药食两用小蓟中细胞毒活性成分解析

本课题组前期研究发现,小蓟乙醇提取石油醚萃取部位具有较好的抑制多种人肿瘤细胞毒活性的作用,现对其中强活性亚组分的化学成分进行研究,挖掘发挥细胞毒活性的功能因子。在体外抑制细胞毒活性指导下,应用多种色谱技术进行分离纯化,采用波谱学方法进行结构鉴定,并结合文献数据对照确定化合物结构。从石油醚的1个活性组分中共分离鉴定了5个甾体化合物,分别为:3β-羟基豆甾-5-烯-7-酮、豆甾-22-烯-3β,5α,6β-三醇、6β-羟基-豆甾-4-烯-3-酮、6β-羟基-豆甾-4,22-二烯-3-酮和6β-羟基-芸苔甾-4-烯-3-酮。5个化合物均为首次从蓟属植物中发现;除化合物α-豆甾-22-烯-3β,5α,6β-三醇外,其余4个化合物对不同人肿瘤细胞均具有一定的抑制活性。     

小蓟中氧化蒲公英赛酮和醇的分离鉴定和细胞毒活性测试

研究小蓟乙醇提取物中显示细胞毒活性的石油醚的化学成分,并对分离得到的化合物进行体外细胞毒活性的筛选。应用各种硅胶和凝胶色谱技术分离纯化,用MS和NMR等波谱学方法,结合文献对照确定化合物结构。从小蓟乙醇提取物的石油醚萃取部位分离得到3个氧化蒲公英赛烷型三萜类化合物,分别鉴定为11α,12α-氧化蒲公英赛酮、11α,12α-氧化蒲公英赛醇和11α,12α-氧化蒲公英赛醇棕榈酸酯。3个化合物均为首次从蓟属植物中发现,它们在人结肠癌细胞、肝癌细胞、胃癌细胞、肺癌细胞和卵巢癌细胞的体外细胞毒活性测试中均显示一定的抑制活性。     

紫红曲中的麦角甾类化合物

研究紫红曲乙醇提取物中显示细胞毒活性的醋酸乙酯萃取部位的化学成分。利用正反相硅胶、凝胶Sephadex LH-20、结合闪式(Flash)柱色谱和制备高效液相色谱等多种色谱手段进行分离纯化,借助核磁和质谱等波谱学方法进行结构鉴定。从紫红曲乙醇提取物的醋酸乙酯萃取部位中分离鉴定了5个麦角甾类化合物,分别为:麦角甾-7,22-二烯-3β,5α,6β-三醇(1),(22E,24R)-麦角甾-7,22-二烯-6-酮-3β,5α,9α-三醇(2),(22E,24R)-23-甲基麦角甾-7,22-二烯-3β,5α,6β-三醇(3),(22E,24R)-23-甲基麦角甾-7,22-二烯-6-酮-3β,5α,9α-三醇(4),麦角甾-4,6,8(14),22-四烯-3-酮(5)。上述5个化合物均为首次从紫红曲中分离得到。除化合物1外,其余化合物均为首次从红曲菌属中发现。在体外MTT法的细胞毒活性测试中,所筛选的化合物在10×10-6mol/L浓度下均未显示细胞毒的活性。     

毛蚶抗菌活性筛选及低极性组分GCMS分析

目的:研究毛蚶的抗菌活性部位及有效成分。方法:毛蚶软组织经乙醇提取后,采用液液萃取法将提取物分为石油醚相、乙酸乙酯相、正丁醇相和水相4个不同的极性部位;采用抑菌圈法和最小杀菌浓度测定法,对毛蚶乙醇提取物和各极性部位进行了抗菌活性测定,并用正相硅胶柱对抗菌活性较好的石油醚相进行了分离纯化,得到甾体组分;采用GC-MS技术对石油醚相和甾体组分进行了化学成分分析。结果:毛蚶石油醚相的抑菌效果最好;从毛蚶石油醚相中鉴定出了30个化合物,主要为脂肪类和甾醇类化合物;从甾体组分中鉴定出8个化合物,其中7个为首次从毛蚶中分离鉴定。结论:毛蚶的石油醚相具有明显的抗菌活性,石油醚相以甾醇类化合物为主。     

野生白木香叶乙酸乙酯提取物化学成分的分离鉴定

为探究沉香茶系列保健食品的主要原料白木香(Aquilaria sinensis)叶片药理活性的物质基础,本研究通过含70%丙酮的水溶液渗漉提取、石油醚和乙酸乙酯多次萃取后,运用硅胶柱色谱、Sephadex LH-20凝胶柱色谱和制备高效液相色谱等技术从野生白木香叶片乙酸乙酯萃取部位中分离纯化得到7个化合物,根据MS、NMR等波谱数据分别鉴定其中6个化合物为麦角甾醇(1)、槲皮素-3-O-β-D-吡喃半乳糖苷(2)、豆甾醇(3)、5,4'-二羟基-7-甲氧基二氢黄酮(4)、谷甾醇(5)、槲皮素-3-O-β-D-吡喃葡萄糖苷(6)。6个化合物按照结构可分为甾醇及其衍生物类(3个),黄酮苷类(2个)和二氢黄酮类(1个)。其中化合物1-2为首次在瑞香科植物中分离得到,化合物4是在瑞香科沉香属植物中首次分离得到的二氢黄酮类化合物,并首次报道了该化合物的2D NMR数据及归属。     

