2-亚甲基-1,3-丙二醇制备工艺研究

通过单因素试验筛选出DMF作为3-氯-2-氯甲基丙烯(CCMP)碱性水解制备2-亚甲基-1,3-丙二醇(MEPO)的溶剂.水解产物采用GC-MS联用仪、GC-900气相色谱仪进行结构分析,确定CCMP水解最佳工艺条件为:转速700 r/min,w(NaOH)=10%,温度92℃,V(CCMP)∶V(NaOH)=1∶5,m(DMF)∶m(CCMP)=0.2,反应时间6 h,在此条件下CCMP的水解率可达95%.     

低温合成三氯蔗糖-6-苯甲酸酯及其工艺优化

以蔗糖-6-苯甲酸酯为原料,建立了一种低温氯代合成三氯蔗糖-6-苯甲酸酯的方法。探讨了氯代剂的用量、助溶剂的用量、反应温度、反应时间和溶剂的用量等因素对反应的影响。最终确定了最优条件为n(vilsmeier试剂):n(蔗糖-6-苯甲酸酯)=9∶1、反应温度为100℃、反应时间11h、V(DMF):m(蔗糖-6-苯甲酸酯)=2∶1(mL∶g)、V(DMF)∶V(DMAc)=5∶1。在此条件下,可在低温合成三氯蔗糖-6-苯甲酸酯,且三氯蔗糖-6-苯甲酸酯的得率达68%。     

速灭杀丁的高效液相色谱分析法

速灭杀丁为中等毒性杀虫剂,通用名Fenvalerrt 其它名:杀灭菊酯,氰戊菊酯、戊酸氰醚酯。化学名称:α—氰基—3—苯氧基苄基—2—4(4—氯苯基)—3—基丁酸酯。化学结构式:     

抗癌药物拉帕替尼两个杂质的合成

目的合成抗癌药物拉帕替尼的两个杂质。方法以N-[3-氯-4-[(3-氟苄基)氧基]苯基]-6-碘喹唑啉-4-胺为起始原料,经Suzuki偶联反应,得到N-[3-氯-4-[(3-氟苄基)氧基]苯基]-6-[(5-甲酰基)呋喃-2-基]-4-喹唑啉胺,直接与还原剂NaBH(OAc)3反应,得到特定杂质N-[3-氯-4-[(3-氟苄基)氧基]苯基]-6-(5-羟甲基呋喃-2-基)-4-喹唑啉胺;起始原料经Suzuki反应后,与2-甲砜基乙胺反应,在NaBH(OAc)3作用下得粗品,经制备液相分离,得到另一特定杂质双[[5-[4-[[3-氯-4-[(3-氟苄基)氧基]苯基]氨基]喹唑啉-6-基]呋喃-2-基]甲基][2-(甲磺酰基)乙基]胺。结果两个目标物经质谱(MS),核磁共振氢谱(1H NMR)确证其化学结构。结论合成的两个杂质可作为拉帕替尼质量控制对照品,本工艺操作可行,原料易得。     

2-亚甲基-1,3-丙二醇制备工艺研究

通过单因素试验筛选出DMF作为3-氯-2-氯甲基丙烯（CCMP）碱性水解制备2-亚甲基-1,3-丙二醇（MEPO）的溶剂.水解产物采用GC-MS联用仪、GC-900气相色谱仪进行结构分析,确定CCMP水解最佳工艺条件为：转速700 r/min,w（NaOH）=10%,温度92℃,V（CCMP）∶V（NaOH）=1∶5,m（DMF）∶m（CCMP）=0.2,反应时间6 h,在此条件下CCMP的水解率可达95%.     

HPLC法定量分析微生物法制备液中产物γ-氨基丁酸和底物L-谷氨酸

建立一种测定微生物法制备液中γ-氨基丁酸(γ-aminobutyric acid,GABA)和L-谷氨酸(L-glutamic,L-Glu)的高效液相色谱法。样品经10%三氯乙酸溶液预处理后,用4 mmol/L氯甲酰芴甲酯进行柱前衍生。采用Phenomenex C18色谱柱(4.6 mm×250 mm,5μm),以A[50 mmol/L乙酸钠溶液(p H 4.8)-甲醇-乙腈-四氢呋喃(82∶8.5∶8.5∶1,V/V)]∶B[50 mmol/L乙酸钠溶液(p H 4.8)-甲醇-乙腈-四氢呋喃(22∶38.5∶38.5∶1,V/V)]=30∶70为流动相,流速1.0 m L/min,柱温40℃洗脱,检测波长265 nm。该方法稳定、灵敏、测定周期短、重复性好。在GABA和L-Glu质量浓度为20~400μg/m L范围内有良好的线性关系。与常用衍生剂邻苯二甲醛相比,衍生产物的稳定性更好,且无需梯度洗脱。     

2-氧代-2,3-二氢-1H-咪唑并[1,2-a]-吡啶鎓氯化物的合成

以2-氨基吡啶和氯乙酰氯为原料,合成2-(2-氯乙酰氨基)吡啶,进一步环合生成2-氧代-2,3-二氢-1H-咪唑并[1,2-a]-吡啶鎓氯化物.分别考察物质的量比、反应温度、反应时间对中间体及目标产物收率的影响.通过单因素试验,确定合成2-(2-氯乙酰氨基)吡啶的较佳工艺条件为:氯仿为溶剂,反应温度0℃,反应时间4 h,n(2-氨基吡啶)∶n(氯乙酰氯)=1∶1.5;合成2-氧代-2,3-二氢-1H-咪唑并[1,2-a]-吡啶鎓氯化物的较佳工艺条件为:乙腈为溶剂,反应温度75℃,反应时间12 h.利用1H-NMR和IR对中间体及目标产物结构进行了表征.     

皮革防霉剂OIT的包合缓释研究

实验研究了采用β-环糊精包合皮革防霉剂N-辛基-4-异噻唑啉-3-酮(OIT)的工艺.通过调整OIT与β-环糊精的质量比、包合时间、包合温度、溶剂混合比例,得到作为皮革缓释长效防霉剂的最佳包合条件:β-环糊精与OIT质量比为5∶1,包合时间1.5h,温度55℃,溶剂混合比例V(乙醇)∶V(水)=1∶2,此条件下可获得较高的包合率产物,并对产物进行了表征,证明了包合物的形成.     

薄层扫描法测定罗汉果糖苷(V)含量的研究

建立采用薄层扫描法测定罗汉果糖苷(V)含量的方法。点样于硅胶G板上,以正丁醇-乙醇-水(8∶2∶3)为展开剂,10 %硫酸乙醇显色,单波长反射法锯齿扫描,λ=5 0 0 nm。罗汉果糖苷(V)在2 .0～16 . 0 μg范围内具有良好的线性关系,r=0 .992 1,平均回收率为97.6 2 % ,RSD为2 .5 9% (n=4 )。该法简便快速、准确灵敏,可用于罗汉果糖苷生产质量监控。     

高沸醇溶剂法提取烟梗中木质素的研究

以1,4-丁二醇水溶液为溶剂,采用高沸醇溶剂法从烟梗中提取木质素.其最佳提取条件为:烟梗原料50 g(干质量),采用1,4-丁二醇水溶液(V(醇)∶V(水)=9∶1),固液比(g∶mL)为1∶10,加入少量浓H2SO4作为催化剂,在220℃下对烟梗进行蒸煮2 h,木质素收率最高.采用紫外光谱和红外光谱对其结构进行表征,结果表明,高沸醇溶剂法提取的烟梗木质素具有木质素类化合物的典型结构特征.     

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