HPLC-MS/MS测定八宝粥中8种霉菌毒素

建立了测定八宝粥中黄曲霉毒素B_1、B_2、G_1、G_2,T-2毒素,赭曲霉毒素A,玉米赤霉烯酮和杂色曲霉素8种霉菌毒素的高效液相色谱串联质谱(HPLC-MS/MS)法。样品经乙腈-水(88:12,V/V)超声提取、离心后,用多功能净化柱净化,以乙腈和5 mmol/L甲酸铵水溶液(含0.1%甲酸)为流动相梯度洗脱,经ZORBAX Eclipse Plus C_(18)色谱柱(2.1 mm×100 mm,1.8μm)分离,多反应监测(MRM)正离子模式进行检测,外标法定量。在0.5~50.0 ng/mL的浓度范围内,8种霉菌毒素均具有良好的线性关系(r≥0.999 6)。此方法的检出限为0.06~0.18μg/kg,平均回收率为73.5%~97.4%,RSD为4.6%~8.2%(n=7)。该方法简便、准确、灵敏,适用于八宝粥中黄曲霉毒素B_1、B_2、G_1、G_2,T-2毒素,赭曲霉毒素A,玉米赤霉烯酮和杂色曲霉素的同时检测。     

超高效液相色谱-串联质谱法快速检测动物饲料中5种霉菌毒素

目的建立一种同步、快速的测定饲料中5种主要霉菌毒素的超高效液相色谱-串联质谱(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)检测方法。方法样品经84%乙腈水(含0.1%甲酸)提取液提取, MLJ-1杂质吸附型固相萃取柱净化。采用0.1mmol/L乙酸铵/0.1%甲酸-水(A)和0.1%甲酸-甲醇(B)作为流动相进行梯度洗脱,质谱采用多反应监测模式(multiplereactionmonitoring,MRM)对霉菌毒素及其同位素内标的定量离子和定性离子进行监测。结果本方法在1min内完成样品净化处理,15 min内完成5种目标化合物的分离分析。5种霉菌毒素在高、中和低浓度添加水平的回收率为83.9%～113.8%,相对标准偏差为0.6%～15.0%(n=6),方法定量限为0.3～4.0μg/kg。结论该方法操作简单、快速,适合饲料中5种主要霉菌毒素同步确证检测。     

高效液相色谱-串联质谱法测定3种水产品中的T-2毒素与HT-2毒素

建立高效液相色谱-串联质谱定量快速检测罗非鱼、南美白对虾和黄金贝中的T-2毒素与HT-2毒素方法。以10 mL乙酸乙酯作为提取溶剂,振荡提取,无水硫酸钠除水,定量移取5 mL提取液氮气吹干后用1 mL含有0.1%甲酸的甲醇-5 mmol/L乙酸铵溶液（3∶7,V/V）复溶,正己烷脱脂净化,基质匹配法外标定量。3 种水产品中T-2毒素和HT-2毒素的检出限分别为2 μg/kg和4 μg/kg。T-2毒素质量浓度为2～100 ng/mL,HT-2毒素质量浓度为4～200 ng/mL,范围内线性良好。在3 种样本中进行3 个水平添加实验（n=6）,T-2毒素回收率为84.3%～109.9%,HT-2毒素的回收率为90.9%～103.2%。T-2毒素的相对标准偏差为2.0%～8.7%,HT-2毒素的相对标准偏差为2.6%～10.6%。本方法简便快速、准确度好、精密度高,适用于3 种代表性水产品中T-2与HT-2毒素的同时检测。     

高效液相色谱-串联质谱法测定杂粮豆类中11种真菌毒素

利用高效液相色谱-串联质谱建立杂粮豆类中11种真菌毒素（包括黄曲霉毒素B1、B2、G1、G2、赭曲霉毒素A、T-2毒素、脱氧雪腐镰刀菌烯醇、伏马毒素B1、B2和B3、玉米赤霉烯酮）同时检测的方法。实验对提取溶剂、提取时间和净化方式等进行优化,建立双体系联合提取方法,首先采用甲醇-水（70∶30,V/V）体系提取,再以乙腈-水（84∶16,V/V）体系二次提取,提取时间3 min,在此基础上采用C18吸附剂进行净化处理。结果表明,11种毒素的线性范围良好,相关系数大于0.999,添加回收率为70.0%～108%,相对标准偏差为1.3%～8.6%。所建方法简单、快速、灵敏度高、重复性好,可满足杂粮豆类中11 种真菌毒素的同时检测需要。     

