广陈皮提取物的HPLC指纹图谱研究

建立广陈皮提取物的高效液相色谱(high performance liquid chromatography,HPLC)指纹图谱,为陈皮提取物原料的质量控制提供依据。采用HPLC法分析测定13批广陈皮样品。色谱柱:Eclipse XDB-C18(4.6 mm×150 mm,5μm);流动相:甲醇-2.0%乙酸水溶液梯度洗脱;检测波长:283 nm;柱温:25℃;流速:1.0 mL/min;上样量:10μL。建立广陈皮提取物的指纹图谱,确定出11个共有峰,广陈皮样品的相似度在0.967~0.974之间。     

苦瓜皂苷高效液相色谱指纹图谱研究

建立苦瓜皂苷类成分的高效液相色谱法(HPLC)指纹图谱.采用中药色谱指纹图谱相似度评价系统,对不同产地苦瓜中皂苷进行HPLC分析,流动相:乙腈和水梯度洗脱;流速:1.0mL/min;色谱柱:ZorbaxSB-C18柱(150×4.6mm,5 μm);柱温:25℃;检测波长:209 nm;进样量:20 μL;分析时间:65 min.确定8个共有峰作为苦瓜皂苷的特征指纹峰;不同产地苦瓜皂苷指纹图谱与对照指纹图谱(R)的相似度均大于0.85.该方法建立的苦瓜皂苷HPLC指纹图谱,为苦瓜鉴别和品质评价、质量控制、制定质量标准提供参考.     

HPLC测定黄精的指纹图谱

目的建立山东泰安黄精的高效液相色谱指纹图谱。方法采用高效液相色谱法(HPLC)比较分析不同批次黄精的指纹图谱,并采用"中药色谱指纹图谱相似度评价系统(2004A版)"计算和处理测定的图谱。色谱条件:安捷伦Eclipse XDB-C18(150 mm×4.6 mm,5μm)色谱柱,乙腈-水溶液为流动相,梯度洗脱,流速1 ml/min,检测波长203 nm,柱温30℃。结果通过共有模式相似度分析可确定16个色谱峰,构成山东泰安黄精指纹图谱特征峰。利用该色谱条件比较山东泰安黄精和河北黄精的指纹图谱,二者有显著差异。结论HPLC建立的黄精指纹图谱稳定性、重复性较好,可为区分其他区域的黄精提供参考。     

可可粉色谱指纹图谱的构建及其质量控制中的应用

目的:建立可可粉高效液相指纹图谱。方法:采用RP-HPLC法。色谱柱为Agilent ZORBAX Extend-C18(250mm×4.6mm,5μm);以乙腈-0.05%磷酸缓冲盐溶液为流动相梯度洗脱;柱温:30℃;流速:0.8mL/min;检测波长:210nm;进样量:10μL。测定10批不同来源可可粉图谱,并运用相似度分析、系统聚类分析对可可粉进行分类研究。结果:建立了精密度、稳定性和重复性均良好的HPLC指纹图谱,确立了5个共有峰,指认了其中3个色谱峰,并建立了可可粉指纹图谱共有模式,测得各批次样品指纹图谱相似度均在0.90以上,系统聚类分析将10批可可粉分为3类。结论:该方法简便易行、准确、重现性好,可以作为可可粉质量评价的重要依据。     

红花椒和青花椒HPLC指纹图谱的分析

采用HPLC法建立了花椒的高效液相指纹图谱。色谱条件为色谱柱:迪马铂金C18(250 mm×4.6 mm,5μm),柱温:30℃,流动相:V(乙腈)∶V(水)=50∶50,流速:0.8 mL/min,检测波长:254 nm,进样量2μL,检测时间:40 min。采用《中药色谱指纹图谱相似度评价系统A版》(研究版)提取HPLC图谱共有模式,计算各批次样品的相似度,结果显示,红花椒特征指纹图谱中有11个共有峰,15批红花椒样品中,除一份样本外,其他14批样品相似度均大于0.97,表明不同产地红花椒内在品质相似;青花椒特征指纹图谱中有10个共有峰,18批青花椒样品相似度都很低,相似度为0.52～0.67,表明不同产地青花椒内在品质差异性很大。红花椒相比青花椒在保留时间约30 min处存在一个比较明显的色谱峰,并采用飞行时间质谱对该特征差异色谱峰进行鉴定,推断该物质为不饱和五烯酰胺,即羟基-γ-山椒素或2'-羟基-N-异丁基-2,4,8,10,12-十四烷五烯酰胺及其同分异构体。     

五指毛桃入药膳的HPLC特征指纹图谱研究

采用高效液相色谱法建立五指毛桃入药膳的HPLC特征指纹图谱,探讨药膳中可作为评价指标的目标药材。运用HPLC分析五指毛桃药膳的指纹图谱。色谱柱:Waters Shield RPC18柱(250 mm×4.6 mm,5μm);流动相为甲醇(A)-0.1%磷酸(B),梯度洗脱;流速1.0 mL/min;检测波长246 nm;柱温30℃,测定10批五指毛桃药膳指纹图谱。在特征指纹图谱中,确定14个共有峰,其中补骨脂素含量最高;十批样品相似度在0.90~0.99,且方法学考察符合规定的标准。五指毛桃入药膳后可以检测出相关特征成分,可以作为药膳质量评价的对象。食材脂肪酸成分对五指毛桃特征成分的检出影响不大。     

