万通酱油HPLC指纹图谱的研究及其在真伪鉴别中的应用

试验摸索出建立万通酱油HPLC指纹图谱共有模式的最佳试验方案,即色谱柱:ODS-C18(250 mm×4.6 mm,5μm);流动相:CH3OH-0.02 mol/L K2HPO4溶液(2∶98);柱温:室温;检测波长210 nm;流速为0.8 mL/min。在该条件下,样品经C18柱脱色处理后,30 min内就完成了HPLC指纹图谱的检测。应用指纹图谱相似度评价系统软件对各样品图谱信息进行处理,选出10批优质正品万通酱油样品生成酱油HPLC指纹图谱共有模式,从中选出7个重复性好的色谱峰作为万通酱油HPLC指纹图谱的特征峰。以相似度大小作为判定万通酱油质量合格与否的标准,将生成的对照指纹图谱与伪品酱油HPLC指纹图谱进行比较,即可判断出真伪。     

苦瓜皂苷高效液相色谱指纹图谱研究

建立苦瓜皂苷类成分的高效液相色谱法(HPLC)指纹图谱.采用中药色谱指纹图谱相似度评价系统,对不同产地苦瓜中皂苷进行HPLC分析,流动相:乙腈和水梯度洗脱;流速:1.0mL/min;色谱柱:ZorbaxSB-C18柱(150×4.6mm,5 μm);柱温:25℃;检测波长:209 nm;进样量:20 μL;分析时间:65 min.确定8个共有峰作为苦瓜皂苷的特征指纹峰;不同产地苦瓜皂苷指纹图谱与对照指纹图谱(R)的相似度均大于0.85.该方法建立的苦瓜皂苷HPLC指纹图谱,为苦瓜鉴别和品质评价、质量控制、制定质量标准提供参考.     

基于高效液相色谱指纹图谱的油菜花粉质量评价研究

目的:构建油菜花粉HPLC指纹图谱,为油菜花粉质量评价以及质量控制提供依据。方法:以芦丁为内标物,采用Diamonsil C18柱(250mm×4.6mm,5μm)为分析色谱柱,乙腈-0.4%磷酸水溶液为流动相梯度洗脱,流速0.8mL/min。结果:10批不同产地油菜花粉的HPLC指纹图谱较相似,各成分得到较好地分离,并根据检测结果确定了10个共有指纹峰。精密度和重复性试验中,各共有指纹峰相对保留时间和相对峰面积的相对标准偏差(RSD)均在3%以内,符合指纹图谱技术要求。结论:该方法具有重现性好,特征性强,方法简便、快速等特点,能够客观反映油菜花粉的指纹特征,可以作为油菜花粉质量评价及控制的表征指标。     

陕西平利绞股蓝氨基酸类成分指纹图谱研究

采用柱前衍生高效液相色谱(HPLC)技术对陕西平利绞股蓝中氨基酸类成分的指纹图谱进行研究。结果表明,以邻苯二甲醛为柱前衍生试剂,Kromasil C18分离,流动相为0.05mol/L醋酸钠+0.5%四氢呋喃-甲醇,采用梯度洗脱,绞股蓝中氨基酸类成分可得到良好的分离,同时对样品中16种氨基酸的含量进行定量;通过对13批样品HPLC图谱的分析,共确定22个色谱峰作为平利绞股蓝的特征指纹峰,利用夹角余弦法、相关系数法、中药色谱指纹图谱相似度评价系统软件进行相似度计算,13批陕西平利绞股蓝指纹图谱相似度0.989~1.00之间,该图谱能综合、准确地反映陕西平利绞股蓝氨基酸类成分的特征,为保护平利绞股蓝原产地域产品提供了新的途径。     

花椒HPLC指纹图谱建立及指标性成分的测定

文章采用HPLC法建立多批次花椒指纹图谱,并测定其主要成分含量。指纹图谱的色谱条件为Wondasil C18色谱柱(250mm×4.6mm,5μm),乙腈-水梯度洗脱,检测波长268nm,柱温30℃,流量0.8mL/min。以其指纹图谱为特征,进行相似度和聚类分析。指纹图谱确定了12个共有峰,所有样品的相似度均大于0.9,表明各产地花椒具有较好的一致性;当类间距离为10时,16批次花椒样品被分成3大类;花椒的2个主要成分羟基-α-山椒素的含量在0.323%～1.570%,羟基-β-山椒素的含量在0.03%～0.622%。花椒样品各批次间指纹图谱和主要成分含量均有一定的差异。建立的花椒HPLC指纹图谱及主要成分含量测定方法可为花椒食品质量控制和评价提供科学依据。     

