毛细管电泳-柱端安培检测中分离毛细管与检测电极对接方式比较的研究

针对目前毛细管电泳中普遍采用的水平式和直立式两种柱端安培检测形式,在各种可能的对接角度下,以邻苯二酚、间苯二酚和对苯二酚3种二酚作为分离分析测试对象,对分离毛细管与检测电极的对接方式进行了优化比较,并对每一种对接方式的分析特性进行了测试。结果表明：在以3种典型的方式对接时,分离毛细管与检测电极为倒直立式对接时,获得的检测灵敏度最高,响应电流最大,水平式次之,直立式最小。     

固相萃取高效液相色谱-质谱法测定动物组织中硝基呋喃代谢产物

研究了对动物组织中4种硝基呋喃类代谢产物AOZ、AMOZ、SEM和AHD的自动固相萃取HPLC-MS分析方法，分别以2-氯苯甲醛和2-硝基苯甲醛作为衍生化试剂，分别用AMOZ-d5、AOZ-d4作内标，用ENSPE柱进行提取，以乙腈-0．1％甲酸为流动相，采用梯度洗脱，可在15min内将4种代谢产物完全分离并进行测定。回收率为85％-90％；检出限可达0．5μg／kg。采用两种衍生化方法可获得较多的定性确证信息。采用本方法研究了硝基呋喃在鸡饲养过程中的残留规律。     

5-(取代吡唑基-4-次甲基)(硫代)巴比妥酸的合成

以冰乙酸为催化剂,将取代吡唑甲醛和巴比妥酸或硫代巴比妥酸在无水乙醇中进行Knoevenagel缩合反应,合成了6个5-（取代吡唑基-4-次甲基）（硫代）巴比妥酸。标题化合物经IR、1^HNMR、元素分析确证结构。     

高效液相色谱法检测鳗鱼中氟苯尼考残留量

建立了鳗鱼肌肉中氟苯尼考残留的分析方法。采用乙酸乙酯作为提取剂,提取液挥干后溶于缓冲液中,经正已烷脱脂、C18SPE小柱净化后,采用高效液相色谱进行分析,方法在1～200ng之间呈线性相关;相关系数r=0．9999。对于0．05、0．10、0．50mg／kg 3个添加水平,平均回收率均在90％以上,相对标准偏差为4．24％～7．36％,方法检出限和定量限分别为9．1μg/kg和22．3μg／kg。     

臭氧发生器所产生气体中氮氧化物的HPLC法测定

基于氮氧化物溶于水生成HNO2和HNO3的反应,采用NaOH溶液收集氮氧化物,用高效液相色谱法测定氮氧化物,并用分光光度法作对比。结果表明,分光光度法所测结果偏低,高效液相色谱法更准确而且简便、快速,选择性好。     

纳米钯膜电极的制备、结构表征和特殊反应性能

用循环伏安方法制备纳米钯膜电极,运用扫描隧道显微镜和原位红外光谱等方法研究其结构和反应性能.STM图像表明,制备的纳米钯膜具有特殊的层状结构,纳米级厚度的层状晶体由直径6nm左右的Pd微晶聚集而成.发现当钯膜厚度为几个纳米时,CO的吸附表现出异常红外效应,即红外谱峰反向和红外吸收显著增强(增强因子可达42.6).纳米钯膜电极对氢的反应也具有特殊的性能,与氢向钯晶格扩散吸收过程相比较,氢吸脱附的表面过程成为主要反应.研究结果还指出,纳米钯膜电极的异常红外效应和对氢反应的特殊性能与钯膜厚度密切关联,并可归结为钯膜材料的纳米尺度效应.     

Making High Selective Molecule Imprinting Polymer (MIP) In Polar Solvent

IntroductionMoleculeimprintingtechnologyhasmadegreatprogressinmakingchiralstationaryphasewithpredeterminedchiralselectivityagainstenantiomerssuchasaminoacidandtheirderivatives;sugarandtheirderivatives;naproxenandmethylbenZylamine'-'.Functionalmonomer...     

VISIBLE LIGHT PHOTOPOLYMERIZATION OF METHYL METHACRYLATE COINITIATED WITH TITANOCENE AND KETOCOUMARIN DYE*

The photosensitive system which can initiate methyl methacrylate with visible light was composedof compound 1 bis(η-5-cyclopentadienyl)-bis[2,6-difluoro-3-(1-H-pyrrolyl)phenyl]titanium (titanocene) andcompound 2 [(3,3'-carbonylbis(7-diethylamino coumarin)] (ketocoumarin dye). The high photosensitiveinitiating efficiency of this photosensitive system could be very promising for efficient system for laser (Ar~+488 nm) to plate and photocuring for thick coating and ink. The variation of UV-visible spectrum ofcompound 2 during irradiation indicates that photolysis of compound 2 is through its triplet state and it canbe quenched by O_2. The much quicker photobleaching of the photosensitive system suggests that there existscertain quick electron transfer reaction between compounds 1 and 2.     

DYE-SENSITIZED PHOTOPOLYMERIZATION OF METHYL METHACRYLATE INITIATED BY COUMARIN DYE/IODONIUM SALT SYSTEM*

The photosensitive initiating system composed of 7-diethylamino-3-(2'-benzimidazolyl)coumarindye (DEDC) and diphenyliodonium hexafluorophosphate (DIHP) which act as the sensitizer and the initiatorrespectively, can be used to initiate the polymerization of methyl methacrylate (MMA). The results showedthat when exposed to visible light, coumarin dye/iodonium salt undergoes quick electron transfer from DEDCto DIHP and free radicals are produced. The visible light photoinduced reaction between DEDC and DIHP ismainly through the excited singlet state of DEDC and thus it is a little sensitive to O_2. The influence ofconcentration of DEDC, DIHP and MMA on the rate of photopolymerization of MMA was also investigated.     

硅烷接枝聚乙烯储存稳定性的研究

利用熔体流动速率测定仪进行了硅烷接枝聚乙烯的水解缩合交联反应的加速试验,发现该反应对水分浓度为一级反应,反应的表现活化能４２ｋＪ／ｍｏｌ,由此可推算Ａ组份的保存期。当催化剂存在时,水解缩合反应明显加快,这时的表观活化能降到２０ｋＪ／ｍｏｌ。