石硖龙眼HPLC指纹图谱的研究

采用高效液相色谱(HPLC)法,建立了石硖龙眼的HPLC 指纹图谱。色谱条件为：Nucleosil C18 反相柱(250mm × 4mm,5μm),流动相为0.01mol/L 的KH2PO4 和甲醇,二元梯度洗脱,流速0.8ml/min,检测波长260nm,柱温4℃。结果表明：14 批次的石硖龙眼水溶性提取物色谱图共有峰13 个。经“中药指纹图谱鉴别分析系统”统计分析,共有峰相对保留时间的相对标准偏差在1.2% 以下,相似度均在0.967 以上。符合指纹图谱的要求,可建立共有模式,作为科学评价石硖龙眼产品质量的检测方法。     

不同产地带鱼高效液相色谱指纹图谱的建立及其聚类分析

摘 要:目的 建立不同产地带鱼高效液相(high performance liquid chromatography, HPLC)指纹图谱,结合聚类分析确定带鱼产地归属。方法 采用乙酸乙酯提取,料液比1:100,Agilent Eclipse XDB C18柱（4.6 mm×250 mm,5 μm）,检测波长210 nm,柱温30℃,进样量20 μl,流速0.5 ml/min,乙腈(A)和0.1%磷酸水(B)为流动相梯度洗脱;通过相似度评价系统和聚类分析对指纹图谱进行分析。结果 采用中药色谱相似度评价系统建立了各产地带鱼HPLC指纹图谱共有模式,确立了13个共有峰和7个特征峰。对7个特征峰聚类分析,结果显示5个产地28个带鱼样品能够按照产地来源正确聚类。结论 方法操作简便、准确可靠、重复性好,可用于带鱼产地归属。     

花椒HPLC指纹图谱建立及指标性成分的测定

文章采用HPLC法建立多批次花椒指纹图谱,并测定其主要成分含量。指纹图谱的色谱条件为Wondasil C18色谱柱(250mm×4.6mm,5μm),乙腈-水梯度洗脱,检测波长268nm,柱温30℃,流量0.8mL/min。以其指纹图谱为特征,进行相似度和聚类分析。指纹图谱确定了12个共有峰,所有样品的相似度均大于0.9,表明各产地花椒具有较好的一致性;当类间距离为10时,16批次花椒样品被分成3大类;花椒的2个主要成分羟基-α-山椒素的含量在0.323%～1.570%,羟基-β-山椒素的含量在0.03%～0.622%。花椒样品各批次间指纹图谱和主要成分含量均有一定的差异。建立的花椒HPLC指纹图谱及主要成分含量测定方法可为花椒食品质量控制和评价提供科学依据。     

胀果甘草悬浮细胞中黄酮类化合物HPLC分析

用HPLC法建立野生胀果甘草与悬浮培养的胀果甘草细胞中黄酮类化合物的HPLC指纹图谱,并采用LC-MS技术推测HPLC共有峰中主要指纹峰的化学结构。采用Agilent EclipseXDB-C18色谱柱(4.6 mm×250 mm,5μm),流动相为乙腈:0.1%冰醋酸,梯度洗脱,流速1.0 mL/min,检测波长310 nm。Agilent1100LC/MSD液质联用系统,ESI源。在设定的色谱条件下,分别得到的野生甘草与甘草细胞中黄酮类化合物指纹图谱,用中国药典相似度评价系统软件进行评价相似度为75.2%,根据LC-MS结果推断了HPLC共有峰中2个主要指纹峰分别为甘草苷和甘草素。结果表明野生甘草中绝大部分黄酮类化合物在甘草细胞中均有合成,使利用细胞悬浮培养生产的甘草黄酮类化合物成为可行的途径。     

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.     

Detection of adulteration of locust bean gum with guar gum by capillary electrophoresis and polarized light microscopy

Capillary electrophoresis (CE) and polarized light microscopy (PLM) were utilized in the detection of the adulteration of locust bean gum with guar gum. For CE analyses, standards of locust bean and guar gums were extracted with 30% CH₃CN, removing the residual proteins from the gum matrix. A 8.75 mM NaH₂PO₄-20.6 mM Na₂B₄O₇ buffer, pH 9, was used to separate these proteins and to identify marker proteins that were present in the guar gum. These markers did not co-migrate with components in the extracts of mechanically processed locust bean gum, and are used as indicators of adulteration. Using PLM with toluidine blue and iodine staining techniques, unadulterated locust bean gum samples were distinguished from mixed samples through the differential staining of components in locust bean versus guar and tara gums. These experiments in the use of CE and PLM provide orthogonal and complementary methods for the verification of 'true' positives and the elimination of 'false' positives.