利用超高压技术提取补骨脂中补骨脂素和异补骨脂素

补骨脂是我国用于生产各种保健品的传统原料之一,其主要活性成分为补骨脂素和异补骨脂素。本实验通过回流提取法和超高压提取法提取补骨脂中补骨脂素和异补骨脂素的对比实验,证明超高压提取法优于回流提取法。通过均匀试验设计优化超高压提取补骨脂素和异补骨脂素的提取工艺,得到补骨脂素最优提取工艺条件为：压力100MPa,乙醇体积分数 53%,液固比90:1(mL/g),提取时间3min;异补骨脂素的最优提取工艺条件为：压力100MPa,乙醇体积分数 55%,液固比90:1(mL/g),提取时间3min。实验证明应用超高压提取法可以实现补骨脂素和异补骨脂素的常温、快速提取,为其在保健品和功能性食品中的应用提供高效的生产方法。     

无花果叶提取物对平菇保鲜效果的研究

为提高无花果叶中有效活性成分——"补骨脂素"的提取率,利用超声波辅助提取补骨脂素,并用正交法优化研究乙醇浓度、液料比、超声温度、提取时间4个因素对无花果叶中补骨脂素提取率的影响,最佳提取参数为:乙醇浓度25%、液料比20∶1m L/g、提取温度40℃、提取时间为30min。将补骨脂素提取液应用于平菇的保鲜,以25%乙醇为对照,结果表明:经补骨脂素提取液处理的实验组平菇呼吸强度、细胞膜渗透率、丙二醛含量低于对照组,可溶性蛋白质含量、可溶性固形物含量均高于对照组。表明无花果叶中补骨脂素提取液能够较好地提高平菇的贮藏品质。     

补骨脂炮制方法优选的研究

目的优选补骨脂的最佳炮制方法。方法以补骨脂素、异补骨脂素和补骨脂酚为测定指标,用高效液相色谱法(HPLC)测定比较补骨脂生品和各种炮制品色谱峰面积及含量变化,筛选最佳炮制方法。结果补骨脂通过炮制后其药用效果有效增强,毒性成分明显减弱,15种炮制方法中酒焙法最优。结论可选用酒制补骨脂作为其临床应用的炮制方法。     

基于高分辨质谱库和特征组分诊断比值法鉴别配制酒和代用茶中非法添加补骨脂

目的:建立一种基于高分辨质谱库筛查和特征比值法确证配制酒和代用茶中非法添加补骨脂的高效液相色谱检测方法。方法:采用高效液相色谱—四极杆—飞行时间质谱仪建立补骨脂中药材特征组分筛查库,结合液相特征组分诊断比值法,对不同采摘时间和产地的共20批次补骨脂模拟的补骨脂配制酒、代用茶样品进行特征组分分析,从13种特征成分中选出2组受产地、采摘时间、加工工艺等影响较小,不同基质组间无显著性差异的特征组分峰面积诊断比值作为确证指标。结果:建立了补骨脂中药材特征组分筛查库,选定出2组特征组分CoryliA/补骨脂酚和补骨脂素/异补骨脂素,绘制箱图确定CoryliA/补骨脂酚的非异常值范围为0.061~0.115,补骨脂素/异补骨脂非异常值范围为1.14~1.68。通过市售样品对建立的筛查和确证方法进行验证。结论:该方法简单高效,适用于配制酒和代用茶中非法添加补骨脂的检测。     

威灵壮骨胶囊质量标准研究

目的:建立威灵壮骨胶囊的质量标准。方法:采用TLC法对处方中的补骨脂和威灵仙进行了定性鉴别研究;采用HPLC法测定淫羊藿苷的含量,选用Cromasil C18(4.6mm×250mm,5μm)色谱柱;乙腈-水(25:75)为流动相,检测波长270nm,流速1.0ml/min。结果:TLC法可鉴别出补骨脂和威灵仙的特征斑点,专属性强,分离度好;淫羊藿苷浓度在0.021～0.192mg/ml范围内与峰面积呈良好的线性关系(r=0.9994),平均回收率为99.38%,RSD=1.61%。结论:该方法简便可行,可用于威灵壮骨胶囊的质量控制。     

