用气相色谱法测定饮料酒中β-苯乙醇含量的探讨

利用气相色谱外标法测定饮料酒中的β-苯乙醇,采用HP-INNOWAX石英毛细管柱(30m×0.32mm×0.25um)进行检测,建立标准曲线相关系数为0.99999,检测限为0.5mg/L,回收率为99％～101％.测定结果证明该方法稳定,重复性好、回收率高.同时指出2-乙基正丁酸溶液(0.02％vol)不稳定,不适合作为标准物质.     

七种花色苷色素中矢车菊-3-葡萄糖苷含量研究

目的:调查研究七种花色苷色素中矢车菊-3-葡萄糖苷的含量.方法:实验采用高效液相色谱法,检测条件为Ultimate(R)LP-C18(5μm,250mm ×4.6mm)色谱柱;甲酸水溶液(1∶9)∶甲醇=85∶15(v/v)梯度洗脱;流速1mL/min;柱温30℃;检测波长535nm.结果:萝卜红、甘薯红、甜菜红中不含矢车菊-3-葡萄糖苷,葡萄皮色素、欧洲越橘色素、红米红、甘蓝红中矢车菊-3-葡萄糖苷含量分别为5.09％、4.15％、10.84％、0.03％.结论:七种花色苷色素中矢车菊-3-葡萄糖苷含量存在明显差异,葡萄皮色素、欧洲越橘红色素、红米红中矢车菊-3-葡萄糖苷含量较高,为矢车菊-3-葡萄糖苷的进一步开发利用提供了可靠的理论依据.     

柱前衍生-高效液相色谱法测定酒中的氰化物

目的 建立柱前衍生-高效液相色谱法测定酒中氰化物含量的方法 .方法 采用异烟酸-巴比妥酸柱前衍生,高效液相色谱法测定.采用菲罗门Gemini C18(4.6 mm×250 mm,5μm)色谱柱,以1％乙酸-乙腈(50:50)为流动相,流速为1.0 ml/min,检测波长为600 nm.结果 氰化物的衍生产物的线性范围为...     

GC-MS法测定羊毛织物中氯菊酯的含量

建立了一种气相色谱-质谱联用(GC-MS)检测羊毛织物中氯菊酯的分析方法.采用HP-5MS(30 m×0.25 mm×0.25 μm)毛细管色谱柱对氯菊酯进行检测.顺反式氯菊酯得到了较好的分离,回收率在88.0％ ～94.3％范围,相对标准偏差RSD在5.4％ ～9.7％之间.另外用适用于纺织品中禁用偶氮染料检测的HP-5 MS(30 m×0.25 mm ×0.25 μm)毛细管色谱柱来检测氯菊酯,节省了测试人员拆装色谱柱的时间,大大提高了检测效率.此方法适用于大批量的检测.     

HPLC法测定曲奇饼干中丙烯酰胺的含量

确定了曲奇饼干中丙烯酰胺含量的高效液相检测方法.样品预处理采用脱脂,固液提取,离心破乳,液液萃取,旋蒸浓缩及氮气吹干,超纯水定容等步骤,经Kromasil ODS色谱柱(250 mm×4.6 mm,5 μm)分离.HPLC检测用甲醇-水(5:95,体积比)为流动相洗脱,VWD检测器检测波长210 nm.方法在0.2/mL～1.0μg/mL浓度范围内具有良好的线性关系(r=0.9998),检出限为4.4ng/mL,RSD为0.37％;定量限14.5 ng/mL,RSD为7.4％,加标回收率在81.6％～101.3％之间.本方法定量准确,操作简单,适用于曲奇饼干中丙烯酰胺的测定.     

白酒中5种生物胺的HPLC定量分析

应用紫外检测-反相高效液相色谱(RP-HPLC)检测技术,建立了白酒中多种生物胺的定量方法.定量方法包括液液萃取(LLE)、丹磺酰氯柱前衍生、氮吹浓缩、RP-HPLC检测.采用Agilent C18色谱柱(4.6 mm×250mm,5μm),流动相采用乙腈和水,进行梯度洗脱,流速为0.4mL/min,柱温为20℃,检测波长为254nm.该方法在线性范围内线性关系良好(R2＞0.99),5种生物胺的最低检测限为0.001 ～ 0.032 mg/L,相对标准偏差(RSD)低于6％,回收率为80.19％ ～104.05％.研究结果表明,白酒中生物胺与发酵酒中不同,其吡咯烷浓度最高.初步检测了三种基本香型的白酒,与浓香型、清香型白酒相比,酱香型白酒具有更低的生物胺.     

芝麻油中芝麻素含量测定的研究

采用先皂化芝麻油,然后用石油醚萃取不皂化物,再用甲醇溶解定容不皂化物的前处理方法,利用高效液相色谱法测定芝麻油中芝麻素的含量.色谱柱为GL Sciences(ODS -3,250 mm×4.6mm,5μm),流动相为甲醇-水(体积比为80∶20),流速1 mL/min,检测波长287 nm,柱温40℃.所得芝麻素的保留时间为8.5 min,芝麻素的平均加标回收率为99.3％(RSD=1.89％),精密度为0.77％.建立的方法能简便、快速、准确测定芝麻油中芝麻素含量.     

RP-HPLC法测定毛鸡骨草中芹菜素-6,8-C-二葡糖苷含量

目的 建立测定毛鸡骨草药材中芹菜素-6,8-C-二葡糖苷含量的方法.方法 用反相高效液相色谱法,色谱柱为Lichrospher C18 (250 mm×4.6 mm,5μm);流动相为甲醇-0.1％三氟乙酸(35:65),流速1.0 mL/min,检测波长272 nm,柱温为室温.结果 芹菜素-6,8-C-二葡糖苷在0.010 2～0.102 0 mg/mL范围内线性关系良好(r=0.999 8);平均回收率(n=6)99.3％,RSD 2.43％.结论 所建方法简捷、快速,结果准确,可为评价毛鸡骨草药材的质量提供可靠的依据.     

分散微固相萃取-超高效液相色谱-高分辨质谱法测定火锅底料中罂粟壳生物碱

目的 建立火锅底料中5种罂粟壳生物碱的超高效液相色谱-高分辨质谱检测方法.方法 样品经基于强阳离子交换吸附剂(PCX)的分散微固相萃取(DMSPE)提取和净化后,以0.1％甲酸水溶液-0.1％甲酸乙腈为流动相进行梯度洗脱,HSS T3色谱柱(2.1 mm×100 mm,1.8μm)分离,高分辨质谱平行反应监测模式采集,...     

卫生整理纺织品中芦荟组分含量的HPLC/DAD测定法

采用高效液相色谱-二级管阵列检测器(HPLC/DAD),建立测定纺织品中芦荟主要成分(芦荟苷,芦荟大黄素和大黄酚)含量的方法.HPLC的色谱柱为Agilent Eclipse XDB-C18(4.6×150 mm,5 m),流动相为甲醇-0.1％磷酸水溶液(80∶20,体积比),流速为1.0 mL/min;检测波长为256 nm和358 nm.通过验证,其标准曲线在检测范围内均呈良好线性(R2≥0.999),日内和日间精密度的相对标准偏差RSD小于2.97％,3个加标水平的平均回收率为95.1％～ 101.1％.     

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