超高效液相色谱-串联质谱法测定牛奶中的黄曲霉毒素M1

目的 建立超高效液相色谱-串联质谱测定牛奶中黄曲霉毒素M_1的方法。方法 采用Acquityuplc BEH C_(18)液相色谱柱(50 mm×2.1 mm,1.7μm),梯度洗脱,多反应监测(MRM)。通过黄曲霉毒素M_1与免疫亲和柱中抗体结合,确定了从牛奶中提取黄曲霉毒素M_1的处理条件并优化了质谱的测定参数。结果 黄曲霉毒素M_1在0.1~10.0 ng/ml的范围内线性良好,其回归标准曲线方程的相关系数为0.997 8,回收率94.8%~98.2%,RSD为2.34%~3.87%,方法定量限为0.005μg/kg。结论 提供了一种有效检测牛奶中黄曲霉毒素M_1的方法。     

高效液相色谱-四极杆-高分辨飞行时间质谱直接进样测定饮用水中8种微囊藻毒素

目的建立了高效液相色谱-四极杆-高分辨飞行时间质谱测定饮用水中8种微囊藻毒素的检测方法。方法水样经亲水聚四氟乙烯滤膜过滤后,采用Poroshell 120 EC-C_(18)色谱柱(2.1mm×100mm,2.7μm)分离,高效液相色谱-四极杆-高分辨飞行时间质谱检测,采用高分辨多反应监测扫描模式进行监测,外标法定量。结果 8种微囊毒素在0.1～50.0μg/L线范围内线性关系良好,相关系数大于0.998以上,方法的检出限在0.05～0.10μg/L。在1、5、10μg/L3个水平浓度添加时,其平均回收率在83.2%～105.4%,相对标准偏差为2.5%～11.8%。结论该方法简单、快速、灵敏度高、重复性好,适合于饮用水中微囊藻毒素的日常检测。     

全自动固相萃取-高效液相色谱法同时测定饮用水中3种微囊藻毒素

建立全自动固相萃取-高效液相色谱法同时测定饮用水中3种微囊藻毒素的方法。采用全自动固相萃取仪代替传统的前处理方式,对大体积水样进行富集,以KH2PO4(p H=3.0)-甲醇(43∶57,v∶v)为流动相,采用二极管阵列检测器进行检测,结果 3种微囊藻毒素在0.1~10.0μg/m L范围内线性关系良好,相关系数r2≥0.999,3种不同微囊藻毒素的检出限均可达到0.05μg/L(S/N=3),加标回收率在86.3%~99.7%范围内,标准偏差为1.70%~2.72%(n=6),该方法用于测定饮用水中3种微囊藻毒素具有操作简单、快速,精密度高、准确可靠等特点。     

液相色谱-三重四级杆串联质谱法快速检测水中微囊藻毒素-LR

目的 建立液相色谱-三重四级杆串联质谱法快速检测水中微囊藻毒素-LR (microcystin-LR, MC-LR)含量的分析方法。方法 将水样直接过0.45 μm滤膜, 经色谱柱XDB-C18, 以乙腈和0.1%的甲酸水为流动相, 梯度洗脱, 柱温25 ℃, 流速0.2 mL/min, 外标法定量。结果 在微囊藻毒素-LR浓度为0.2~20 μg/L的范围内呈良好的线性关系(r2=0.999)。平均加标回收率在96.8%~101.7%, 相对标准偏差为0.21%~1.80%。检出限为0.2 μg/L, 定量限为0.5 μg/L。结论 该方法快速, 准确, 适用于水样中MC-LR的检测, 为相关检测机构的监测工作提供参考。     

水产品及螺旋藻片中微囊藻毒素检测方法研究

建立了超高效液相色谱-串联质谱法检测水产品及螺旋藻片中微囊藻毒素的高灵敏度色质联用快速检测方法。样品经溶剂超声提取、固相萃取净化,氮气吹至近干并定容后,通过超高效液相色谱-串联四极杆质谱仪检测。分离柱为Waters Acquity BEH C18柱(1.7μm,2.1 mm×100 mm);流动相为0.3%甲酸水溶液-乙腈;流速0.4 mL/min。4种不同基质样品中有害毒素微囊藻毒素MCYST-RR和MCYST-LR的检测限分别为0.7μg/kg和0.3μg/kg。4种不同基质样品中微囊藻毒素的回收率为80.0%～103.6%,相对标准偏差(RSD)为2.2%～14.6%(n=5),在0.01μg/mL～10μg/mL浓度范围内呈良好的线性关系,线性回归系数r2均大于0.999。     

