检测凉茶中非法添加的吗啡、可待因、蒂巴因、罂粟碱、那可丁等5种罂粟壳类生物碱。方法:采用Agilent Poroshell 120 EC-C₁₈（2.1 mm×100 mm,2.7 μm）色谱柱分离,含0.1%乙酸的5 mmol/L乙酸铵溶液-甲醇为流动相梯度洗脱,在电喷雾离子源正离子模式下,采用多反应监测(MRM)方式测定,外标法定量。结果:吗啡、可待因的线性范围为2.5～100 ng/mL,蒂巴因、罂粟碱、那可丁的线性范围为0.5～20 ng/mL,5种罂粟壳类生物碱的线性相关系数均大于0.995（R>0.995）。检出限吗啡、可待因为0.8 μg/g,罂粟碱、蒂巴因、那可丁为0.2 μg/g。5种生物碱成分的3个添加水平在液体基质中回收率为84.5%～105.1%,RSD不大于6.3%（n=6）,固体基质中回收率为72.5%～112.3%,RSD不大于7.1%（n=6）。应用方法对150批凉茶样品进行了抽检,其中6批检出。结论:该方法操作简便,准确可靠,适用于快速分析测定凉茶中的5种罂粟壳类成分。     

UPLC-ESI-MS/MS同时测定火锅底料中的罂粟壳生物碱

建立了超高效液相色谱-电喷雾串联质谱(UPLC-ESI-MS/MS)测定火锅底料中那可丁、罂粟碱、蒂巴因、可待因和吗啡残留量的快速、准确的检测方法。该法通过加入0.1 mol/L盐酸溶液,再用NaOH溶液调pH至中性,乙腈溶液提取,最后用新型材料EMR Lipid净化管净化。试验以添加不同质量浓度标准溶液的方式绘制校准曲线,并以可待因-D_3和吗啡-D_3为内标进行检测,从而大大提高了定量的准确性。结果表明,那可丁、罂粟碱和蒂巴因的线性范围为1.0~20.0 ng/mL,可待因和吗啡的线性范围为5.0~100.0 ng/mL,相关系数均在0.999以上。5种生物碱的方法检出限为0.05~2μg/kg,方法定量限为0.2~7.0μg/kg。在加标量为0.5,2.0和5.0μg/kg水平下,5种待测物平均回收率为82.0%~100.8%,测定结果的相对标准偏差为2.1%~10.2%。该方法操作简单、灵敏度高、准确可靠,可用于火锅底料中5种非法添加罂粟壳生物碱的定量及确证分析。     

不同前处理方法对食品中罂粟壳检测效果对比

采用高效液相色谱-三重四极杆质谱联用法作为检测方法,通过对比QuEChERS法和固相萃取法(Oasis PRiME HLB和Oasis MCX)对不同食品基质火锅底料、辣椒粉和肉汤中5种生物碱检测效果的影响,优选食品中罂粟壳检测的普适性前处理方法。结果表明:5种生物碱中罂粟碱、那可丁、蒂巴因在0.2~10 μg/L,可待因、吗啡在1~50 μg/L的浓度范围内呈现出良好的线性关系,决定系数(R2)均大于0.9994;采用QuEChERS法和固相萃取法(Oasis PRiME HLB和Oasis MCX)分别对样品进行前处理后,测得的基质效应分别为0.12%~0.44%,0.02%~0.82%,0.07%~0.41%,检出限分别为0.1~5.0、0.1~8.0、0.1~5.0 μg/kg;回收率和相对标准偏差(RSDs)分别为70.6%~105.3%,64.2%~116.9%,73.6%~102.5%和2.0%~8.5%,1.6%~8.3%,1.6%~7.8%(n=6)。同时本研究对50批次市售火锅底料、辣椒粉、肉汤等样品进行检测,发现1批次石锅鸡汤含有那可丁、罂粟碱、蒂巴因和吗啡4种生物碱,所检出的生物碱成分与高效液相色谱-四极杆-飞行时间质谱仪的一级质谱匹配度良好。因此,固相萃取法(Oasis MCX)更适用于食品中罂粟壳检测的提取和净化,能够满足对不同基质食品中罂粟壳的定性、定量分析。     

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.