固相萃取柱净化-超高效液相色谱-串联质谱法快速测定液态乳中14 种真菌毒素

建立使用固相萃取柱净化液态乳中14 种真菌毒素（黄曲霉毒素B1、黄曲霉毒素B2、黄曲霉毒素G1、黄曲霉毒素G2、黄曲霉毒素M1、赭曲霉毒素A、橘霉素、T-2毒素、杂色曲霉素、伏马毒素B1、伏马毒素B2、玉米赤霉烯酮、脱氧雪腐镰刀菌烯醇、青霉酸）多残留的超高效液相色谱-串联质谱检测方法。样品经含0.1%甲酸-乙腈沉淀蛋白和提取,固相萃取柱Oasis PRiME HLB净化后,以0.1%甲酸溶液与乙腈为流动相,经ACQUITY UPLC HSS T3色谱柱（2.1?mm×100?mm,1.8?μm）分离,梯度洗脱,采用电喷雾-正离子多反应监测模式,外标法定量。结果表明：14?种真菌毒素的定量限（RSN≥10）为0.5～5?μg/kg,高、中、低3?个添加水平时,平均回收率为67.7%～112.7%,相对标准偏差为0.43%～7.28%。该方法的检测速度快,净化效果较好,基质干扰较少,灵敏度高,结果准确、可靠,可用于液态乳中真菌毒素的检测分析。     

UPLC-MS/MS法测定玉米中13种真菌毒素

建立了超高压液相色谱串联质谱法(UPLC-MS/MS)测定玉米中脱氧雪腐镰刀菌烯醇及其乙酰化衍生物、玉米赤霉烯酮、黄曲霉毒素B1/B2/G1/G2、伏马毒素B1/B2、赭曲霉毒素A、T-2和HT-2等13种真菌毒素的分析方法。样品采用乙腈∶水∶乙酸(80∶19∶1,V/V/V)提取后,经过稀释、离心和过滤的前处理操作即可进行仪器测定。结果表明,13种真菌毒素的定量限在1~200μg/kg之间,3个浓度添加水平回收率为80%~114%,相对标准偏差为0.9%~10.9%,基体标准物质测定结果均在标准值±不确定度的范围内。     

液相色谱-串联质谱联用法测定酱油中T-2毒素残留

目的:研究以液相色谱-串联质谱联用法测定酱油中T-2毒素含量的方法。方法:液相色谱-串联质谱法。用乙腈-0.1%甲酸溶液提取酱油,经C18净化,电喷雾正离子多反应监测(MRM)模式检测。结果:T-2毒素在1～25μg/L的系列浓度范围呈线性相关,酱油中T-2毒素的检测限为2.0μg/kg,定量限为5.0μg/kg,在2～20μg/kg的添加浓度范围内平均回收率为85.5%～98.2%。结论:该方法灵敏度高,重现性好,可作为酱油中T-2毒素残留量检测方法。     

高效液相色谱-串联质谱法测食品中的赭曲霉毒素A

研究建立高效液相色谱-串联质谱联用技术检测食品中赭曲霉毒素A的方法。根据不同样品,用甲醇-2%碳酸氢钠溶液(60:40,V/V)或甲醇-水(80:20,V/V)提取样品中的赭曲霉毒素A,经OchraTest亲和柱净化,以甲醇-5mmol/L(含0.1%甲酸)乙酸铵为流动相,采用正离子模式对赭曲霉毒素A进行检测。结果回收率在82.3%～98.5%之间,检出限为0.1μg/kg。该方法适用不同基质样品,准确性好、灵敏度高、抗干扰能力强,方法检出限可满足欧盟等最新限量要求。     

免疫亲和柱净化-液相色谱-串联质谱法同时测定水产品中8种霉菌毒素

目的:建立免疫亲和柱净化-液相色谱-串联质谱法(LC-MS/MS)同时测定水产品中8种霉菌毒素残留。方法:样品经乙腈水溶液(84:16,V:V)提取,多毒素免疫亲和柱净化。色谱柱为Agilent Proshell 120 SB·C₁₈(2.1 mm×100 mm,2.7μm),流动相为甲醇-5 mmol/L乙酸铵(含0.1%甲酸),梯度洗脱,流速为0.4 mL/min,柱温为40℃。采用电喷雾离子源正负离子同时扫描,多反应监测模式(MRM)进行质谱检测。结果:8种霉菌毒素在1.0～50.0 ng/mL范围内线性关系良好(R²>0.992),方法检出限在0.05～0.50μg/kg之间,定量限在0.17～1.65μg/kg之间;8种霉菌毒素加标回收率在75.6%～106.3%之间,相对标准偏差(RSD)为3.5%～9.3%。结论:该方法操作便捷、灵敏度高、准确可靠,能满足水产品中多种霉菌毒素残留快速检测需求。     

