高效液相色谱法测定叔丁基对苯二酚含量的方法学研究

建立了HPLC叔丁基对苯二酚含量的方法:色谱柱:Shim-pack Vp-ODS(150mm×4.6 mm,5μm)接Cl8保护柱(20mm×4.6mm,5μm);以乙腈∶水=32∶ 68(V/V,含1%乙酸)作为流动相;流速:0.8mL/min;检测波长:290nm;柱温:25℃.结果表明TBHQ浓度在2×10-4～1.0mg/mL范围内与峰面积线性关系良好r≥0.9999,最低检测限为4ng,并建立了回收率及日内和日见精密度实验.     

反相高效液相色谱法检测单烷基二苯醚的质量分数

应用反相高效液相色谱法检测辛烯和二苯醚烷基化产物中单取代辛烷基二苯醚(C8-ADPO)的质量分数。色谱柱为C8色谱柱(250 mm×4.6 mm);流动相为V(甲醇)∶V(二氯甲烷)=8∶2;检测波长242 nm。C8-ADPO质量浓度为10~1 000 mg/L时与其峰面积成线性关系,线性方程为Y=7 912.08X+94 627.00,线性相关系数R=0.999 1,RSD为0.96%,回收率为100.0%~105.0%。     

辣素超声提取-HPLC测定方法研究

研究了用高效液相色谱法测定辣椒中的辣椒素。色谱柱:(ODSC18反向柱,4.6mm×250mm,5μm);流动相:甲醇∶水=8∶2(V/V);紫外检测器波长280nm;流速0.8mL/min;柱温30℃。结果表明:该方法具有灵敏度高、准确度好和可靠性强等优点。     

柱层析法分离万寿菊叶黄素

本试验研究了万寿菊叶黄素的分离方法及分离条件。采用高效液相色谱法(HPLC)测定叶黄素的含量,色谱柱为岛津VP-ODSC18柱(150mm×4.6mm,5μm),检测波长454nm;以甲醇-0.1%磷酸溶液为流动相进行梯度洗脱,流速1.0mL/m in;柱温30℃;进样量10μL;校准曲线法定量,在0.6~2.0μg范围内具有良好的线性关系,回归方程为Y=1.16×107C+4.99×104,相关系数r=0.9984。采用柱层析法分离万寿菊叶黄素的皂化液,实验结果表明:固定相采用硅胶G(100~200目);胡萝卜素洗脱剂为V(石油醚)∶V(乙酸乙酯)=5∶1;叶黄素洗脱剂为V(石油醚)∶V(乙酸乙酯)=1∶1;层析柱规格为Φ26×510mm;使用皂化液直接湿法上样;吸附时间为30m in;上样量为0.4mL皂化液/g硅胶;柱温为常温;皂化液可直接上样;在以上条件下,经分离回收溶剂后得到含量为83.3%的叶黄素产品。该方法有良好的分离能力,便于操作,产品纯度稳定。硅胶在重复使用5次以内,对分离效果的影响不明显。     

酸水解-柱前衍生法测定鲍鱼中氨基酸含量

优化测定三亚鲍鱼氨基酸试验条件。运用酸水解法处理样品,2,4-二硝基氟苯柱前衍生化,辅以高效液相色谱(HPLC)测定氨基酸含量;色谱条件为:色谱柱,Inertsil ODS-3 C_(18)柱(4.6 mm×150 mm,5μm);流动相A,含1%N,N-二甲基酰胺的0.05 mol/L醋酸钠-醋酸缓冲液(pH 6.4);流动相B,乙腈-水(1︰1,V/V),流动相A︰流动相B为70︰30(V/V);检测波长360 nm;流速1 mL/min;柱温33℃。结果发现,样品氨基酸总含量为808.73 mg/g。此方法样品处理充分彻底,操作简单,各氨基酸分离良好;与常规方法相比,HPLC法测定简便快速,精密度高,检出限低,回收率高,准确性好,结果令人满意。     

