液相色谱-串联质谱法测定百日咳和百白破疫苗中百日咳杆菌气管细胞毒素

百日咳杆菌气管细胞毒素（TCT）是一种引起百日咳及百日咳相关疫苗不良反应的毒性糖肽。尽管各国药典均规定了百日咳疫苗产品中TCT的含量限度，但均没有推荐TCT的含量测定方法。该研究发展了一种液相色谱-串联质谱法用于TCT的含量测定。实验优化了包括色谱柱类型和流动相组成在内的TCT色谱条件。虽然TCT在反相色谱模式和亲水作用色谱（HILIC）模式下均具有较好的保留，但HILIC模式与蛋白质沉淀的前处理方法兼容性更好，因此采用HILIC模式分离TCT。优化所得的方法具有较宽的线性范围（5.76~369 ng/L），良好的重复性（峰面积的相对标准偏差不大于3.9%），各种基质中均有较好的回收率（96.4%~102.5%），且定量限是药典要求的TCT最高限量的1/1279。将本方法用于共纯化百日咳疫苗、组分百日咳疫苗、共纯化无细胞百白破疫苗和组分无细胞百白破疫苗中TCT的检测，所有产品均未检出TCT，表明被检样品具有较好的工艺条件可避免TCT在产品中的残留。     

用于筛膜反应器的γ-MnO_2纳米粉的合成

醋酸锰与柠檬酸发生沉淀反应生成锰配合物,经热分解和酸处理手段最终制备出γ-MnO2纳米材料,用X射线衍射、差热/热重分析、透射电镜及原子力显微镜等手段对合成的样品进行了表征.同时考察了反应条件对反应速度、最终产品粒度的影响.结果表明,通过对反应条件的控制可以在一定程度上控制产品的粒度,得到了均粒度和超细粒度的γ-MnO2纳米材料.对于异丙醇和环己烷等氧化脱氢反应,γ-MnO2纳米筛膜反应器与传统的固定床反应器相比反应物的转化率提高了20%.     

乳状液膜法制备超细碳酸钙

探讨了不同流动载体的煤油、司本 - 80与碳酸钠水溶液制成的乳状液的稳定性 .考察了外相氢氧化钙水溶液中Ca2 + 浓度、膜相磷酸三丁酯的量及乳水比等因素对Ca2 + 迁移率的影响 .经TEM测定 ,破乳后的沉淀颗粒粒径不超过 10 0nm .     

一维链状配位聚合物[Ag(bix)(NO3)(H2O)]n的合成和晶体结构

A one-dimensional (1D) Z conformation coordination polymer, [Ag(bix)(NO₃)(H₂O)]_n was obtained by the reaction between AgNO₃ and flexible ligand of 1,4-bis(imidazol-1-ylmethyl)-benzene under hydrothermal conditions. It crystallizes in triclinic with space group P1. The crystallographic data of the compound are: a=0.777 1(2) nm, b=1.043 4(3) nm, c=1.082 7(3) nm, α=71.403(4)°, β=80.946(5)°, γ=88.794(4)°. The 1D chainlike structure was connected by π-π interaction between phenyl rings, leading to a 2D layered network. The lattice water and the NO₃^- anions were involved between the layers, therefore the 2D layered structure further extended to an intricate 3D framework. CCDC: 257100.     

The structural characterization of some palladium (Ⅱ) complexes of 1,10-phenanthroline and amino acids by NMR spectroscopy

The complexes [Pd(phen)(aa)]Cl.3H2O, where phen is 1,10-phenanthroline and aa is the anion of glycine (gly), .DL-alanine (ala), DL-serine (ser) or DL-asparagine (asn), were synthesized and characterized by spectroscopies. The NMR signals were assigned completely on the basis of the double irradiation, 1H-1H COSY and 1H-13C COSY techniques. In the 1H NMR spectra of phen in the complexes, the signals of 2-H and 9-H show upfield shifts 0.8-1 ppm, while the signals of 4-H and 3-H show downfield shifts or almost no shift, as compared to the free phen ligand, and the signal of 4-H appears in the lowest field. The signals of ring B which is trans to the carboxyl group show significant upfield shifts as compared to those of ring A. The probable structures were described on the basis of a metal-non-bonded hydrogen interaction, trons effect and ligand-ligand interaction. There may exist three conformation isomers in the [Pd(phen)(asn)]Cl.3H2O complex at room temperature. The preferred conformation isomer is about     

