基于DNA酶表面增强拉曼的皮蛋中痕量Pb2+检测方法

表面增强拉曼散射(surface enhanced Raman scattering,SERS)光谱法常被用于重金属离子的分析与检测。将SERS与适配体和DNA酶相结合,能更好地对痕量重金属进行检测分析。在pH 7.2的三羟甲基氨基甲烷(trihydroxymethyl aminomethane,Tris)-HCl缓冲液和0.09 mol/L NaCl条件下,单链DNA(ssDNA)和DNA酶在80℃杂交成双链DNA(dsDNA)。在dsDNA和混合溶液存在下,银纳米(silver nanoparticles,AgNPs)发生聚集,聚集的AgNPs与罗丹明6G(rhodamine 6G,Rh6G)作用,在613 cm~(-1)处出现较强SERS特征峰。Pb~(2+)可将dsDNA裂解切割,释放出ssDNA,形成比表面积和粗糙度均增大的AgNPs-ssDNA-Pb~(2+)大分子缔合物。随着Pb~(2+)浓度的增大,释放出的ssDNA增多,形成的AgNPs-ssDNA-Pb~(2+)增多,AgNPs-ssDNA-Pb~(2+)与Rh6G作用增强,导致613 cm~(-1)处的SERS峰强度增大。据此建立DNA酶SERS法测定痕量Pb~(2+)的新方法,在2.5×10~(-8) mol/L～7.5×10~(-7) mol/L Pb~(2+)之间,线性关系良好,Pb~(2+)最低测出浓度为1.0×10~(-8) mol/L。新方法用于检测皮蛋中的痕量Pb~(2+),相对标准偏差均在10%以内,回收率在99.5%～107.7%之间。     

共振散射光谱法测定牛奶中的四环素

在1.0×10~(-5) mol/L的盐酸溶液中,四环素可与Co~(2+)发生络合反应形成螯合阳离子,该阳离子再与带负电的铝试剂通过静电引力作用形成三元离子缔合物,从而使反应体系的共振散射强度显著增强。在最优条件下,体系的共振散射强度增加值(△I)与四环素浓度在2.0×10~(-7 )mol/L～1.5×10~(-5) mol/L范围内呈良好的线性关系,回归方程为△I=1.247×10~7c+16.44(c为Tc的浓度,mol/L),检出限为4.81×10~(-8) mol/L,相关系数为0.997 1,据此建立一种测定四环素的新方法。将该方法用于检测牛奶样品中的四环素,加标回收率在99.28%～101.70%之间。     

微波消解-流动注射化学发光法快速测定调味品中的微量铬

为快速测定调味品中的铬含量,以八角、白蔻、黑胡椒为样品,经微波程序消解后,用无水亚硫酸钠将Cr~(6+)还原成Cr~(3+),用流动注射化学发光体系测定调味品中的铬含量。结果表明:最佳条件下,铬在1.0×10-7~8.0×10-7 mol/L浓度范围内有良好的线性,相关系数r=0.9996。对1.0×10~(-13) mol/L Cr~(3+)测定的相对标准偏差RSD为3.2%(n=11),按3倍标准偏差计算的检出限为2.3×10-12 mol/L,八角、白蔻、黑胡椒中铬的质量比分别为14.97,23.13,39.28μg/g,加标回收率为91.84%~97.47%。该方法选择性好、快速灵敏,用于调味品中铬的测定,结果令人满意。     

基于聚丙烯酰胺分子印迹包金核壳纳米粒子对食用油中黄曲霉素B1的SERS检测

在金纳米粒子周围包覆聚丙烯酰胺黄曲霉素B1分子印迹聚合物,制得以金纳米为核,分子印迹聚合物为壳的核壳结构纳米粒子。黄曲霉素B1分子可以被聚丙烯酰胺壳层空穴特异性捕获,进入金纳米粒子等离子体共振磁场有效范围而实现黄曲霉素B1的SERS检测,检测线性范围为3×10~(-11)~3×10~(-4)mol/L,相关系数R~2为0.982,检测限达到3×10~(-11)mol/L。将建立的方法用于食用油样品中的黄曲霉素B1检测,黄曲霉素B1的含量在4.65×10~(-9)~4.98×10~(-5)mol/L之间,样品回收率为89.84%~101.24%,相对标准偏差为4.51%~13.11%。结果表明,本方法快速准确,操作简便,可以用于食用油中黄曲霉素B1的快速检测。     

8-羟基喹啉类荧光探针的合成及其对食品中Al~(3+)含量的检测

设计合成Al~(3+)荧光探针L(2-((E)-((2-(((E)-(4-硝基苯基)二氮烯基)苯基)氨基)乙基)亚氨基)甲基喹啉-8-醇),并利用元素分析、核磁、质谱等方法对探针结构进行表征。该探针在溶液中本身荧光很弱,但Al3+结合后荧光显著增强。由此,建立了一种测定Al~(3+)的新方法。该方法对Al~(3+)测定的线性范围为1×10~(-8)~1.4×10~(-6) mol/L,检出限为5.8×10~(-9) mol/L,相对标准偏差为5.89%,回收率在96.5%~105.9%之间,具有选择性好、灵敏度高、线性范围宽、操作简单等优点。     