高效液相色谱串联质谱法测定花生及制品中的五种真菌霉素

建立了高效液相色谱-串联质谱(HPLC-MS/MS)测定花生及制品中黄曲霉毒素B1、黄曲霉毒素M1、脱氧雪腐镰刀菌烯醇、赭曲霉毒素A、玉米赤霉烯酮五种真菌霉素的快速分析方法。用甲醇-水(55:45,V/V)对样品进行提取,采用真菌毒素免疫亲和柱萃取,在ESI+模式下采用多反应监测(MRM)模式进行检测。目标物在C18色谱柱上实现了有效分离,在6 min内完成一个样品的分析,相关系数(r2,n=6)大于0.999,检测结果稳定、灵敏。黄曲霉毒素B1、黄曲霉毒素M1、脱氧雪腐镰刀菌烯醇线性范围0.5~50.0μg/L,检出限为0.05μg/kg(LOD,S/N=3),赭曲霉毒素A、玉米赤霉烯酮线性范围5.0~100.0μg/L,检出限为0.5μg/kg(LOD,S/N=3),方法回收率为86.8~102.7%,精密度RSD为0.36~4.79%。该方法快速、灵敏,适用于花生及制品中黄曲霉毒素B1、黄曲霉毒素M1、脱氧雪腐镰刀菌烯醇、赭曲霉毒素A、玉米赤霉烯酮五种真菌霉素的检测与确证。     

Reliable identification of grapevine rootstock varieties using RAPD PCR on woody samples

Since grapevine ( Vitis spp .) rootstock material is being traded increasingly as disbudded woody material a lack of distinctive morphological features on such material necessitates an alternative and reliable means of identification. Methods described here were developed for rapid and efficient extraction of DNA from woody samples rich in phenolic compounds and polysaccharides, and for subsequent identification of varieties by RAPD PCR. Using these methods, and with the application of only one selected RAPD primer, we were able to differentiate sixteen rootstock varieties, including the seven varieties most commonly used in Germany. Problems commonly encountered with reproducibility of RAPD patterns were avoided by choosing primers with a dinucleotide sequence and a high G/C content that allowed a rather high annealing temperature of 45°C. Methods described here should also be useful for other horticultural crops, especially those with woody tissues rich in phenolic compounds and polysaccharides.     

An internet compendium of analytical methods and spectroscopic information for monomers and additives used in food packaging plastics

An internet website (http://cpf.jrc.it/smt/) has been produced as a means of dissemination of methods of analysis and supporting spectroscopic information on monomers and additives used for food contact materials (principally packaging). The site which is aimed primarily at assisting food control laboratories in the European Union contains analytical information on monomers, starting substances and additives used in the manufacture of plastics materials. A searchable index is provided giving PM and CAS numbers for each of 255 substances. For each substance a data sheet gives regulatory information, chemical structures, physico-chemical information and background information on the use of the substance in particular plastics, and the food packaging applications. For monomers and starting substances (155 compounds) the infra-red and mass spectra are provided, and for additives (100 compounds); additionally proton NMR are available for about 50% of the entries. Where analytical methods have been developed for determining these substances as residual amounts in plastics or as trace amounts in food simulants these methods are also on the website. All information is provided in portable document file (PDF) format which means that high quality copies can be readily printed, using freely available Adobe Acrobat Reader software. The website will in future be maintained and up-dated by the European Commission's Joint Research Centre (JRC) as new substances are authorized for use by the European Commission (DG-ENTR formerly DGIII). Where analytical laboratories (food control or other) require reference substances these can be obtained free-ofcharge from a reference collection housed at the JRC and maintained in conjunction with this website compendium.     