HPLC测定祖卡木胶囊中罂粟碱的含量

目的建立HPLC测定祖卡木胶囊中罂粟碱含量的方法。方法色谱条件:DIKMAC8(250mm×4.6mm,5μm)色谱柱;流动相为甲醇-乙腈-1%乙酸铵-1%三乙胺(40∶20∶39∶1);流速1.0mL/min,检测波长为240nm。结果罂粟碱的线性范围为10.91～218.16ng,r=0.9999,平均回收率为97.5%,RSD=1.01%。结论本法处理简便,测定结果准确,重复性好,可用于本品的质量控制。     

高效液相色谱-蒸发光散射检测器定量分析谷胱甘肽含量

为了快速定量检测溶液中的谷胱甘肽(GSH)含量,建立了应用C18反相柱,HPLC-ELSD测定GSH含量的方法,确定了高效液相色谱分离条件。色谱条件为:色谱柱(Kromasil C18,250×4.6mm,5μm);流动相:V(H2O)∶V(CH3CN)∶V(TFA)=96.2∶3.7∶0.1;柱温:室温;流速:1.0mL/min;进样量:20μL;漂移管温度90℃;氮气流速:1.5L/min;i mpactor on模式;增益(Gain):1。结果表明,在此条件下,GSH浓度的自然对数与峰面积的自然对数成很好的线性关系(R2=0.9995);精密度2.15%;最低检测限30.73mg/L;加标回收率99.78%。该方法快速、简便、准确,适合从复杂体系中快速检测谷胱甘肽的含量。     

反相高效液相色谱法快速测定复方维生素片中微囊化β-胡萝卜素

目的建立一种快速测定复方维生素片中微囊化β-胡萝卜素的反相高效液相色谱法。方法样品经0.1 mol/L的碳酸钠溶液破坏微囊,甲醇-乙腈(7∶3,V/V)混合溶液超声提取,采用Agilent SB-C_8柱(4.6 mm×150 mm,5μm)分离,流动相为甲醇-乙腈(9∶1,V/V),检测波长为448 nm。结果β-胡萝卜素在本试验色谱条件下能完全分离,其线性范围为0.41~6.20μg/ml,平均回收率99.4%~103.3%,RSD2.0%。结论该方法操作简便,能测定复方维生素片中微囊化β-胡萝卜素,精密度和回收率高,重复性好,结果符合要求。     

辣椒中辣椒素类物质的检测方法及稳定性研究

目的:通过对GB/T 21266-2007中辣椒素和二氢辣椒素检测的色谱条件的优化,使辣椒素和二氢辣椒素的测定更加快速,并考察辣椒素与二氢辣椒素贮存过程中的稳定性。方法:高效液相色谱法,色谱条件为C18色谱柱(4.6mm×250mm,5μm),流动相为甲醇∶水(V∶V=70∶30),流速为1mL/min,检测波长为280nm,进样量10μL,柱温30℃。结果 :与GB/T 21266-2007的色谱条件相比,检测时间缩短了约12min。提取出的辣椒素与二氢辣椒素在室温条件下贮存一个月,其含量没有发生剧烈波动。结论:此色谱条件能对辣椒素和二氢辣椒素进行有效检测,且能明显缩短两者的保留时间;提取出的辣椒素与二氢辣椒素室温条件下短时间内能保持稳定。     

高效液相色谱法测定贵州顶坛花椒中麻味成分羟基-β-山椒素的含量

为了对贵州顶坛花椒中的麻味成分进行定量测定,从贵州产顶坛花椒中分离得到麻味特征性成分羟基-β-山椒素,并建立高效液相色谱方法定量检测花椒中羟基-β-山素椒的含量。色谱柱:YMC-Pack ODS-A(6.0mm×150mm,5μm);流动相:乙腈∶水(V/V为45∶55);流速为0.7 mL/min,柱温为35℃,波长为254nm;线性范围为0.01~0.14μg,相关系数R2=0.9994,检测限为0.0002μg,回收率在97.92%~103.60%,相对标准偏差(RSD)2.0%。结果表明:贵州顶坛花椒中羟基-β-山椒素的含量较高,符合其"麻味重"的特点。     

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