大豆中二硝基苯胺类除草剂多残留的气相色谱法定量检测及质谱确证

建立以凝胶渗透色谱法(GPC)和固相萃取法(SPE)及气相色谱法(GC)联用技术测定大豆中10种二硝基苯胺类除草剂(氟乐灵、乙氟灵、环丙氟、氯乙氟灵、仲丁灵、异乐灵、二甲戊乐灵、二硝胺、氨基丙氟灵和磺乐灵)多残留检测方法.目标农药经正己烷饱和的乙腈提取,凝胶渗透色谱除去大豆中大部分油脂及色素,再经Florisil柱净化和富集,依次用6 mL二氯甲烷和6 mL二氯甲烷+丙酮(99+1)洗脱.目标农药采用电子捕获检测(GC/ECD),外标法定量,并经质谱(MS)确证.两个添加水平重复6次,回收率分别为74%～105%和59%～105%;相对标准偏差＜20%;检出限为1.8～7.6 μg/kg;定量限为6～38 μg/kg.     

三线性直接分解法分析高维灰色体系

对于由多个两维测量数据组成的三维阵，本文提出一种新三线性直接分解方法。采用高维ＰＣＡ分解，从三维阵中直接提取抽象光谱和抽象浓度，再结合ＱＺ算法，唯一地确定混合物中各组分光谱的浓度。该方法可以排除其它未知组分的干扰，适用于高维灰色体系定性定量分析和多点校准。用模拟数据讨论了光谱分离度对该方法的影响，应用于混合维生素Ｂ１、Ｂ２和Ｂ６的荧光分析，求得的光谱和浓度与实验值吻合很好。     

以Cyanex272为载体的乳状液膜迁移和分离铅的研究

用Ｃｙａｎｅｘ２７２－Ｓｐａｎ８０－甲苯乳状液膜体系研究了铅的迁移行为，确定了铅迁移的适宜条件。在此条件下，许多常见离子如Ｃｕ＾２＋、Ｃｏ＾２＋、Ｎｉ＾２＋、Ｃｄ＾２＋等均不迁移，Ｈｇ＾２＋迁移率很低。因此Ｐｂ＾２＋能与这些离子得到快速且完全的分离。这对分析测定及三废处理等工作具有实际意义。     

铁基超细粒子催化剂结构与还原行为的Mssbauer谱研究

铁基超细粒子催化剂具有优良的F-T反应性能。本工作利用原位Mssbauer谱辅以XRD技术研究了含有钾助剂的F-T合成铁基超细粒子催化剂的结构与还原行为,考察了催化剂组成和第二金属组分(Mn,Zn,Mg)的影响。“纯”铁超细粒子催化剂在氢气中很容易经Fe_3O_4还原为零价铁。第二金属组分的引入,一方面阻碍了催化剂的还原,另一方面稳定了Fe~(2+)的存在而使其成为还原的主要中间相,这有利于反应条件下形成类尖晶石结构的活性相。对于Fe-Mn催化剂,上述效应随锰含量的增加而更趋显著。铁基超细粒子催化剂在氢气中的还原能力依“纯”Fe>Fe-Zn>Fe-Mn>Fe-Mg的顺序递减,这在一定程度上反映了铁与第二金属组分之间相互作用的强弱。     

草酸锰分解过程的机理函数判别和动力学研究

用等温热重和线性升温热重分析法研究了草酸锰热分解过程,提出了判断其机理函数的3步判别法。经实验和理论分析证明,该反应受随机成核和晶核随后生长的过程(A_3a机理)支配,其活化能E=103.95 kJ/mol,频率因子A=4.448×10~8min~(-1).动力学补偿效应为IgA=0.09661E-1.2856     

毛蕊杜鹃挥发油化学成分研究

毛蕊杜鹃(Rhododendron tubulosum Ching ex wang wei-yei)系杜鹃花科杜鹃花属植物,分布于四川、西藏、甘肃和青海,其中青海分布最广,藏民常作为单方草药用于治疗肺炎和老年慢性气管炎,具有镇咳、祛痰作用,本文用自制的同时水汽蒸馏-溶剂萃取装置,从采自青海玉树州的毛蕊杜鹃鲜叶和嫩枝提取挥发油,用毛细管气相色谱-质谱和Kovats指数双重定性法对     

Deposition of Layer－by－layer Inorganic－organic Nano－hybrid Ultrathin Films onto SBA－15

Deposition of inorganic-organic nano-hybrid ultrathin films onto mesoporous silicate materials has been proven possible by using layer-by-layer assembly method. In combination with sol-gel method, titania, subsequently dye molecules (or polymer) were successfully fabricated onto the inner wall of SBA-15. Their structures were preliminarily characterized by FTIR and solid-state UV-Vis spectroscopy, thermal analysis, and BET surface area measurements,respectively.     

Synthesis of monodisperse poly(chloromethylstyrene-co-divinylbenzene) beads and their application in separation of biopolymers

The monodisperse, porous poly(chloromethylstyrene-co-divinylbenzene) beads of 7.9 microm were prepared by a single-step swelling and polymerization method. The seed particles prepared by dispersion polymerization exhibited good absorption of the monomer phase. Based on this media, a weak cation-exchange (WCX) stationary phase for HPLC was synthesized by a new chemically modified method. The prepared resin has advantages of biopolymer separation, high column efficiency, low column backpressure, high protein mass recovery, and good resolution for proteins. The dynamic protein-loading capacity of the synthesized WCX packings was 18.2 mg/g. Five proteins were separated in 3.0 min using the synthesized WCX stationary phase. The experimental results show that the obtained WCX resin has very weak hydrophobicity. The WCX resin was also used for the rapid separation and purification of lysozyme from egg white in 5.0 min with only one step. The purity and specific bioactivity of the purified lysozyme were found to be more than 93% and 70 245 U/mg, respectively.