Chlorohydrins of bisphenol A diglycidyl ether (BADGE) and of bisphenol F diglycidyl ether (BFDGE) in canned foods and ready-to-drink coffees from the Japanese market

BADGE.2HCl and BFDGE.2HCl were determined in 28 samples of ready-to-drink canned coffee and 18 samples of canned vegetables (10 corn, 5 tomatoes and 3 others), all from the Japanese market. HPLC was used as the principal analytical method and GCMS for confirmation of relevant LC fractions. BADGE.2HCl was found to be present in one canned coffee and five samples of corn, BFDGE.2HCl in four samples of canned tomatoes and in one canned corn. No sample was found which exceeded the 1mg/kg limit of the EU for the BADGE chlorohydrins. However the highest concentration was found for the sum of BFDGE.2HCl and BFDGE.HCl.H₂O at a level of 1.5mg/kg. A Beilstein test confirmed that all cans containing foods contaminated with BADGE.2HCl or BFDGE.2HCl had at lest one part coated with a PVC organosol.     

European priorities for research to support legislation in the area of food contact materials and articles

A strong science base is required to underpin the planning and decision-making process involved in determining future European community legislation on materials and articles in contact with food. Significant progress has been made in the past 5 years in European funded work in this area, with many developments contributing to a much better understanding of the migration process, and better and simpler approaches to food control. In this paper this progress is reviewed against previously identified work-areas (identified in 1994) and conclusions are reached about future requirements for R&D to support legislation on food contact materials and articles over the next 5 or so years.     

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.     

Aroma characterization of various apricot varieties using headspace–solid phase microextraction combined with gas chromatography–mass spectrometry and gas chromatography–olfactometry

The characterization of the aromatic profile of several apricot cultivars with molecular tracers in order to obtain objective data concerning the aromatic quality of this fruit was undertaken using headspace–solid phase microextraction (HS–SPME). Six apricot cultivars were selected according to their organoleptic characteristics: Iranien, Orangered, Goldrich, Hargrand, Rouge du Roussillon and A4025. The aromatic intensity of these varieties measured by HS–SPME–Olfactometry were defined and classified according to the presence and the intensity of grassy, fruity and apricot like notes. In the six varieties, 23 common volatile compounds were identified by HS–SPME–GC–MS. Finally, 10 compounds, ethyl acetate, hexyl acetate, limonene, β-cyclocitral, γ-decalactone, 6-methyl-5-hepten-2-one, linalool, β-ionone, menthone and (E)-hexen-2-al were recognized by HS–SPME–GC–O as responsible of the aromatic notes involved in apricot aroma and considered as molecular tracers of apricot aromatic quality which could be utilized to discriminate apricot varieties.     

Tests of potential functional barriers for laminated multilayer food packages. Part I: Low molecular weight permeants

The advent of the functional barrier concept in food packaging has brought with it a requirement for fast tests of permeation through potential barrier materials. In such tests it would be convenient for both foodstuffs and materials below the functional barrier (sub-barrier materials) to be represented by standard simulants. By means of inverse gas chromatography, liquid paraffin spiked with appropriate permeants was considered as a potential simulant of sub-barrier materials based on polypropylene (PP) or similar polyolefins. Experiments were performed to characterize the kinetics of the permeation of low molecular weight model permeants (octene, toluene and isopropanol) from liquid paraffin, through a surrogate potential functional barrier (25 μm-thick oriented PP) into the food simulants olive oil and 3% (w/v) acetic acid. These permeation results were interpreted in terms of three permeation kinetic models regarding the solubility of a particular model permeant in the post-barrier medium (i.e. the food simulant). The results obtained justify the development and evaluation of liquid sub-barrier simulants that would allow flexible yet rigorous testing of new laminated multilayer packaging materials.     

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.     

Influence des ions sur le pouvoir hydratant de l'ure e: e tude sur peau de porc ex vivo

This study deals with the influence of ions (NaCl and MgSO4) in a W/O emulsion containing 10% urea. Moisturization kinetics are assessed by corneometry on pig skin ex vivo. The formula's influence on urea penetration is measured by infrared spectrometry with an ATR device and the stripping method. Corneometry and spectroscopy were chosen to record simultaneously the hydratation levels and urea localization into superficial cell layers. Urea crystallization after evaporation of emulsions and aqueous solutions is described. Results show that urea does not hydrate nor penetrate when applied to the skin through an aqueous gel. In a W/O emulsion, sodium chloride increases the ability of urea to moisturize without improving penetration. In vitro urea crystallization is disturbed by sodium chloride or magnesium sulphate for solutions and emulsions. This stabilization by ions is correlated with good moisturization values. The stabilization of urea in the solute state provided by ions increases its water epidermal binding capacity without enhancing penetration.