高效液相色谱法测定猴头菇中4种核苷含量

目的：运用高效液相色谱法分析猴头菇中尿苷、肌苷、乌苷、腺苷的含量.方法：色谱条件为：Grace Prevail SelectC18（4.6＆#215;150 mm,5μm）分析柱;流动相为A（水）-B（甲醇）二元梯度洗脱,梯度为：0-4.0 min,B％为0→2％;4.0-10.0min,B％为2％→10％;10.0-16.0min,B％为10％→95％;16.0-20.0min,B％为95％→100％;20.0-25.0min,B％为100％→100％;柱温25℃;进样量10μL;流速1mL· min-1;检测波长254 nm.结果：尿苷、肌苷、鸟苷和腺苷分另别在2.0-181.0 μg·mL-1（r=1.0000）、1.5-190.0 μg·mL-1（r=0.9999）、0.8-126.4μg·mL-1（r=0.9999）和1.0-171.2μg·mLmL-1（r=1.0000）范围内线性关系良好.加样回收率（n=3）分别为99.5％（RSD=2.8％）、100.5％（RSD=3.2％、98.9％（RSD=3.4％）和98.1％（RSD=3.7％.三个产地猴头菇的核苷含量差异比较大,浙江江山猴头菇的尿苷、鸟苷、腺苷含量是所测样品中最高的,分别为：1.44 mg·g-1、1.06 mg·g-1和2.72 mg·g-1,猴头菇中肌苷含量极低,仅在浙江常山和福建莆田产猴头菇中检出,浙江江山猴头菇未检出.结论：本法能够快速、简便地测定猴头菇中主要核苷的含量,为其质量控制提供保证.     

HPLC同时测定风寒感冒颗粒中葛根素和升麻素苷的含量

目的建立高效液相色谱法(HPLC)同时测定风寒感冒颗粒中葛根素和升麻素苷含量的方法。方法采用Agilent ZORBAX SB-C18色谱柱(250 mm×4.6 mm,5μm),乙腈-0.1%磷酸梯度洗脱,柱温40℃。结果在0.040 70~2.0340μg范围内,葛根素进样量与峰面积呈良好线性关系,Y=5270.2X-10.331(r=1.000);在0.000 817 6~0.040 88μg范围内,升麻素苷进样量与峰面积呈良好线性关系,Y=16 003.6X-6.765(r=0.9999);平均回收率分别为100.5%和101.1%,RSD分别为1.3%和1.2%。结论此法准确,灵敏度高,重复性好,为风寒感冒颗粒全面的质量控制提供了科学依据。     

RP-HPLC法测定甘草梅中甘草酸和甘草苷的含量

目的:建立用RP-HPLC法同时测定甘草梅中甘草酸和甘草苷含量的方法.方法:超声辅助醇提取.采用LiChrospher RP-Cl18色谱柱(250ram×4.6mm,51xm),以乙腈-水(1.O%甲酸)为流动相,梯度洗脱.结果:甘草酸在0.094～11.75μg范围内呈良好线性关系,回归方程为Y=1013.4854X-5.6802(r=1.0000),平均回收率为97.5%,RSD=1.65%;甘草苷在0.044～11μg范围内呈良好线性关系,回归方程为Y=1340.0528X+148.0769(r=O.9995),平均回收率为97.8%,RSD=1.51%.结论:该方法操作简便,结果可靠.     

高效液相色谱法同时测定小茴香中芦丁和茴香醛的含量

建立同时测定小茴香中芦丁和茴香醛含量的反相高效液相色谱(RP-HPLC)梯度洗脱法。采用ZORBAX-SB-C18色谱柱(150mm×4.6mm,5μm);以0.1%(体积比)磷酸水溶液-甲醇为流动相进行梯度洗脱,流速为0.6 mL/min,柱温为25℃;检测器波长为265nm进行检测。芦丁在0.04088~0.4088μg范围内线性关系良好,R2=0.9998;茴香醛在0.01434~0.1434μg范围内线性关系良好,R2=1.0000。该方法简单快速,分离度较好,可以作为小茴香的质量控制方法之一。     

HPLC法测定酒萸肉中马钱苷含量

目的 建立高效液相色谱法测定酒萸肉中马钱苷含量方法.方法 色谱柱Agilent C18柱 (4.6mm×150mm,5μm);流动相乙腈-水(15:85);检测波长240nm;流速1.0ml·min-1;结果马钱苷在5～50μg·mL-1的浓度范围内具有良好的线性关系(r=0.9995).回收率为97.73%,RSD=0.48%.结论 该方法简便、可靠、准确,可用于测定酒萸肉中马钱苷含量.同时暂定酒萸肉中马钱苷含量限度不得低于0.60%.     