高效液相色谱-串联质谱法同时测定保健食品中淫羊藿苷、金丝桃苷、补骨脂素

目的建立高效液相色谱-串联质谱法(high performance liquid chromatography-tandem mass spectrometry,HPLC-MS/MS)测定保健食品中淫羊藿苷、金丝桃苷、补骨脂素的分析方法。方法样品经70%甲醇提取后,采用0.1%甲酸(A)和乙腈(B)作为流动相进行梯度洗脱,质谱离子源选用电喷雾离子(electron spray ionization,ESI+)源,采用多离子检测模式(multiple reaction monitoring,MRM)对定量离子和定性离子进行监测,在液相色谱-串联质谱仪上测定。结果在15 min内完成3种目标化合物的分离分析。3种功能成分在0.25、0.5和5 mg/kg添加水平的回收率为84.3%~95.0%,相对标准偏差为0.67%~2.11%(n=7),方法检出限分别为0.05、25、10μg/kg。结论该方法快速、准确、灵敏,适合保健食品中淫羊藿苷、金丝桃苷、补骨脂素的同时检测。     

HPLC法同时测定金银花等样品中6种绿原酸异构体的含量

目的:建立HPLC法同时测定茶叶、枸杞叶、地瓜叶、咖啡、金银花中新绿原酸、绿原酸、隐绿原酸、异绿原酸B、异绿原酸A和异绿原酸C的含有量。方法:采用50%甲醇溶液为提取剂,超声波辅助提取30 min,提取液的分析采用Agilent Eclipse XDB-C18色谱柱(4.6 mm×250 mm,5μm),流动相乙腈-0.1%甲酸溶液,梯度洗脱;流速1.0 mL/min,进样量10μL,检测波长327nm,柱温30℃。结果:6种绿原酸异构体在0.50~50 mg/L范围内线性关系良好(r>0.9995),检出限1.1~1.5 mg/kg,定量限3.7~5.0 mg/kg;在不同植物样品基质中平均加样回收率93.5%~102%,RSD>3.17%。结论:该方法简便,重复性好,准确度高,可用于植物样品中绿原酸及其异构体的含量测定及产品质量控制。     

超高效液相色谱-三重四级杆质谱法测定保健食品中六种功能成分

建立一种保健食品中黄芪甲苷、毛蕊异黄酮葡萄糖苷、甜菜碱、补骨脂素、异补骨脂素和淫羊藿苷的检测方法。样品经甲醇40℃超声提取60 min,采用水（A）和0.1%甲酸乙腈（B）作为流动相,利用超高效液相色谱-三重四极杆质谱联用仪,选用电喷雾离子（electron spray ionization,ESI+）源、正离子检测模式（positive mode,MRM）进行测定。结果表明,6种功能成分的回收率为85.7%～108.5%,该方法实验室内变异系数为0.91%～4.32%(n=7),方法检出限为0.02～0.60μg/kg。该方法准确、灵敏、高效,适合于中药类保健食品中特征成分黄芪甲苷、毛蕊异黄酮葡萄糖苷、甜菜碱、补骨脂素、异补骨脂素和淫羊藿苷的分析检测。     

HPLC法测定洋葱中异蒜氨酸

目的:建立HPLC法测定洋葱中异蒜氨酸的含量。方法:色谱条件:C18色谱柱(250mm×4.6mm),流动相:100%水;流速:0.8mL/min;检测波长:230nm;柱温:25℃;进样量:20μL。结果:红皮、黄皮、白皮洋葱中异蒜氨酸含量分别为0.876、0.839、0.377mg/g(n=3);加样回收率为102.9%,RSD%=2.3%(n=3),异蒜氨酸浓度在23~420μg/mL范围内线性关系良好(r=0.9999)。结论:本HPLC法操作简单,结果准确,重复性好。      

HPLC法测定洋葱中异蒜氨酸

目的:建立HPLC法测定洋葱中异蒜氨酸的含量.方法:色谱条件:C18色谱柱(250mm×4.6mm),流动相:100%水;流速:0.8mL/min;检测波长:230nm;柱温:25℃;进样量:201μL.结果:红皮、黄皮、白皮洋葱中异蒜氨酸含量分别为0.876、0.839、0.377mg/g(n=3);加样回收率为102.9%,RSD%=2.3%(n=3),异蒜氨酸浓度在23～4201μg/mL范围内线性关系良好(r=0.9999).结论:本HPLC法操作简单,结果准确,重复性好.     

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