纳米Ce-ZnO催化降解酸性染料条件优化及回收利用

掺杂稀土元素Ce制备纳米Ce-ZnO催化剂,以甲基橙溶液为酸性染料代表,对纳米Ce-ZnO催化降解甲基橙条件进行优化,并对催化剂的回收循环使用效果进行研究。在催化时间为3 h条件下,通过正交试验确定纳米Ce-ZnO催化降解甲基橙溶液的最佳条件为催化温度25℃,甲基橙溶液pH 2,催化剂添加量1.0 g/L。在最优催化条件下,纳米Ce-ZnO对3×10~(-5) mol/L甲基橙溶液的降解率达到90%左右,对不同浓度(1×10~(-5)、3×10~(-5) mol/L和5×10~(-5) mol/L)甲基橙溶液的降解均符合一级动力学方程。以聚偏二氯乙烯(PVDC)膜为载体,键合Ce-ZnO制备的Ce-ZnO/PVDC膜材料对3×10~(-5) mol/L甲基橙溶液的降解率提高到95%以上,且循环3次使用后对甲基橙溶液的催化降解率保持在70%左右。因此,纳米Ce-ZnO催化剂及其PVDC膜材料在降解酸性染料方面有进一步开发应用前景。     

纳米磁珠-电化学适配体传感技术检测牛奶中氨苄青霉素

为满足牛奶中氨苄青霉素高效检测的需要,以纳米磁珠为载体,适配体与氨苄青霉素特异性结合为基础,构建氨苄青霉素电化学适配体传感器。采用碳二亚胺交联法制备修饰有氨苄青霉素的磁珠,该磁珠可与待测样中的氨苄青霉素共同竞争反应体系中的适配体和辣根过氧化物酶,随后利用磁性玻碳电极将上述磁珠吸附于电极检测表面进行电化学测定。最佳条件下,该传感器在1.0×10－12～1.0×10－8 mol/L浓度范围内传感器响应电流与氨苄青霉素浓度呈现良好的线性关系,检测限可达1.0×10－12 mol/L。采用该方法测定市售牛奶样品中的氨苄青霉素,精密度和回收率满意。     

Fe~(3+)-H_2O_2-刚果红体系阻抑动力学光度法检测鱼肉中氟含量

在酸性介质中,痕量F-对Fe~(3+)催化H_2O_2化刚果红褪色反应有显著的抑制作用,且阻抑褪色的程度与氟离子含量呈良好的线性关系,由此建立了一种新阻抑动力学光度法测定微量氟离子含量的新方法。在最优化的反应条件下,氟含量在8.0×10~(-7)~2.0×10~(-5)mol/L内符合比尔定律,检出限为2.8×10~(-7)mol/L。该法用于鱼肉中氟离子含量的测定,回收率在95.50%~98.00%。     

CdTe量子点同步荧光法测定番茄中链霉素残留

采用水热法制备巯基乙酸修饰的CdTe量子点,基于链霉素对CdTe量子点同步荧光强度的增强效应,建立一种测定链霉素含量的同步荧光法,并对测定条件如缓冲溶液pH值、量子点浓度和反应时间进行优化。样品经甲醇超声提取后,加入含1.0mL CdTe量子点溶液(3.5×10~(-5) mol/L)和1.0mL Tris—HCl缓冲溶液(pH=6.0)的溶液中,室温反应10min后,测定反应体系在345nm处的同步荧光强度(Δλ=230nm)。结果表明,链霉素浓度在5.0×10-7~1.0×10~(-5) mol/L时与体系相对同步荧光强度存在良好的线性关系,相关系数为0.999 7,检出限为1.0×10~(-8) mol/L。该方法操作简单、快速、灵敏度高,可用于番茄样品中链霉素残留的测定。     

双硫腙修饰丝网印刷电极同时检测茶汤中的Cu(II)和Pb(II)

在乙酸-乙酸钠缓冲溶液(0.1 mol/L、pH 5.0)中,利用双硫腙修饰丝网印刷电极阳极溶出伏安法分别于-0.18 V、-0.76 V阳极溶出峰同时测定重金属离子Cu2+和Pb2+。通过优化测定条件,得到最佳参数为:双硫腙修饰量3μg、pH 5.0、富集电位-1.1 V、富集时间210 s。在此条件下,Cu2+和Pb2+浓度分别在1.0×10-10-1.0×10-5mol/L、1.0×10-10-1.0×10-6mol/L范围内与峰电流呈良好的线性关系(RCu=0.9991,RPb=0.9934),检测限分别为0.35×10-10mol/L、0.41×10-10mol/L。该方法简单、快速、灵敏,可用于检测茶汤中的Cu2+和Pb2+。     

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