裂解色谱法研究PMR型聚酰亚胺前体的反应过程

用裂解气相色谱法研究ＰＭＲ型聚酰亚胺前体在反应中的化学变化过程，以裂解产物醇和环戊二烯的生成率表示酰胺化或酰亚胺化及交联的程度，结果表明，酰胺化或酰亚胺化在５０℃以下不发生，在１８０～２２０℃完成，降冰片烯端基在１５０℃以下不发生交联反应，在２８０℃，１０～１８小时可完成交联反应。     

A Facile Synthesis of Ethyl 2,4-Dimethoxy-6-perfluoroalkyl-benzoates via Acyclic Precursors

Introduction Polysubstituted arenes are important intermediates in synthetic medicines and dyestuffs, and the fluorinated analogues are more attractive as a result of their lipo-philicity and the increment of activity.1,2 Therefore, to study the convenient and efficient synthesis of polysub-stituted arenes is valuable in organic synthetic method-ology. We have designed a simple synthesis of fluori-nated polysubstituted arenes through the intramolecular Wittig reaction of a new phosphorous ylid…     

短尾蝮新突触前毒素和细胞毒素的纯化及部分序列

用反相高效液相色谱技术对中国产短尾蝮蛇(Agkistrodon blomhoffii brevicaudus)毒中的毒性蛋白重新进行了纯化,结果从中获得了3个由约122个氨基酸残基构成的毒蛋白(AgTx-1,AgTx-2和AgTx-3)。三者对小鼠的LD_(50)分别为0.075,0.51和6.6mg/kg。在小鸡颈二腹肌标本上的毒理分析表明,AgTx-1和AgTx-2均在阻遏接头传递之后,亦不影响肌肉对乙酰胆碱的敏感性。在AgTx-3的作用下,标本的间接收缩则由于舒张不全而逐渐变小,最后停止在挛缩状态。部分氨基酸序列测定结果又表明,AgTx-1和AgTx-2的N-端32肽序列完全相同。考虑到AgTx-1的LD_(50)在粗毒中的含量及其序列等均与前文报道的β-AgTx极为相似,故我们认定它们为同一毒素,并定名为β_1-AgTx。而AgTx-2则应是新的突触前毒素,相应地定名为β_2-AgTx,至于AgTx-3便是新发现的细胞毒素。     

A new C21-steroidal glycoside from Cynanchum stauntonii

A new C21-steroidal glycoside with two known compounds were isolated from the root of Cynanchum Stauntonii.Based on thespectral analysis,including MS,1H NMR,13C NMR,DEPT,1H-1H COSY,13C-1H COSY,HMQC and HMBC,their chemicalstructures were determinated as glaucogenin-C 3-O-a-L-cymaropyranosyl-(1→4)-b-D-digitoxopyranosyl-(1→4)-β-D-canaropyranoside(1),stigmasterol(2)and ursolic acid(3).     

分子印迹技术在样品前处理中的应用

分子印迹聚合物具有选择性高、稳定性好及制备简单的特点,可用于生物、医药、环境样品等复杂基体中痕量分析物的高选择性分离与富集,因此在样品前处理中的应用特别引人关注.本文介绍了分子印迹技术的基本原理,综述了分子印迹技术在样品前处理中应用的研究进展.     

免疫亲和柱净化/柱前衍生化-高效液相色谱荧光检测法测定粮谷中的T-2毒素

建立了免疫亲和柱净化/柱前衍生化-高效液相色谱荧光检测器测定粮谷中T-2毒素含量的方法。样品经甲醇-水(体积比为80∶20)混合溶剂提取,通过免疫亲和柱(IAC)净化,以氰酸蒽(1-AN)为衍生化试剂、4-二甲基氨基吡啶(DMAP)为催化剂进行衍生,以ZORBAX Eclipse XDB-C18 柱为分离柱,乙腈-水(体积比为80∶20)为流动相进行高效液相色谱分离及荧光检测，荧光检测的激发波长为381 nm，发射波长为470 nm。T-2毒素的质量浓度为0.01~1.5 mg/L时与峰高呈良好的线性,相关系数为0.9985。在0.01~1.5 μg/g添加水平下，回收率为79.7%~94.5%,相对标准偏差小于7%；检出限（S/N＝3）为0.01 μg/g。该方法净化效果好,灵敏度高,操作简便快速。     

云南晋宁梅树村剖面前寒武系—寒武系界线化石Sm-Nd同位素年龄测定

本文首次采用化石Sm-Nd等时线方法测定了前寒武系—寒武系界线的年龄。样品采自云南晋宁梅树村剖面的中谊村段磷块岩。根据4个软舌螺化石样品得出的年龄值为距今562.8±7.9Ma;由这4个样品和2个胶磷矿样品获得的年龄值为562.1±5.7Ma,这些数据表明,略低于中谊村段的前寒武系-寒武系界线参考点A的年龄距今约为570Ma,而位于中谊村段近顶部的界线参考点B的年龄距今约为560Ma。该结果为准确标定寒武系底界在国际地质年表中的位置提供了重要依据。     

仪器信息网全新推出仪器行业一站式培训服务

仪器信息网6月份大改版后推出了全新的培训栏目（http：／／www．instrument．com．cn／training／），汇集各种仪器行业培训信息和资料，为您提供从培训信息查询到在线报名一站式培训服务，满足您各种培训需求。培训栏目由五个部分组成：     

Synthesis and Characterization of Fluoro- and Chloro- bimetallic Alkoxides as Precursors for Luminescent Metal Oxide Materials via Sol-Gel Technique

Heterobimetallic alkoxides are broadly recognized as versatile precursors for luminescence materials, and efforts are being made to develop novel routes by applying the concept of geometrical molecular design, for their synthesis and to design a single source precursor suited to photoluminescent materials. Novel and new series of bimetallic alkoxides has been prepared by metathesis route. They exhibit a lower sensitivity towards hydrolysis and so they are easier to handle as compared to other alkoxides. All the compounds were characterized by elemental analysis, FT-IR and multinuclear NMR spectroscopies. FT-IR revealed that the molecular structure of these metal alkoxides was retained to a large extent in 4 ： 1 halogenated alcohol-benzene solution. The heteronuclear NMR spectroscopy provided useful information about chemical shifts for better understanding the likely structure based on interactions with their coordinate metals. The mass spectra show similar types of fragmentation pattern. SEM-EDS analyses showed consistency with the formulation. XRD patterns show an enhanced homogeneity at high temperature. TGA measurements show that thermal decomposition occured in steps that depended entirely on the chemical compositions and the synthesis routes. SEM observation reveals that the morphology and particle size strongly depend on synthesis routes for their precursors.     

聚[2—甲氧基—5—（4—溴—丁氧基）对苯乙炔]新型前聚物的合成及…

采用不同方法由三铳盐合成新型的聚电解质前聚物及可溶于有机溶剂的侧链溴代聚对苯乙炔前聚物，发现侧链烷氧取代基上的铳盐并不参与聚合，所得前聚物加热都可转化为聚对苯乙炔。