石花菜醇提物成分分析

目的：研究石花菜的成分,为其功能食品的研发提供基础数据。方法：采用薄层色谱、液-质谱联用方法分析石花菜醇提物的化学成分的丰富度。通过硅胶柱、高效液相等色谱方法对其进行分离纯化,并用气-质谱联用、核磁结合文献确证化合物结构;并对部分化合物抗氧化活性进行测定。结果：薄层色谱、液-质谱联用分析表明石花菜醇提物中含有丰富的次级代谢产物,且很可能是甾醇类成分。采用气-质谱联用方法从中鉴定到29个化合物（5个为甾醇类化合物）,其中棕榈酸（46.76%）、棕榈酸乙酯（13.82%）、胆甾醇（7.20%）、胆甾-4,6-二烯（4.99%）为含量最高的4个化合物。经色谱分离、核磁鉴定出9个单体化合物,分别为胆甾醇（1）、1,2-二醇植烯（2）、帕格甾醇C(3)、6-羟基-胆甾-4-烯-3-酮（4）、胆甾-5-烯-7-酮（5）、胆甾-5-烯-3β,7α二醇（6）、胆甾-5-烯-3β,7β二醇（7）、胆甾-4-烯-6-酮（8）、3-羟乙基-2-甲基-马来酰亚胺（9）。其中,化合物7清除DPPH自由基和ABTS自由基能力最好,其IC50值分别为180μg/mL和12.2μg/mL。结论：首次系统研究了石花菜醇...     

加拿大一枝黄花化学成分的研究

目的分离和鉴定加拿大一枝黄花Solidago canadensis的化学成分。方法用色谱技术分离、纯化,通过理化常数和波谱分析鉴定化合物结构。结果从乙醇提取物中分离鉴定了7个化合物,分别为2-羟基-6-甲氧基苯甲酸(Ⅰ)、3-甲酰吲哚(Ⅱ)、3β,4α-二羟基-6β-当归酰-13Z-烯-15,16-克罗烷内酯(Ⅲ)、3β,4α-二羟基-6β-巴豆酰-13Z-烯-15,16-克罗烷内酯(Ⅳ)、α-菠菜甾醇(Ⅴ)、山柰酚(Ⅵ)和槲皮素(Ⅶ)。结论化合物Ⅱ为首次从该属植物中分离得到,化合物Ⅰ、Ⅲ～Ⅴ均为首次从该种植物中分离得到。     

露兜簕果萜类化合物的分离和鉴定

将露兜口果的乙醇提取物依次用有机溶剂萃取,浓缩得浸膏,再对石油醚部分浸膏采用薄层色谱、硅胶柱层析、重结晶等方法进行分离纯化,得到物质F5-1,利用波谱技术(ESI-MS、1H-NMR、13C-NMR、IR)并结合化合物的理化性质鉴定了该化合物的结构,为五环三萜类化合物,齐墩果酸(3β-hydroxy-olea-12-en-28-oic acid)是首次从该植物中分离得到.     

加拿大一枝黄花化学成分的研究

目的 分离和鉴定加拿大一枝黄花Solidago canadensis的化学成分.方法 用色谱技术分离、纯化,通过理化常数和波谱分析鉴定化合物结构.结果 从乙醇提取物中分离鉴定了7个化合物,分别为2-羟基-6-甲氧基苯甲酸(Ⅰ).3-甲酰吲哚(Ⅱ)、3β,4α-二羟基-6β-当归酰-13Z-烯-15,16-克罗烷内酯(Ⅲ)、3β,4α-二羟基-6β-巴豆酰-13Z-烯-15,16-克罗烷内酯(Ⅳ),α-菠菜甾醇(Ⅴ)、山柰酚(Ⅵ)和槲皮素(Ⅶ).结论 化合物Ⅱ为首次从该属植物中分离得到,化合物Ⅰ、Ⅲ-Ⅴ均为首次从该种植物中分离得到.     

一株黄芪内生真菌甾醇类代谢产物的分离和鉴定

目的:研究分离自夏季黄芪根部的内生真菌AR-17-S03的次级代谢产物。方法:采用组织学的方法从恒山黄芪中分离内生真菌,真菌的鉴定采用形态学法结合分子生物学法,采用硅胶柱色谱法、薄层层析制备色谱(pTLC)、Sephadex LH-20凝胶柱色谱法和半制备HPLC色谱法分离内生真菌代谢产物,采用质谱法、核磁共振法结合物化性质鉴定分离得到的9个化合物。结果:经形态学结合分子生物学鉴定该菌株黑曲霉,为9个甾醇类化合物鉴定为麦角甾醇、过氧化麦角甾醇、胆固醇、啤酒甾醇、23-甲基麦角甾-7,22-二烯-3β,5α,9α-三醇、5α,8α-表二氧麦角甾-6,9(11),22-三烯-3β-醇、5α,8α-表二氧-23-甲基麦角甾-6,22-二烯-3β-醇、麦角甾-4,6,8(14),22-四烯-3-酮、3β,5α-二羟基麦角甾-7,22-二烯-6-酮。结论:其中,23-甲基麦角甾-7,22-二烯-3β,5α,9α-三醇、5α,8α-表二氧-23-甲基麦角甾-6,22-二烯-3β-醇、麦角甾-4,6,8(14),22-四烯-3-酮是首次从黄芪内生真菌中分离得到。     

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