HPLC法同时测定大蒜及蒜薹中的大蒜辣素和二烯丙基二硫

建立了同时测定大蒜和蒜薹中大蒜辣素和二烯丙基二硫的高效液相色谱测定方法。样品经超声辅助提取后,采用乙腈-水(60∶40)作为流动相,经过色谱柱symmetry C18(4.6 mm×250 mm,5μm)分离,220 nm下检测。结果表明:大蒜辣素在13.75~275.00μg/m L(r=0.9997)范围内,二烯丙基二硫在0.65~26.00μg/m L(r=0.9995)范围内,线性关系良好;大蒜辣素和二烯丙基二硫的平均回收率分别为97.93%(RSD=0.45%)和98.13%(RSD=0.78%)。该方法样品前处理简单,测定快速,定性定量准确,回收率高,精密度好,适用大蒜及蒜薹中大蒜辣素和二烯丙基二硫含量的同时测定。     

HPLC测定清热明目丸中绿原酸、柚皮苷、黄芩苷的含量

目的建立高效液相色谱法(HPLC)同时测定清热明目丸中绿原酸、柚皮苷、黄芩苷的含量。方法采用Agilent Eclipse XDB-C_(18)(250 mm×4.6 mm,5μm)色谱柱,以乙腈-0.4%磷酸溶液为流动相,梯度洗脱,流速为1.0 ml/min,检测波长为283 nm。结果绿原酸、柚皮苷、黄芩苷浓度分别在1.937~77.48μg/ml(r=0.9998)、1.028~41.12μg/ml(r=0.9999)、1.841~73.64μg/ml(r=0.9999)范围内与峰面积呈良好线性关系;平均加样回收率分别为98.6%,98.6%,99.1%,RSD分别为1.6%,1.2%,1.2%(n=9)。结论建立的分析方法能同时测定绿原酸、柚皮苷、黄芩苷3种成分,该方法快速简便、结果准确,可用于清热明目丸的质量控制。     

高效液相色谱法测定减肥类保健食品中番泻苷A、番泻苷B的含量

目的建立一种用于测定减肥类保健食品中番泻苷A、番泻苷B的高效液相色谱(high performance liquid chromatography,HPLC)检测方法。方法采用ZORBAX SB-C_(18)柱(4.6 mm×150 mm,5μm),以乙腈-0.1%磷酸水溶液为流动相进行梯度洗脱,流速为1.0 mL/min,柱温为40℃,二极管阵列检测器进行检测,检测波长为254 nm。结果番泻苷A、番泻苷B分别在2.050~20.50μg/mL(r=0.9999)、1.803~18.03μg/mL(r=0.9993)范围内呈良好线性关系,定量限分别为30、27μg/kg;平均回收率分别为96.8%、95.1%,相对标准偏差分别为1.3%、2.3%。结论该方法简单、可行,结果准确、可靠,适用于减肥类保健食品中番泻苷A、番泻苷B含量的测定。     

高效液相色谱法同时测定蛹虫草中四种核苷类活性成分

采用超声波提取,建立了高效液相色谱法同时测定蛹虫草中四种核苷类活性物质的分析方法。优化了色谱条件选用Diamosil C18(250mm×4.6mm,5μm)色谱柱,以水-甲醇梯度洗脱,检测波长260nm,虫草素、腺苷、鸟苷及尿苷在此条件下得到了很好的分离。该方法灵敏度高、定量准确、重现性好、回收率高(97.1%~98.3%),其测定RSD范围为1.19%~4.62%(n=5)。     

HPLC法同时测定党参中5种核苷和碱基

建立了超声辅助提取结合高效液相色谱(HPLC)测定党参中胞苷、尿苷、腺嘌呤、鸟苷和腺苷含量的方法。党参的最佳提取条件为:20倍量的纯净水超声提取60 min,提取2次。采用Venusil MP C_(18)(2)色谱柱(4.6 mm×250 mm,5μm)分离和测定目标分析物,流动相为甲醇-水梯度洗脱,检测波长260 nm,体积流量1.0 m L/min,柱温35℃。结果表明,5种化学成分的质量浓度与峰面积的线性关系良好(R~20.9995),平均回收率为97.05%~101.08%,RSD≤3.01%。不同产地党参核苷类成分含量有所差异,18个党参样品中胞苷、尿苷、腺嘌呤、鸟苷、腺苷及核苷总量介于68.71~478.82、171.33~629.60、33.63~140.05、221.31~651.37、143.26~511.78、679.87~2011.67μg/g之间。本研究所建立方法操作简便,精密度、稳定性和重复性良好,准确可靠,适用于党参药材中5种核苷和碱基成分的同时测定,为全面客观地认识党参药材功效物质基础、丰富和发展党参药材多指标评价体系研究提供科学依据。     

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