高效液相色谱法同时检测啤酒中的酪醇和色醇

本文建立了HPLC法同时检测啤酒中的酪醇和色醇。方法所采用的多极校正标准线性关系良好，样品加标平均回收率为95％-98％，RSD均小于1．5％（n=5），方法检出限分别为0．05mg/L（酪醇）和0．01mg／L（色醇）。     

LLE-UPLC-FLD法测定橄榄油中羟基酪醇和酪醇的含量

建立了液液萃取-超高效液相色谱串联荧光检测器(LLE-UPLC-FLD)快速分离和测定橄榄油中羟基酪醇和酪醇含量的方法。橄榄油样品经乙醇提取后,以0.2%(v/v)甲酸乙腈溶液和0.2%(v/v)甲酸水为流动相,梯度洗脱,采用BEH(50 mm×1.0 mm,1.7 μm)色谱柱,柱温为35 ℃,流速为0.15 mL/min,进样量为2.0 μL,使用荧光检测器在激发波长为300 nm,发射波长为350 nm下进行检测,整个分析过程仅需10 min。羟基酪醇和酪醇的检出限(S/N=3)及定量限(S/N=10)分别为0.11,0.13和0.31,0.39 μg/g,2种组分按高、中、低3个浓度水平加标回收率均高于89.52%;在最优条件下,对20批不同产地橄榄油中的羟基酪醇和酪醇进行检测,羟基酪醇和酪醇的含量范围分别在1.28~20.34及1.03~21.22 μg/g之间;该法简便快速,重复性良好,结果准确可靠,可用于橄榄油中酪醇和羟基酪醇含量的测定。     

响应面法优化橄榄果渣羟基酪醇提取工艺

本研究比较了超声辅助水解与振荡水浴水解提取橄榄果渣中羟基酪醇的工艺。在单因素实验基础上,以提取温度、盐酸浓度、料液比和水解时间为因素,以羟基酪醇提取量(mg/g)为指标,运用响应面法优化提取工艺。结果表明:羟基酪醇的最佳提取工艺为提取温度88 ℃、盐酸浓度1.2 mol/L、料液比 1:36 g/mL、水解时间86 min,此时羟基酪醇的实际提取量为(3.38±0.12) mg/g,与理论值无明显差异。经UPLC检测方法学考察,羟基酪醇在1.28~203.40 μg/g内线性范围关系良好,精密度与稳定性均达到检测要求。本研究对橄榄果渣中羟基酪醇提取工艺条件具有借鉴意义。     

柱前衍生-HPLC法测定啤酒中生物胺及其形成规律研究

建立了柱前衍生-高效液相色谱(HPLC)法同时检测啤酒中8种生物胺的方法,并研究了啤酒酿造原料、酿造过程及腐败菌的生物胺形成规律。样品经5%三氯乙酸溶液提取后,经丹磺酰氯衍生,然后用HPLC进行定性和定量分析。该方法对8种生物胺具有良好的分离效果,并具有线性范围广,精密度和重复性高等优点,适用于啤酒中生物胺的检测。运用该方法对啤酒酿造原料(麦芽和酒花)中生物胺进行检测,发现除β·苯乙胺外其他7种生物胺均有检出,其中色胺和腐胺含量最高。麦汁和发酵过程中主要含有色胺和腐胺,主要来源于原料麦芽。将2株啤酒腐败乳酸菌-乳酸短杆菌(Lactobacillus brevis)BS49和类布氏乳杆菌(Lactobacillus parabuchneri)BS201接入到无菌啤酒中,分析其生物胺形成规律。这2株菌能在啤酒中生长繁殖,并且随着菌体生长啤酒中生物胺含量发生显著变化,接BS49号菌的啤酒中酪胺由0.2 mg/L增加到8 mg/L,接BS201号菌的啤酒中组胺由0.1 mg/L增加到6 mg/L,因此组胺和酪胺可作为判断啤酒在贮藏过程中是否污染乳酸菌的重要指标。     

高效液相色谱法测定保健食品中的羟基酪醇

目的建立高效液相色谱法测定保健食品中羟基酪醇的方法。方法样品用二甲基亚砜进行超声提取后,采用Waters Spherisorb ODS2色谱柱(250 mm×4.6 mm, 5μm)进行分离,以0.12%甲酸水溶液-0.12%甲酸甲醇溶液为流动相等度洗脱,柱温为30℃,流速1 mL/min,紫外检测器进行检测,外标法定量。结果羟基酪醇在12.45～498.0μg/mL范围内线性关系良好,相关系数大于0.999;检出限为0.03g/100g;定量限为0.12 g/100 g;平均回收率为99.5%～100.6%,相对标准偏差值为0.55%～1.13%。结论该方法简便、快捷、高效、准确,适用于保健食品中羟基酪醇的测定。     

