高效液相色谱法测定食品中大豆异黄酮含量

建立食品中大豆异黄酮含量测定的高效液相色谱法。样品以甲醇 :水 (80 :2 0 )于 6 5°C水浴中振荡提取 ,氢氧化钠皂化 ,冰醋酸酸化 ,离心过滤后用液相色谱分析。色谱柱为HypsilBDSC18(5 μ ,4 .6× 2 5 0mm )柱 ,梯度洗脱 ,流动相A为水 :甲醇 :冰乙酸 (88:10 :2 ) ,流动相B为 2 %冰乙酸的甲醇溶液 ,流速 0 .4mL/min ,紫外检测波长 2 6 0nm ,柱温 32°C。各组分 (大豆甙 ,黄豆甙 ,染料木甙及其相应甙元大豆黄素 ,黄豆黄素 ,染料木素 )的峰面积与其相应浓度呈良好的线性相关 ,r >0 .9999。以豆奶粉和奶粉为基质 ,六种大豆异黄酮加标回收试验的平均回收率分别为 85 .1% - 138.1%和 6 7.8% - 95 .9% ,RSD分别在 5 .5 % - 17.8%和 1.8% - 9.5 %之间。采用建立的方法测定了黄豆、豆芽、蚕豆、腐竹、豆腐、豆浆、豆奶粉、奶粉等样品中大豆异黄酮含量 ,测定结果令人满意。     

高效液相色谱法测定大豆中异黄酮的含量

用高效液相色谱法测定了大豆中六种异黄酮成分,同时比较了不同浓度乙醇制备样品对含量测定的影响。结果显示大豆中极性异黄酮含量高,低极性异黄酮甙元含量低。测定大豆中异黄酮含量的乙醇浓度最好控制在60％-80％。色谱柱采用日本岛津公司的Shim-Pack CLC ODS柱(150×6．0mmID5μm),流动相为MeOHHACH2O（303.566.5),流速为0-8．5min时1．0ml／min,5．8-47min时1．5ml／min,柱温为50℃,检测波长为254。     

高效液相色谱-质谱法在大豆异黄酮测定中的应用

应用高效液相色谱 -质谱法检测东北地区生产的 6个品种的大豆及其胚芽中异黄酮的含量 ,检测到 6种类型的异黄酮。 6个品种的大豆全豆异黄酮含量为 0 .15 1%～ 0 .388% ,胚芽异黄酮含量为 1.4 5 6 %～ 3.0 3% ,所测大豆因品种差异而致异黄酮含量相差 1倍以上。在天然状态下 ,异黄酮主要以丙二酰形式存在 ,所测结果在 80 %以上。在全大豆中 ,异黄酮以染料木素糖苷 (genistin)及其衍生物为主 ,占异黄酮总含量的 5 6 %～ 6 8% ,在胚芽中 ,异黄酮以大豆黄素糖苷 (daidzin)和黄豆黄素糖苷 (glycitin)及其衍生物为主 ,分别占异黄酮总含量的 4 5 %～ 5 1%和2 1%～ 2 8%。     

高效液相色谱测定水解大豆中异黄酮方法研究

该研究建立大豆提取物中大豆异黄酮高效液相色谱测定方法,通过正交实验确立糖苷型大豆异黄酮转化为游离型大豆异黄酮最佳酸水解工艺条件:盐酸浓度为2．0 mol/L,水解温度为80℃, 水解时间为1．5 h;采用ZorbaX 80A Extend-C18 4．6×150 mm 4 μm色谱柱,MeOH-1．8％冰乙酸水溶液(35:65,V／V)为流动相,MeOH 35％-50％梯度洗脱,流速1．0 ml/min,检测波长为260nm等色谱条件下测定甙元含量,并通过换算因子计算大豆异黄酮含量。     

高效液相色谱法检测大豆异黄酮含量

采用超声波法提取豆粕中大豆异黄酮,通过高效液相色谱法测定其含量.确定色谱条件为:色谱柱Waters RP18 (5μm,3.9×150mm),流动相甲醇∶水∶磷酸=52∶48∶0.2,柱温30℃,流速0.7mL/min,检测波长260nm.该测定方法变异系数(RSD)小于3%.采用高效液相色谱法测定异黄酮含量,具有灵敏、准确、重现性好等优点.超声提取法具有缩短提取时间和简化工艺等优点.     

