QuEChERS-超高效液相色谱串联质谱法测定发酵黑茶中的10种真菌毒素

建立了云南普洱茶、湖南黑茶、广西六堡茶和湖北老青茶等发酵黑茶黄曲霉毒素B1（AFB1）、黄曲霉毒素B2（AFB2）、黄曲霉毒素G1（AFG1）、黄曲霉毒素G2（AFG2）、脱氧雪腐镰刀菌烯醇（DON）、3-乙酰基脱氧雪腐镰刀菌烯醇（3-AcDON）、玉米赤霉烯酮（ZEN）、T-2毒素（T-2）、HT-2毒素（HT-2）、赭曲霉毒素A（OTA）等10种真菌毒素的简单、快速、高灵敏度超高效液相色谱-串联质谱检测方法。样品采用乙腈/水溶液（84+16）提取试样、QuEChERS净化,试样以C18柱分离,多反应监测（MRM）模式进行定量与定性分析,采用外标法定量。结果表明,在优化的条件下,10种真菌毒素在各自的线性响应范围内线性关系良好,相关系数（r）均不小于0.9995,定量限（LOQ）为0.1~10 μg/kg,在三个不同加标水平下平均回收率为61.9%~120.3%,相对标准偏差（RSD）为3.2%~16.1%。采用建立的方法对市面上销售的黑茶中的10种真菌毒素进行了筛查,数批产品检出真菌毒素。该方法简单、准确、可靠,可适用于发酵黑茶中多种真菌毒素的快速分析。     

多功能柱净化-超高效液相色谱串联质谱法同时测定水产品中11种真菌毒素

建立了同步测定水产品中黄曲霉毒素B1(AFB1)、黄曲霉毒素B2(AFB2)、黄曲霉毒素G1(AFG1)、黄曲霉毒素G2(AFG2)、黄曲霉毒素M1(AFM1)、赭曲霉毒素A(OTA)、玉米赤霉烯酮(ZEN)、脱氧雪腐镰刀菌烯醇(DON)、3-乙酰基脱氧雪腐镰刀菌烯醇(3-Ac DON)、15-乙酰基脱氧雪腐镰刀菌烯醇(15-Ac DON)、镰刀菌烯酮(Fus-X)等11种真菌毒素的超高效液相色谱-串联质谱分析方法。试样样品以乙腈/水溶液(84+16)提取,Myco Spin 400多功能柱净化,Waters ACQUITY UPLCTM BEH C18柱分离,多反应监测(MRM)模式进行定量与定性分析,外标法定量。结果表明,11种目标物在各自的线性响应范围内线性关系良好,相关系数(r)≥0.9918,定量限(LOQ)为0.1~20.0μg/kg,加标平均回收率(n=3)为62.8%~115.3%,相对标准偏差(RSD)为2.6%~19.0%。该方法前处理简单、净化效果好、灵敏度高、重现性好,适合于水产品中痕量真菌毒素的多残留快速检测。     

免疫亲和柱净化-超高效液相色谱串联质谱法同时测定火锅底料中的5种真菌毒素

目的：建立复合免疫亲和柱净化、超高效液相色谱串联质谱检测火锅底料中的黄曲霉毒素B1(Aflatoxins B1,AFB1)、黄曲霉毒素B2(Aflatoxins B2,AFB2)、黄曲霉毒素G1(Aflatoxins G1,AFG1)、黄曲霉毒素G2(Aflatoxins G2,AFG2)、赭曲霉毒素A(Ochratoxin A, OTA)的方法。方法：样品提取后,经复合免疫亲和柱净化,以0.1%甲酸水和甲醇为流动相梯度洗脱,用Agilent EclipsePlus C18 RRHD色谱柱分离,ESI+进行多反应监测,内标法定量。结果：5种真菌毒素的线性范围在0.1～10.0 ng/mL,相关系数(r)>0.999,检出限0.1μg/kg,定量限0.3μg/kg。3个加标水平下(0.2、5.0、10.0μg/kg)的回收率在81.38%～97.87%之间,相对标准偏差为0.79%～6.18%。结论：该方法快速准确,可用于火锅底料中5种真菌毒素的定性、定量检测。     

