色谱法监测β-D-吡喃葡萄糖苷的合成

用改进的Koenigs-knorr法立体选择性地合成了2,3,4,6-四乙酰基-香叶基-1-O-β-D-吡喃葡萄糖苷(GLY-A)和香叶基-β-D-吡喃葡萄糖苷(GLY-B)两种键合态香料前体.采用薄层色谱法(TLC)监控反应条件;硅胶柱层析色谱法(SGCC)分离并纯化产物;反向液相色谱法(RP-HPLC)测定样品纯度...     

香料前体香叶醇-β-D-葡萄糖苷的合成、纯化与表征

为了开发热稳定型香原料,采用改进的Koenigs-knorr法立体选择性地合成了香叶醇-β-D-葡萄糖苷(Geranyl-β-D-Glycoside,GGLY);以反相液相色谱法(ReversePhaseHPLC,RP-HPLC)检测并确定最优反应条件;硅胶柱层析梯度洗脱分离制备样品,产物纯度达99.2%;然后综合IR、LC/MS/MS、1HNMR、13CNMR进行结构鉴定,确证制备的产物为香叶醇糖苷。     

硅胶柱层析纯化花生根中白藜芦醇工艺研究

通过薄层层析和硅胶柱层析以及HPLC纯度检测实验研究发现,以氯仿与甲醇之比为9∶1的常压硅胶柱层析的洗脱溶剂,硅胶吸附剂与样品量之比50∶1,经硅胶柱层析纯化可以使白藜芦醇粗品的纯度从39%提高到99%以上。     

柱层析分离提纯麝香草酚的研究

采用薄层层析和硅胶柱层析分离纯化了麝香草酚,并用气相色谱法测定纯化后的样品中麝香草酚的含量.薄层层析分离麝香草酚的适宜条件:点样量约2μL,在环己烷/无水乙醚(4/1,v/v)中展开,然后碘缸中显色15min,得到清晰的黄色斑点.硅胶柱层析分离烷基化产物中的麝香草酚的适宜条件:0.3mL的麝香草酚粗成品上10mm×400mm硅胶(60～100目)层析柱,流动相为环己烷/无水乙醚(4/1,v/v),流速为0.4mL/min,分离出的麝香草酚纯度为99%.     

利用硅胶柱层析分离纯化平贝总碱的研究

目的：对东北特产平贝母的生物碱进行分离纯化研究。方法：用硅胶柱层析法对平贝总碱进行分离纯化,固定相为薄层层析硅胶G,流动相为乙酸乙酯- 甲醇- 氨水(17:2:1)。用HPLC-ELSD 法对分离出的贝母素甲和贝母素乙的纯度进行测定。结果：分离出贝母素甲和贝母素乙,贝母素甲纯度为93.19%、贝母素乙纯度为92.09%。结论：采用的硅胶柱层析分离纯化可得到纯度较高的分离组分。     

柱层析分离提纯麝香草酚的研究

采用薄层层析和硅胶柱层析分离纯化了麝香草酚,并用气相色谱法测定纯化后的样品中麝香草酚的含量。薄层层析分离麝香草酚的适宜条件:点样量约2μL,在环己烷/无水乙醚(4/1,v/v)中展开,然后碘缸中显色15min,得到清晰的黄色斑点。硅胶柱层析分离烷基化产物中的麝香草酚的适宜条件:0·3mL的麝香草酚粗成品上10mm×400mm硅胶(60~100目)层析柱,流动相为环己烷/无水乙醚(4/1,v/v),流速为0·4mL/min,分离出的麝香草酚纯度为99%。      

β-D-吡喃葡萄糖苷类香料前体的合成及表征

为了开发热稳定型香原料,由改进的银盐法合成了香叶基-β-D-吡喃葡萄糖苷、顺-3-己烯基-β-D-吡喃葡萄糖苷、薄荷基-β-D-吡喃葡萄糖苷,并与相转移法、路易斯酸催化法进行了比较,以香叶基-β-D-吡喃葡萄糖苷的合成为例,制备高效催化剂,探讨了催化剂、温度、时间等对糖苷化反应产率的影响,优化后收率为51%。以TLC、HPLC监控反应进程,采用IR、LC/MS、1H-NMR、13CNMR等进行了结构鉴定,对醇类香料的糖苷化反应进行了研究。     

叶黄素的分离纯化及其清除羟自由基活性

运用KOH-甲醇溶液皂化法将叶黄素酯转化为游离叶黄素,进一步采用硅胶柱层析进行分离纯化,并对不同纯度产品中叶黄素的含量进行HPLC法测定;以没食子酸丙酯为参照,采用流动注射化学发光法测定不同纯度叶黄素产品清除.OH的效果。结果表明:叶黄素浸膏通过皂化,游离叶黄素的含量由1.35%提高到30.25%,进一步柱层析处理得到80.32%的叶黄素产品;不同纯度叶黄素产品均具有较强的清除.OH活性,且其抗氧化活性与叶黄素的含量正相关。     

多烯酸磷脂的合成制备方法及表征

以藻油甘油酯为起始原料,先通过皂化获得多烯酸原料,再经过两步方法制备多烯酸磷脂化合物,两步的总收率是31.0%。反应粗产物采用硅胶柱层析进行分离纯化,对制备的多烯酸磷脂主要成分进行了红外光谱以及高效液相色谱的初步鉴定,证实所合成的产物与预期的目标化合物多烯酸磷脂结构一致,产物中多烯酸磷脂的总含量是97.04%。     

鸢尾异黄酮的分离纯化及抑菌活性研究

目的研究鸢尾中异黄酮的分离纯化工艺及抑菌活性。方法醇提法提取野生鸢尾叶中的异黄酮,采用硅胶柱层析结合半制备高效液相色谱法对鸢尾异黄酮进行分离纯化和含量测定,以乙酸乙酯:丙酮:无水乙醇=5:1:0.5(v/v/v)为柱层析洗脱剂对鸢尾异黄酮进行分离纯化;以甲醇:0.4%磷酸=90:10(v/v)为高效液相色谱(HPLC)流动相,柱温30℃,检测波长265 nm,进样量20μl,流速1 ml/min测定含量和纯度。采用牛津杯法检测鸢尾异黄酮对枯草芽孢杆菌和大肠杆菌的抑菌活性。结果与结论分离纯化后的鸢尾异黄酮纯度为91.29%,提取率为1.62%。抑菌试验结果表明,鸢尾异黄酮对大肠杆菌和枯草芽孢杆菌均有显著的抑制作用,最小抑菌浓度分别为1.25 mg/ml和0.625 mg/ml,表明鸢尾异黄酮有显著抑菌活性。     

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