层状K4Ag2Sn3S9·2H2O的溶剂热合成与表征

用溶剂热法合成了K4Ag2Sn3S9·2H2O,通过单晶X射线衍射、DSC、TG、IR和紫外漫反射光谱等手段对其进行了表征.结果表明,K4Ag2Sn3S9·2H2O属单斜晶系,P21/m空间群,a=0.78071(2)nm,b=2.73508(1)nm,c=1.05008nm,α=90°,β=103.87(6)°,γ=90°,Z=4.其层状结构内具有一维孔道,钾离子分离在层间及层内孔道中.     

甲烷与二氧化碳重整制取合成气反应的研究 (I)Sr_(1-x)La_xNiAl_(11)O_(19)催化活性表征

对具有磁铅石结构的Ｓｒ１－ｘＬａｘＮｉＡｌ１１Ｏ１９对甲烷与二氧化碳重整反应的催化活性、积炭量和稳定性进行了研究．不同还原温度下催化剂的ＸＲＤ和催化活性的实验结果表明，金属镍是ＣＨ４＋ＣＯ２重整反应的活性组分，金属镍含量越大，反应活性越高．反应后催化剂积炭量的分析结果说明，在相同镍含量和分散度的情况下，Ｌａ３＋离子对Ｓｒ２＋离子调变，可以降低催化剂的表面酸性，提高催化剂的抗积炭能力．ＬａＮｉＡｌ１１Ｏ１９是一种具有较好催化活性、稳定性和抗积炭性能的催化剂．     

用高分辨率电感耦合等离子体-原子发射光谱仪测定高纯铬中的杂质元素

本文报道了高分辨率、高灵敏度的顺序扫描型电感耦合等离子体原子发射光谱仪(ICPS-8100)在高纯物质分析中的应用。对元素分析线进行优化选择;采用轴向观测方式,对高纯铬中μg/g级的杂质元素As、Sn、Sb、Pb进行直接同时测定,分析结果令人满意。     

Locking Function of a Key Residue in Kinesin＇s Gating Mechanism

In kinesin＇s mechanochemical cycle, ATP＇s binding to the nucleotide-free leading head is exquisitely gated so that futile hydrolysis is effectively avoided, Experiments show that, when both kinesin heads bind to a microtubule~ ATP cannot bind to kinesin＇s leading head when the neck linker （NL） of this head has a backward orientation. How NL＇s backward orientation is maintained needs understanding on a structural basis. By using steered molecular dynamics and rrmtation simulations, we investigate the backward-pointing conformation of the leading head＇s NL under different inter-head tensions. We find that the NL cannot keep in a strict backward orientation solely by the inter-head tension. LYS325 （amino acid sequence in 2KIN） has an assistant locking function which locks the NL and β0 to the β-domain. This locking function has an enhanced positive cooperation with the inter-head tension. When the inter-head tension is weakened, this locking function can be broken, resulting in a loose backward orientation of the NL. The difference between the strict and loose backward orientation of the NL might be a crucial factor in the gating mechanism. These results are consistent with relevant experiments and proposals.     

熔盐热裂解大豆油的特性研究

以大豆油为原料,在ZnCl₂-KCl熔融盐体系中考察了进料速量、载气流量、反应温度及进料量对其热裂解的影响。采用气相色谱-质谱联用仪(GC-MS)表征生物油组成。结果表明,进料速量和载气流量主要通过改变大豆油的反应停留时间影响裂解效果。当进料速率为1.2 g/min及不通载气时,大豆油停留时间较长,裂解较充分;随着温度升高,生物油得率增大,含氧化合物含量及酸值上升;随着进料量增大,生物油得率稳定在70%左右,但脱羧效果有所下降。经过催化加氢,生物油性质得到了明显的改善,组分分布与0^#柴油分布大体相似。