基于HPLC 指纹图谱和定量分析法评价酸枣仁质量

目的：建立中药酸枣仁高效液相色谱(HPLC)指纹图谱,为科学评价不同产地酸枣仁药材质量提供新方法。方法：采用UltimateTM C18 柱 (250mm × 4.6mm,5μm),乙腈- 超纯水梯度洗脱,流速1.0mL/min,检测波长210nm,柱温30℃。通过夹角余弦法和相关系数法计算17 批样品的相似度,并对其进行聚类。结果：聚类分析表明,17批不同规格样品被聚为3 类,即主产区、一般产区和次品。主产区酸枣仁相似度均高于0.9239,酸枣仁皂苷A 含量范围为0.8123～1.1109mg/g。结论：采用HPLC 法建立指纹图谱并结合指标成分定量分析的方法可作为酸枣仁质量评价的参考依据。     

可可粉色谱指纹图谱的构建及其质量控制中的应用

目的:建立可可粉高效液相指纹图谱。方法:采用RP-HPLC法。色谱柱为Agilent ZORBAX Extend-C18(250mm×4.6mm,5μm);以乙腈-0.05%磷酸缓冲盐溶液为流动相梯度洗脱;柱温:30℃;流速:0.8mL/min;检测波长:210nm;进样量:10μL。测定10批不同来源可可粉图谱,并运用相似度分析、系统聚类分析对可可粉进行分类研究。结果:建立了精密度、稳定性和重复性均良好的HPLC指纹图谱,确立了5个共有峰,指认了其中3个色谱峰,并建立了可可粉指纹图谱共有模式,测得各批次样品指纹图谱相似度均在0.90以上,系统聚类分析将10批可可粉分为3类。结论:该方法简便易行、准确、重现性好,可以作为可可粉质量评价的重要依据。     

不同产地辣木叶HPLC指纹图谱研究

目的高效液相色谱法(HPLC)建立辣木叶指纹图谱,为辣木叶的质量控制和评价提供参考。方法选用Diamonsil C_(18)色谱柱(4.6 mm×250 mm,5μm),检测波长230 nm,流动相为甲醇-0.05%磷酸水溶液梯度洗脱),流速1.0 ml/min,柱温为35℃,进样量10μl;以没食子酸为参照峰,在相同的色谱条件下测定9批不同产地的辣木叶药材,用软件"中药色谱指纹图谱相似度评价系统(2012版)"对9批辣木叶进行相关分析。结果建立了辣木叶的HPLC指纹图谱,9批辣木叶的相似度在0.63～0.87之间,指定了15个共有峰,2个已确认成分,分别为没食子酸和异槲皮素;以对照图谱为对照,各共有峰的相对保留时间RSD均小于2.0%,各共有峰的相对峰面积差别显著,表明这9批辣木叶原材化学成分种类差别较小,各成分含量差别较大。结论此法具有良好的精密度、重复性、稳定性,可为辣木叶的质量评价与控制提供科学依据。     

基于离子液体辅助提取的羊肚菌HPLC指纹图谱分析

目的:建立一种绿色环保的羊肚菌高效液相指纹图谱分析方法。方法:采用离子液体-水溶液绿色溶剂提取样品,通过单因素考察离子液体种类、离子液体碳链长度、离子液体质量分数、提取时间、料液比对提取量的影响,确立了最终提取条件为40%[OMIM]PF₆水溶液(料液比1:10)湿法研磨样品10 min;同时使用绿色高效液相色谱法对羊肚菌进行分析检测:Agilent ZORBAX SB-AQ C₁₈色谱柱(4.6 mm×150 mm,5 μm),0.2%乙酸-乙醇作为绿色流动相体系进行梯度洗脱,流速1.0 mL/min,柱温40℃,检测波长260 nm。采用"中药色谱指纹图谱相似度评价系统(2012版)"对20批试验样品(14批六妹羊肚菌、6批其他食药用菌)进行相似度评价,采用SPSS 22.0软件对所有样品进行了聚类分析和主成分分析。结果:建立了羊肚菌的HPLC指纹图谱,标定10个共有峰,鉴定了5个核苷类成分(尿嘧啶、胞苷、尿苷、鸟苷、腺苷),20批试验样品中14批羊肚菌样品相似度均大于0.9,另外6批常见食药用菌相似度在0.25~0.65之间;聚类和主成分分析结果显示羊肚菌样品与其他食药用菌在本实验条件下化学成分存在显著差异,可有效鉴别羊肚菌和常见食药用菌。结论:本试验建立了简便、绿色、快速的羊肚菌HPLC指纹图谱分析方法,有助于提升羊肚菌的综合质量评价水平。     

白芷HPLC指纹图谱的研究

目的建立白芷的高效液相色谱(HPLC)指纹图谱。方法采用HPLC,色谱柱:Agilent C18(250mm×4.6 mm,5μm),梯度洗脱,流动相A为0.01%三氟乙酸水溶液,流动相B为甲醇,流速1.0 ml/min,柱温30℃,检测波长300 nm,建立了21批白芷的HPLC指纹图谱。结果与结论本研究建立的指纹图谱可较好地反映白芷的质量,可为其质量控制提供参考。     

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