柱层析法分离大豆磷脂

通过实验探讨了使用低压制备色谱柱在等度洗脱方式下分离大豆磷脂中的磷脂酰肌醇(PI)、磷脂酰乙醇胺(PE)、磷脂酰胆碱(PC)等成分.结果表明,在使用100cm×26 mm规格的色谱柱、氯仿-甲醇(2∶1)作为流动相、流速控制在3.0 mL/min,负载量为0.25 g/150 g硅胶(100～200目)的条件下可以分离得到PI纯度在90%以上、PE纯度在80%以上、PC纯度在95%以上的各种产品.     

高效液相色谱法测定大豆磷脂类保健食品中的磷脂酰胆碱、磷脂酰乙醇胺、磷脂酰肌醇

目的建立高效液相色谱检测法测定大豆磷脂类保健食品中磷脂酰胆碱(phosphatidylcholines,PC)、磷脂酰乙醇胺(phosphatidylethanolamine, PE)、磷脂酰肌醇(phosphatidylinositol, PI)含量的方法。方法大豆磷脂类保健食品试样经正己烷:异丙醇(1:1, V:V)提取,经氨基柱(250 mm×4.6 mm, 5μm)分离,以流动相为无水乙醇-乙腈-水(50:40:10, V:V:V)为流动相等度洗脱,流速为0.4 mL/min,检测波长为205 nm,外标法定量。结果磷脂酰胆碱、磷脂酰乙醇胺、磷脂酰肌醇在一定浓度范围内线性关系良好,相关系数大于0.999;检出限分别为1.3、5.0、1.0 mg/g,加标回收率分别为95.5%、99.5%、94.9%,精密度均为0.3%。结论本方法准确度高、重复性好,适用于保健食品中磷酯类物质含量的测定。     

高纯度磷脂酰肌醇的提取工艺研究

以低磷脂酰胆碱(PC)含量大豆粉末磷脂为原料,建立以碱性乙醇为溶剂结合冷冻纯化制备高纯度磷脂酰肌醇(PI)的方法。在单因素实验的基础上利用响应面优化实验确定PI的最佳提取条件为:冷冻时间17 h,冷冻温度-20℃,提取温度40℃,料液比1∶27,98%乙醇与25%氨水体积比100∶4,提取时间40 min,提取次数3次。在最佳条件下,产物PI含量为82.62%,得率为14.29%。     

高效液相色谱法测定磷脂软胶囊中磷脂酰胆碱、磷脂酰肌醇、磷脂酰乙醇胺的含量

目的建立高效液相色谱法同时检测磷脂软胶囊中磷脂酰胆碱(phosphatidyl cholines, PC),磷脂酰乙醇胺(phosphatidyl ethanolamine, PE),磷脂酰肌醇(phosphatidylinositol, PI)3种组分的含量。方法样品用甲醇超声提取后,经Bridge?HILIC色谱柱(4.6 mm×150 mm, 5μm)分离,以0.9 mmol/L甲酸铵溶液-乙腈为流动相进行梯度洗脱,流速为1.0 mL/min;柱温30℃;检测波长为205 nm,外标法定量。结果磷脂酰胆碱,磷脂酰乙醇胺,磷脂酰肌醇在浓度0.025～0.250mg/mL范围内线性关系良好,相关系数均大于0.99,检出限分为0.300～1.386 mg/g,定量限为1.002～4.624 mg/g,加标回收率分别为90%～105%,相对标准偏差为1.0%～4.0%。结论该方法高效,便捷,准确度高,适用于磷脂软胶囊中3种磷脂成分的同时检测。     

大豆磷脂酰肌醇的提取工艺研究

为探究溶剂分提法提取较高纯度的磷脂酰肌醇(PI),以提取PC后的大豆粉末磷脂为原料,在单因素实验的基础上,进行响应面优化实验,以PI含量为指标,确定了以碱性乙醇为溶剂提取磷脂酰肌醇的最佳工艺条件:温度为40℃、液料比为20∶1、碱性乙醇氨水浓度为2.60mL 25%氨水/100mL无水乙醇、时间50min、提取两次。在此条件下,磷脂酰肌醇的纯度为58.86%,得率为70.14%。      

大豆磷脂酰肌醇的提取工艺研究

为探究溶剂分提法提取较高纯度的磷脂酰肌醇(PI),以提取PC后的大豆粉末磷脂为原料,在单因素实验的基础上,进行响应面优化实验,以PI含量为指标,确定了以碱性乙醇为溶剂提取磷脂酰肌醇的最佳工艺条件:温度为40℃、液料比为20∶1、碱性乙醇氨水浓度为2.60mL 25%氨水/100mL无水乙醇、时间50min、提取两次。在此条件下,磷脂酰肌醇的纯度为58.86%,得率为70.14%。     

HPLC法测定大豆磷脂及其保健品中PC、PI、PE

建立了高效液相色谱紫外检测器测定大豆保健品中磷脂酰胆碱、磷脂酰乙醇胺、磷脂酰肌醇的测定方法。采用NH2色谱柱(3.0 mm×150 mm×5μm),流动相为乙醇∶乙腈∶水=50∶40∶10(体积比),流速0.4 m L/min下,紫外检测器波长为206 nm处进行测定。样品经正己烷∶异丙醇=1∶1(体积比)混合液溶解并使用流动相稀释后直接进样分析。在线性范围内相关性良好,相关系数R2≥0.999,各添加水平回收率为91.12%~105.61%,RSD为4.85%,日内和日间精密度均小于4%,磷脂酰胆碱、磷脂酰乙醇胺、磷脂酰肌醇定量限分别为1.5 mg/L、1.2 mg/L和0.9 mg/L。本方操作简单、准确、成本低,适合于分析大豆磷脂及其保健品中三种主要磷脂的含量。     

大豆磷脂酰肌醇分离方法综述

该文阐述大豆磷脂中磷脂酰肌醇高效液相色谱法(HPLC)、柱层析法、溶剂法、酶法等分离方法,并介绍通过一些化学反应方法制备高纯度磷脂酰肌醇及其应用。     

大豆磷脂中PC、PE、PI测定方法的研究

为准确快速地对大豆磷脂中的主要成分磷脂酰胆碱（PC）、磷脂酰乙醇胺（PE）、磷脂酰肌醇（PI）进行定量分析,对分析柱、流动相、检测波长进行了选择与优化,最终建立了以Lichrosorb Si-60为分析柱,205nm波长下,以V（正己烷）：V（异丙醇）：V（1％乙酸）=8：8：1为流动相的高效液相色谱测定法。     

油菜、菊花和荷花蜂花粉中磷脂的色谱分析

以油菜、菊花、荷花蜂花粉为原料,采用薄层层析法(thin layer chromatography,TLC)法分离纯化蜂花粉中的磷脂,并用高效液相色谱法(high-performance liquid chromatography,HPLC)法测定磷脂酰肌醇(PI)、磷脂酰丝氨酸(PS)、脑磷脂(PE)、卵磷脂(PC)及溶血卵磷脂(LPC)的含量。结果表明：3种蜂花粉中总磷脂含量为1.19～3.98g/100g,3种花粉存在极显著差异(P＜0.01);PC是蜂花粉磷脂的主要成分,占总磷脂的34.30%～59.69%;在油菜蜂花粉中检测到PI、PS、PE、PC、LPC,菊花蜂花粉未测出PI,荷花蜂花粉未测出PI、LPC。结论：油菜蜂花粉中磷脂种类最丰富、总含量最高,是花粉磷脂的较好来源。     

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