超高效液相色谱-质谱联用法检测地理标志产品松江大米中8种真菌毒素的含量

建立超高效液相色谱-三重四极杆质谱法同时检测大米基质中8种真菌毒素的方法,对地理标志产品松江大米中真菌毒素的污染情况进行监测。大米样品经提取液乙腈水混合液（84:16,v:v）超声提取后,取部分提取液加入内标溶液,混匀后过多功能净化柱MycoSep229净化,采用Waters Acquity UPLC?BEH?C18色谱柱 (2.1 mm×50 mm, 1.7 μm),以0.1%（v:v）甲酸水溶液-乙腈作为流动相进行梯度洗脱,分离黄曲霉毒素B1（Aflatoxin B1, AFB1）、黄曲霉毒素B2（Aflatoxin B2, AFB2）、黄曲霉毒素G1（Aflatoxin G1,AFG1）、黄曲霉毒素G2（Aflatoxin G2, AFG2）、伏马毒素B1（FumonisinsB1, FB1）、伏马毒素B2（FumonisinsB2, FB2）、伏马毒素B3（FumonisinsB3, FB3）、赭曲霉毒素A（Ochratoxin A, OTA） 8种真菌毒素化合物,该方法采用电喷雾离子化正离子模式,以多反应监测方式进行。AFB1、AFG1、FB1、FB2、FB3、OTA 6种真菌毒素在0.5-15μg/L范围内线性良好,AFB2、AFG2在0.125-3.75μg/L范围内线性良好,线性相关系数r均大于0.999;8种化合物定量限(limit of quantifications, LOQs)范围为0.01-0.25 μg/kg,比国标中相同方法的定量限降低2-80倍不等;在低、中、高三水平加标,其回收率均在95%~120%范围内,相对标准偏差(relative standard deviations, RSDs)为1.5%~8.9% (N=6)。本方法前处理简单,方法利用率高,结果准确可靠,利用该方法检测的20批新上市松江大米中真菌毒素污染情况比较乐观,对人体的健康危害较低。     

HPLC-MS/MS法测定曲霉菌代谢物中黄曲霉毒素及同系物

建立了同时检测曲霉菌代谢物中黄曲霉毒素和同系物的高效液相色谱-线性离子阱质谱测定方法。产黄曲霉毒素B1(AFB1)寄生曲霉(菌株3.124)经PDA固体培养基培养,提取净化后经线性离子阱(QTrap)质量分析器分析(正离子模式,多反应检测),以AFB1二级碎片(MS2)信息和其同系物分子式信息预测代谢物MRM方法,检出3.124代谢物中黄曲霉毒素B2(AFB2)、黄曲霉毒素G1(AFG1)、黄曲霉毒素G2(AFG2)、O-甲基杂色曲霉素(MST)、杂色曲霉素(ST)5种真菌毒素,并用标准品进行了确证。结果表明,AFB2和AFG2在0.5μg/L~40μg/L,其它4种代谢物在0.2μg/L~40μg/L范围内线型关系良好,相关系数均大于0.99。本方法 6种代谢物日内回收率81.3%~92.3%,相对标准偏差(RSD)为3.4%~6.2%;日间回收率82.1%~91.7%,RSD为3.8%~7.7%。该方法为快速检测霉菌代谢物中的同系物提供新的方法。     

高效液相色谱法同时检测粮食中常见8 种真菌毒素的含量

建立免疫亲和柱净化-高效液相色谱法同时测定粮食中黄曲霉毒素B1（aflatoxins,AFB1）、黄曲霉毒素B2（AFB2）、黄曲霉毒素G1（AFG1）、黄曲霉毒素G2（AFG2）、赭曲霉毒素A（ochratoxin A,OTA）、玉米赤霉烯酮（zearalenone,ZEN）、呕吐毒素（deoxynivalenol,DON）和T-2毒素的检测方法。样品经乙腈-水提取后,用免疫亲和柱净化,Agilent Elipse Plus C18（100 mm×4 mm,3.5 μm）色谱柱分离,以甲醇-乙腈-水-乙酸为流动相,流速1 mL/min,柱温35 ℃,进样量20 μL,检测系统为可变波长检测器串联光化学衍生器串联荧光检测器。根据信噪比为3的峰响应值,确定各真菌毒素的检出限为：AFB1 0.446 ng/mL、AFB2 0.152 ng/mL、AFG1 0.523 ng/mL、AFG2 0.334 ng/mL、ZEN 7 ng/mL、OTA 0.7 ng/mL、DON 200 ng/mL、T-2毒素100 ng/mL。样品中各真菌毒素的平均加标回收率,玉米为80.0%～104.5%,小麦为83.2%～102.8%,方法精密度为2.6%～10.2%。从样品前处理到分析整个过程耗时约2 h。本方法简便、快速、灵敏度高,适用于粮食中多种真菌毒素的快速测定。     

利用液相色谱对原粮的真菌毒素检测——HPLC法测定玉米赤霉烯酮

<正>真菌毒素是一种真菌产生的有毒代谢产物。常见的污染粮食的真菌毒素包括:玉米赤霉烯酮(zearalenone,ZEN)、赭曲霉毒素A(ochratoxin A,OTA)、黄曲霉毒素B1(aflatoxins,AFB1)、黄曲霉毒素B2(AFB2)、黄曲霉毒素G1(AFG1)、黄曲霉毒素G2(AFG2)、呕吐毒素(deoxynivalenol,DON)以及T-2毒素等。根据大量研究文献及实验室的长期监测数据,出现很多粮食中同时遭到多种真菌毒素污染的情况。在基层实验室检测仪器配置情况的基础上,我国     