不同发酵豆粕中6种大豆异黄酮成分含量的比较研究

目的：比较不同菌种发酵豆粕中6 种大豆异黄酮成分的含量。方法：采用高效液相法测定不同菌种发酵豆粕中6 种大豆异黄酮成分的含量,所用的菌种为酵母菌、乳酸菌、少孢根霉菌和芽孢杆菌。以Alltima C18(150mm × 4.6mm,5μm)为色谱柱,用甲醇- 水为流动相进行梯度洗脱,流速为1mL/min,柱温为35℃,检测波 长为254nm。结果：6 种大豆异黄酮成分在各自线性范围内,峰面积与进样量呈良好的线性关系(r ≥ 0.9998);回收率为97%～102%(RSD ＜ 3%)。结论：以同批豆粕为原料,采用不同菌种制成的发酵豆粕中,大豆异黄酮成分的含量存在明显的变化。     

一测多评法测定保健食品中6种大豆异黄酮类成分

建立一测多评方法实现只用一个对照品同时测定保健食品中6种大豆异黄酮类成分的含量,以解决含大豆异黄酮类成分保健食品对照品昂贵不易获得的难题。样品经甲醇超声波辅助提取后,采用Waters Xbridge C_(18)(150 mm×4.6 mm,3.5μm)色谱柱,以2%乙酸和乙腈为流动相进行梯度洗脱,260 nm并辅以DAD紫外检测器检测。通过5种待测成分与染料木苷的相对保留时间、DAD光谱及参照图谱完成待测成分确认;通过研究确立其他5种待测成分与染料木苷的校正系数进行含量测定,一定线性范围内得到不同浓度对照品在不同仪器、人员及色谱柱上的校正系数RSD为0.4%~3.5%;3批不同来源保健食品中6种大豆异黄酮类成分测定结果与常规外标法所得结果结果偏差为0.3%~5.8%;所建立的一测多评方法可用以大豆异黄酮及其相关保健食品的定量分析及质量评价方法。     

反相高效液相色谱法同时测定保健品原料中的4种大豆异黄酮

建立了同时测定保健品原料中4种大豆异黄酮含量的高效液相色谱分析方法。采用ODS-C18色谱柱(250mm×4·6mm;5μm),流动相A为甲醇∶水=1∶1,流动相B为甲醇∶乙酸乙酯=1∶1,采用梯度洗脱,用100%流动相A洗脱5min后,在5~20min内使流动相A由100%下降至10%,并在10%保持5min;二极管阵列检测器,检测波长为270nm;流速0·8mL/min。采用外标法定量,大豆苷(Daidzin,D),染料木苷(Genistin,G),大豆苷元(Daidzein,De),染料木素(Genistein4,7-dimethylether,Ge)4种组分线性关系良好,相关系数0·9920~0·9999,检测限为0·15~0·35μg/mL。加标回收率分别为107%、103%、101%、104%,RSD分别为3·3%、2·4%、3·8%、4·5%。该方法简便、快速、准确,是多种大豆异黄酮定量测定的可靠方法之一。     

高效液相色谱法测定大豆胚轴中DDMP皂甙αg和βg

为检测大豆中的αg和βg含量 ,应用高效液相色谱 -差示折射法 (HPLC -dRI)测定大豆皂甙样品中DDMP皂甙αg和 βg含量 ,色谱柱为ODS -AM - 30 3柱 (YMC ,4 6mm× 2 5 0mm ,5 μm) ,流动相为含 0 1%三氟乙酸的乙腈 水 (4 0 6 0 )。DDMP皂甙αg和 βg分别在 1 38～ 6 88μg和 1 6 2～ 8 12 μg范围内线性关系良好 ,平均回收率为 93 4 %和 94 2 % ,RSD为 4 0 7%和 4 2 8%。方法准确度高 ,重现性好 ,适用于大豆皂甙样品中DDMP皂甙以及其它大豆皂甙的含量测定。     

大豆乳清水一级浮渣粉中大豆异黄酮的 提取工艺研究

建立了一种针对大豆乳清水一级浮渣粉(SP)中大豆异黄酮的提取、分离和纯化方法。结果表明:以60%乙醇为提取溶剂,在料液比1∶5、提取温度60～70℃下采用胶体磨提取2次,每次0. 75 h,每100 g SP可提取干物质20 g,大豆异黄酮含量为2. 08%。该20 g提取物加20 g Ca3(PO4)2、8 g Ca(HCO3)2和400 m L 95%乙醇沸腾回流1 h,过滤浓缩后可得3. 05 g膏状物,大豆异黄酮含量为13. 6%,除杂分离效果好。用大孔树脂ADS-21对膏状物吸附洗脱,浓缩得大豆异黄酮产品,含量为83. 5%,为洗脱前膏状物的6. 14倍。     

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