Synthesis, Characterization and the Effect of Glucose-lowering of Guanidino Acid Oxovanadium（Ⅳ） Complexes

Two guanidino acid oxovanadium(Ⅳ) complexes have been synthesized. Preliminary tests in vivo have shown that the two title complexes all display lowering glucose activity in vivo to STZ-rats. The effect of glucose-lowering of guanidino acetic acid oxovanadium(Ⅳ) complex in vivo is higher than that of guanidino propanoic acid oxovanadium(Ⅳ) complex.     

超高效液相色谱-串联质谱法测定白芷中51种禁用农药的残留量

将白芷药材粉碎至通过孔径为(250±9.9)μm的网筛,并称取此白芷粉末样品2.00g于聚丙烯管中与水10mL混匀,再加入含1%(体积分数)乙酸的乙腈10.0mL,涡旋1min后加入无水硫酸镁4g和乙酸钠1g,剧烈振荡3min,离心5min,取其上清液5.0mL置于已盛有无水硫酸镁900mg、N-丙基乙二胺(PSA)450mg和硅胶300mg的净化管中,剧烈振荡5min使净化完全,离心5min。移取上清液3.0mL于40℃水浴中减压蒸缩至近干。加入50μg·L^-1的磷酸三苯酯内标溶液300μL,加入乙腈定容至1.0mL,经0.20μm滤膜过滤,取其滤液,按仪器工作条件进行超高效液相色谱-串联质谱法分析。选用Eclipse Plus C18色谱柱和以不同比例的(A)含10mmol·L^-1甲酸铵的0.1%(体积分数)甲酸溶液和(B)乙腈的混合液为流动相,按梯度洗脱程序对白芷中可能残留的51种禁用农药进行色谱分离,并在电喷雾离子源正、负离子(ESI+和ESI-)电离方式和动态多反应监测(dMRM)模式条件下进行串联质谱法测定。采用基质匹配标准曲线法定量。51种农药的质量浓度在一定范围内与其对应的峰面积呈线性关系,并测得其检出限(3S/N)为0.3~5.0μg·kg^-1。标准加入法回收试验的结果显示,其中大部分农药的回收率在71%以上,测定值的相对标准偏差(n=6)均小于20%。按此方法分析了70批白芷样品,共检出16种农药,其中甲拌磷亚砜的检出率达95%,最高检出量为15.2μg·kg^-1;甲拌磷砜和毒死蜱的检出率均为10%,最高检出量依次为3.5,45.0μg·kg^-1,其余13种农药的检出率均低于5%,且检出量均较低。     

Optimized Separation of Nine Xanthones by Microemulsion Electrokinetic Chromatography

A microemulsion electrokinetic chromatography method has been firstly used for the separation of the therapeutically important xanthones from Securidaca inappendiculata. The separation of the nine xanthones was systematically optimized with respect to pH, composition of microemulsion,addition of cyclodextrins, applied voltage and column temperature. Baseline separation was successfully achieved for the nine xanthones, which was also compared with that by micellar electrokinetic chromtography.     

桥联双（甲巯咪唑）化合物的合成和配位性能

研究了桥联双(甲巯咪唑)化合物(Ⅰ_a—Ⅳ_a、Ⅰ_b)的合成和配位性能。UV谱显示Ⅰ_a—Ⅳ_a与UO_2~(2+)离子(硬酸)配位,溶液中形成3:1的配合物。Ⅰ_b与Hg~(2+)、Au~(3+)离子(软酸)配位形成2:1的配合物,用CNDO/2方法计算了各配体分子中原子净电荷密度和HOMO、LUMO能量。     

Ce0.8Y0.2O1.9-Ca3(PO4)2-K3PO4复合电解质在中温区的质子导电性及在常压合成氨中的应用

A precursor of Ce_0.8Y_0.2O_1.9(YDC) solid electrolyte was synthesized by the gol-gel method. YDC and phosphates powders were prepared by mixing the YDC and phosphates according to different weight ratios. The mixtures of the YDC and binary phosphates were ground and sintered at 1 400 ℃. The proton conductivity in solid electrolyte of the sintered samples was examined using electrochemical methods at 400～800 ℃. Ammonia was synthesized from nitrogen and hydrogen at atmospheric pressure in the solid state proton conducting cell reactor. The optimal condition for the ammonia production was determined. The result indicated that composite electrolyte of 80wt% YDC: 20wt% binary phosphates as proton conductor could obtain the highest ionic conductivity and ammonia production rate among the four samples, the rate of evolution of ammonia was up to 9.5 × 10^-9 mol·s^-1·cm^-2.     