用HPLC法检测土耳其啤酒中瓜萎镰菌醇(呕吐毒素)的研究

本研究用带有波长为220nm的紫外.可见光探测器的高效液相色谱测定土耳其啤酒中瓜萎镰菌醇(DON)的污染水平.样品的乙腈-水(21+4,v/v)萃取物在装满氧化铝.硅藻土-木炭(0.50克+0.25克+0.60克)的萃取柱中洗脱,且柱芯用乙腈-水(21+4,v/v)预洗过,C18固相萃取柱用作第二次洗脱.DON的最低检出量是125μg/L(2.5ng的加入量).从市场上收集的50种啤酒样品都不含有检出量的DON.对于含有已知量(1mg/L)DON的啤酒,市场返回率是83.2%(SD 5.44,n=5).在土耳其消费的啤酒样品中检测到DON的存在,这是一项开创性的研究.     

盐酸法和β-葡萄糖苷酶法水解橄榄叶提取物制备羟基酪醇的比较

采用盐酸和β-葡萄糖苷酶分别水解橄榄叶提取物制备羟基酪醇。通过单因素实验和正交实验得出了酸水解的较优参数为:时间6h、温度80℃、盐酸浓度为0.2mol/L、液料比为50∶1(mL/g)。酶水解的最佳工艺参数为:温度50℃、时间5h、pH7.0、加酶量25U/mg。通过酶解的方法羟基酪醇最高含量为3.91%,而酸解的羟基酪醇最高含量为7.83%。从生产成本和提高羟基酪醇含量考虑,盐酸法优于酶法。     

代谢工程改造大肠杆菌增产酪醇

酪醇是橄榄苦苷、红景天苷和羟基酪醇等许多重要价值天然产物的前体物质,建立一个酪醇高产的平台菌株具有重要意义。由于大肠杆菌(Escherichia coli)具有繁殖速度快、易于基因操作等优点,该研究选择E.coli BL21 (DE3)作为宿主菌株。通过在质粒pRSFDuet-1中应用组成型启动子P_cspA过量表达来自荷兰芹的芳香醛合成酶(aromatic aldehyde synthase, AAS),得到105.97 mg/L酪醇。在敲除苯丙氨酸竞争途径(pheA)、丙酮酸竞争途径(ptsG、crr、pykF)及对羟基苯乙酸(feaB)竞争途径以及解除反馈抑制(tyrR)的菌株中过量表达AAS,获得1 055.36 mg/L酪醇。为了进一步强化代谢流,对E.coli来源的乙醇脱氢酶AdhE、AdhP、YahK及FrmA和酿酒酵母来源的Adh6进行了筛选。结果表明,酿酒酵母来源的Adh6表现最佳的脱氢酶活性,产生了1 516.86 mg/L酪醇,产量提升了43.73%。基于启动子组合调控策略平衡代谢流,酪醇产量达到1 810.46 mg/L,提升了19.40%。...     

高效液相色谱法测定β-酪啡肽

以SinoChrom 300A C8柱为分离柱,对高效液相色谱法测β-酪啡肽进行了研究.结果表明,以水(内含体积分数为0.1%TFA)和体积分数95%乙腈(内含体积分数为0.1%TFA)分别为流动A相和B相,在梯度洗脱流速1.0 mL/min,检测波长215 nm条件下,β-酪啡肽-5和β-酪啡肽-7被有效分离且具有较大的响应值,峰面积和保留时间具有良好的稳定性.同时在β-酪啡肽-5和β-酪啡肽-7质量浓度分别为1.0 g/L和1.2 g/L时,进样体积与峰面积呈良好的线性关系(回归系数r分别为0.9950和0.9955).该法可快速准确分离分β-酪啡肽.     

油橄榄叶中羟基酪醇的提取及分离纯化

对油橄榄叶中的羟基酪醇进行提取及分离纯化。采用酶法对油橄榄叶中的羟基酪醇进行提取,大孔吸附树脂分离纯化。通过单因素实验和正交实验得到酶法提取羟基酪醇的最佳工艺为:酶解时间80 min,pH值为7,温度40℃,酶浓度为30μg/mL,在此条件下得到的羟基酪醇含量为3.72 mg/g。静态吸附实验筛选出DA-201大孔吸附树脂为分离纯化羟基酪醇的最佳树脂,动态吸附-脱附实验得到羟基酪醇分离纯化的最佳工艺为:上样液质量浓度为60μg/mL,上样流速为3 BV/h,脱附剂为体积分数80%的乙醇,脱附流速为3 BV/h,脱附剂用量为2 BV。按照以上最佳实验条件操作,1 g油橄榄叶可得到羟基酪醇总油状物为3.85 mg,纯度为87.01%。     

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