粮油中黄曲霉毒素检测研究

正黄曲霉毒素(AFT)是由黄曲霉和寄生曲霉在温度、湿度合适的条件下产生的真菌毒素,其存在对人体具有极强的致癌、致畸等危害,包括AFB1、AFB2、AFG 1、AFG 2等~([1,2])。全世界每年约有1/4的食品会受到黄曲霉毒素的污染,花生、玉米等原料在生产、运输中易受黄曲霉毒素的污染~([3])。现有免疫亲和柱净化-高效液     

高效液相色谱法测定食用植物油中6种真菌毒素

建立了基于分散液液微萃取技术（DLLME）的高效液相色谱法同时测定食用植物油中6种真菌毒素的方法。样品经石油醚脱脂，乙腈-水-乙酸（体积比84∶ 15∶ 1）超声提取，CHCl3为萃取剂液液萃取净化及柱前衍生化后，以Agilent XDB-C18色谱柱（4.6 mm×150 mm, 3.5 μm）分离，梯度洗脱，经荧光检测器检测。结果表明：食用植物油中6种真菌毒素的线性关系良好，相关系数均大于0.999，方法检出限为0.2~0.5 μg/kg，样品的平均加标回收率为75.88%~105.25%，相对标准偏差为0.5%~9.5%。该方法可用于食用植物油中黄曲霉毒素（AFB1、AFB2、AFG1、AFG2）以及赭曲霉毒素（OTA、OTB）6种真菌毒素的同时检测。     

液相色谱—串联质谱法同时检测食品中的4种黄曲霉毒素

建立同时对食品中的4种黄曲霉毒素进行定性定量分析的高效液相色谱三重四极杆质谱确证方法.样品经甲醇-水提取、免疫亲和柱净化后,用高效液相色谱-串联质谱进行分析测定.黄曲霉毒素在所测浓度范围内与峰面积呈良好的线性关系,r＞0.998,平均加标回收率在80.6％～ 100.6％,相对标准偏差(RSD)在1.1％～7.5％,AFB1、AFG1的最低检出限为0.2 μg/kg,AFB2、AFG2的最低检出限为0.05 μg/kg.该方法快速、灵敏、准确、可靠,是食品中的黄曲霉毒素B1、B2、G1、G2测定的理想方法.     

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.     

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.     

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.     

Analysis of benzo[a]pyrene in spiked fatty foods by second derivative synchronous spectrofluorimetry after microwave-assisted treatment of samples

A simple, rapid and inexpensive method has been developed for the determination of benzo[a     

The development of reference materials for paralytic shellfish poisoning toxins in lyophilized mussel. II: Certification study

This paper describes the second part of a project undertaken to develop certified mussel reference materials for paralytic shellfish poisoning toxins. In the first part two interlaboratory studies were undertaken to investigate the performance of the analytical methodology for several PSP toxins, in particular saxitoxin and decarbamoyl-saxitoxin in lyophilized mussels, and to set criteria for the acceptance of results to be applied during the certification exercise. Fifteen laboratories participated in this certification study and were asked to measure saxitoxin and decarbamoyl-saxitoxin in rehydrated lyophilized mussel material and in a saxitoxin-enriched mussel material. The participants were allowed to use a method of their choice but with an extraction procedure to be strictly followed. The study included extra experiments to verify the detection limits for both saxitoxin and decarbamoyl-saxitoxin. Most participants (13 of 15) were able to meet all the criteria set for the certification study. Results for saxitoxin.2HCl yielded a certified mass fraction of <0.07 mg/kg in the rehydrated lyophilized mussels. Results obtained for decarbamoyl-saxitoxin.2HCl yielded a certified mass fraction of 1.59+/-0.20 mg/kg. The results for saxitoxin.2HCl in enriched blank mussel yielded a certified mass fraction of 0.48 +/- 0.06 mg/kg. These certified reference materials for paralytic shellfish poisoning toxins in lyophilized mussel material are the first available for laboratories to test their method for accuracy and performance.     

Announcing a new international peer-reviewed journal:Food Science and Human Wellness now accepting manuscript submission in English

<正>We are pleased to announce the launch of a new international peer-reviewed journal-Food Science and Human Wellness,ISSN 2213-4530,which is an open access journal,produced and hosted by Elsevier B.V.on behalf of Beijing Academy of Food Sciences.Food Science and Human Wellness is an international peer-reviewed English journal that provides a forum for the dissemination of the