A New Kind of Void Soap-free P（MMA-EA-MAA） Latex Particles

Soap-flee P(MMA-EA-MAA) particles with narrow size distribution were synthesized by seeded emulsion polymerization of methyl methacrylate (MMA), ethyl acrylate (EA) and methacrylic acid (MAA), and large voids inside the particles were generated by alkali posttreatment in the presence of 2-butanone. Results indicated that the size of void and theparticle volume were related with the amount of 2-butanone. The generation mechanism of voids was proposed.     

中孔分子筛SO42-/Zr-MCM-41催化裂解聚丙烯反应研究

采用水热合成法制备了不同硅锆比的中孔分子筛Zr-MCM-41,用强酸性基团SO42-对其进行修饰,制得SO42-/Zr-MCM-41中孔分子筛.采用XRD、FT-IR、NH3-TPD及氮气吸附脱附等技术对其结构和酸强度进行表征.通过改变硅锆比、负载不同的酸性基团对Zr-MCM-41的酸性进行调变,并将其用于催化聚丙烯(PP)的裂解反应,结果表明S i/Zr=40的SO42-/Zr-MCM-41具有较好的催化裂解活性.另外,与热裂解以及HZSM-5和Zr-MCM-41为催化剂时PP的裂解反应结果进行了比较,结果证明SO42-/Zr-MCM-41不仅具有较高的裂解转化率,而且具有较高的液体产物收率,适宜于空间位阻较大的PP的催化裂解反应.     

含噁二唑单元共轭聚合物合成与性质研究

单体 2 ,5 双 (4 溴苯 ) 1,3,4 二唑 (M Ⅰ )与 1,4 二乙烯基 2 ,5 二正丁氧基苯 (M Ⅱ ) ,在钯催化下通过Heck偶合反应合成得到共轭聚合物 ;单体和聚合物进行了1 H NMR ,1 3C NMR、质谱、FT IR、UV、荧光光谱、GPC、元素分析、热分析等测试 ;二唑 (OXD)基团是一种很好的生色团 ,对氧和热特别稳定 ,二唑环的亲电子性能使其特别适合于作为电子传输层 ,聚合物能发射很强的绿色荧光 ,它将是一类潜在的光电高分子材料     

马来酸酐封端聚碳酸亚丙酯的大分子偶联反应

自从 1 969年井上祥平[1] 发现二氧化碳 (CO2 )可以同环氧化合物直接共聚合成脂肪族聚碳酸酯(APC)以来 ,这一学科领域受到科学家的广泛关注[2～ 8] .这是因为CO2 所产生的温室效应 ,成为使全球变暖的主要因素[9,10 ] .已经确定CO2 使气侯变暖占诸多因素中的 66% .目前大气中CO2 的体积浓度为 345ppmv,由于人类的各类活动每年以 1ppmv的速度递增 .因此 ,降低CO2 排放量已成为全人类共同关注的热点之一 .另一方面 ,CO2 的固定化以及消耗、利用显然是一个应积极鼓励的研究课题 .目前人们已经将CO2 同环氧乙烷 (EO)、环氧丙烷 (PO)、环…     

毛细管气相色谱法分离分析二甲砜和二甲亚砜

采用毛细管气相色谱法对间接电氧化法合成的二甲砜及反应物二甲亚砜进行了分离分析。研究了分离二甲砜、二甲亚砜的最佳条件，内标法定量。两种化合物的线性范围在2－30μg，且有较好的精密度。