三通道自动固相萃取-高效液相色谱四极杆串联质谱法检测水中8种痕量微囊藻毒素

目的建立三通道自动固相萃取-高效液相色谱-四极杆串联质谱法检测水中痕量的8种微囊藻毒素的分析方法。方法采用高自动化的前处理设备,采用C18固相萃取小柱富集浓缩,应用液相色谱-四极杆串联质谱法定性定量地检测8种微囊藻毒素。结果该方法检测水中的8种微囊藻毒素检出限为0.01~0.6μg/L,在0.25~62.5μg/L的线性范围中,线性相关系数大于0.99。结论该方法自动化程度高、灵敏度高、定性定量准确、测定浓度范围广。     

超高效液相色谱-串联质谱测定鸡饲料中黄曲霉毒素B_1

建立一种用超高效液相色谱-串联质谱法测定鸡饲料中黄曲霉毒素B_1的检测方法,并对广州市售11种鸡饲料进行了分析。试样经70%甲醇-水溶液超声提取,黄曲霉毒素B_1免疫亲和柱净化;以乙腈-0.1%甲酸水溶液为流动相梯度洗脱,采用Waters Acquity UPLC–BEH C_(18)柱(2.1 mm×50 mm×1.7μm)色谱柱分离,电喷雾正离子模式进行质谱测定。结果表明:该方法的黄曲霉毒素B_1检出限为0.5 ng/m L,线性范围为0.5000~50.00 ng/m L,相关系数为0.993 7,以空白样品为基质3个加标水平下黄曲霉毒素B_1的平均回收率为88.8%~93.5%,RSD5.0%。该方法准确高效,重现性好,可实现鸡饲料中黄曲霉毒素B_1的测定。     

免疫亲和柱净化-高效液相色谱-串联质谱法测定鱼肉和肝脏中河鲀毒素

目的采用免疫亲和柱净化鱼肉和肝脏中的河鲀毒素,建立高效液相色谱-三重四级杆质谱串联(LC-MS/MS)方法检测鱼肉和肝脏中的河鲀毒素,为水产品中的河鲀毒素检测提供方法依据。方法选用Zic-Hilic色谱柱(150 mm×2.1 mm,5μm),以10 mmol/L甲酸铵-0.1%甲酸-乙腈为流动相,采用梯度洗脱进行分离。样品用1%乙酸-甲醇沉淀蛋白提取,上清液加入PBS缓冲液后经免疫亲和柱净化,将洗脱液氮吹至干定容后上机测定。多重反应监测(MRM)方式检测。结果河鲀毒素的线性范围为1.0~1 000.0 ng/ml,鱼肉和肝脏中河鲀毒素的检出限分别为0.3和0.2μg/kg,回收率在52.4%~72.6%之间。结论本方法特异性强、提取效果好、无基质抑制效应,适用于鱼肉和肝脏中河鲀毒素的痕量检测。     

固相萃取-高效液相色谱法双检测器同时测定水中莠去津和苯并(a)芘

目的建立固相萃取-高效液相色谱法双检测器同时测定水中莠去津和苯并(a)芘分析方法。方法用大体积固相萃取柱富集莠去津和苯并(a)芘,二氯甲烷洗脱,使用Eclipse XDB-C18分析柱(150 mm×4.6 mm,5μm),采用乙腈-水体系作为流动相,梯度洗脱,二极管阵列检测器(DAD)和荧光检测器(FLD)检测。结果方法线性范围莠去津和苯并(a)芘分别为50~800μg/L、5.19~83.04μg/L,r均0.999;方法检出限分别为0.01、0.000 5μg/L;定量限为0.03、0.001 5μg/L;莠去津和苯并(a)芘在水中平均回收率分别为88.9%和90.4%;RSD均6.8%。结论该方法准确灵敏、精密度好,适用于水样中莠去津和苯并(a)芘测定。     

高效液相色谱-串联质谱法测定水产品中7种微囊藻毒素

建立了高效液相色谇串联质谱法同时测定水产品中7种微囊藻毒素（微囊藻毒素-RR、微囊藻毒素-YR、微囊藻毒素-LR、微囊藻毒素-LA、微囊藻毒素-LW、微囊藻毒素-LF、微囊藻毒素．LY）的分析方法。样品用90%醇水（P／g）溶液提取,经离心、固相萃取柱净化后,用C18柱,以0．1％甲酸乙腈．0．1％甲酸溶液为流动相,梯度洗悦分离,使用三重四级杆质谱检测器捡测,以保留时间及特征离子对定性,外标法定量。结果表明,7种微囊藻毒素在线性范围内线性关系良好,相关系数均不低于0．9990,方法的定量限（以信噪比为10计）为0．2-0．5μg／kg,添加水平为1．0-20μg／kg时,回收率为71．5-106％,相对标准偏差（n=6）为312～9．1％。该法前处理简单、回收率高、精密度好,适用于水产品中7种微囊藻毒素的测定。     

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