Liquid-liquid extraction pretreatment samples method used for pharmacokinetic study of rhubarb in rats after oral administrated

Objective:Pretreatment of biological samples is the most critical step in pharmacokinetic studies,especially pre-treatment of plasma samples.The pretreatment of biological samples in pharmacokinetic study of Traditional Chinese Medicines (TCM) is difficult due to the complexity of the ingredients.An organic solvent system ethyl acetate:acetone (10:1) solution used for liquid-liquid extraction has been developed in this study and compared with the commonly used protein precipitation method.Methods:Rats,Beagle dogs and humans plasma samples were adopted in this study in order to demonstrate the universality of the pretreatment method.Feasibility of this pretreatment method was also verified through its application to the pharmacokinetics of rhubarb in rats.Results:According to the results of extraction recovery matrix effect,it was indicated that the liquid-liquid extraction methods with new organic solvent might be suitable for variety of structures of compounds and various types of plasma samples.The pharmacokinetic study result showed that the developed pretreatment method could successfully be used for simultaneous determination of three active compounds modin,emodin-8-O-β-D-glucopyranoside (EDG) and rhein in rat plasma with high sensitivity,accuracy,and recovery by liquid chromatography tandem mass spectrometry (LC-MS/MS).Conclusion:The pretreatment method of liquid-liquid extraction methods with new organic solvent could be successfully applied for multi-component pharmacokinetics of TCM.

反萃沉淀法制备草酸铜超细粉体

采用反萃沉淀法,以H2C2O4-乙醇水溶液反萃CCl4-TOA-CuCl2组成的有机相中的铜离子,利用相界面传质反应过程获取CuC2O4超细粉体。采用X射线衍射分析、电子显微分析(SEM和TEM)、激光粒度分析等手段,考察了有机相铜浓度、反萃液中乙醇的浓度、反萃温度以及反萃时间等操作条件对草酸铜超细粉体的粒径和形貌的影响。结果表明,在反萃沉淀过程中,有机相中铜浓度、反萃液中乙醇浓度、反萃温度对草酸铜沉淀颗粒的粒径和粒径分布影响较大,反萃时间的影响小;在适宜条件(有机相中TOA40%(体积比)和Cu2+浓度0.1mol/L,反萃液中草酸浓度0.1mol/L和乙醇浓度80%(体积比),反萃温度15℃以及反萃时间2h)下,可制备粒径约100nm的草酸铜超细粉体,粉体为蓝青色单斜晶系结构的球形颗粒。

微囊引发剂控制聚合凝胶体系成胶实验研究

就地聚合凝胶是改善油藏非均质性的重要手段之一。针对就地聚合凝胶体系成胶时间过快,以聚乙烯醇缩丁醛为壁材,乙醇与水混合液为溶剂,采用界面沉淀法制备了以过硫酸铵为活性芯的微囊延迟成胶剂,并对微囊调控就地聚合凝胶体系成胶时间的性能进行研究。将0.05%聚乙烯醇缩丁醛的乙醇溶液与含有过硫酸铵和0.6%复配稳定剂(OP-10和吐温80)的水溶液按体积比7∶3混合,可制得平均粒径0.7~1.5μm的微囊引发剂,其中水中过硫酸铵的最佳质量浓度为0.2%~0.4%。在40~90℃条件下,通过调节微囊引发剂加量,可使就地聚合凝胶体系成胶时间大于30 h。岩心评价实验表明,微囊引发剂能顺利注入平均渗透率为50×10^-3μm^2的岩心中,并引发就地聚合凝胶体系聚合成胶,产生有效封堵;非均质驱油实验表明,凝胶封堵后可提高采收率20.24%。

四氢萘为良溶剂液/液界面法制备多级C60晶体（英文）

采用液/液界面法制备了不同形貌的多级C60结构。以四氢萘作良溶剂,异丙醇、乙醇、甲醇作不良溶剂,通过优化实验条件,成功制备了形貌特殊、界面清晰的C60晶体结构。此晶体表面粗糙度能通过乙醇洗涤得到进一步提高。通过对晶体内部形貌的观察,证实了晶体的多级自组装结构。红外、拉曼光谱和热重分析表明晶体仅由C60组成,不含溶剂分子。在纳米尺度上,通过X-射线衍射证实了分子水平上C60分子按照面心立方结构方式排列。此法制备的多级结构C60晶体比高温转变、溶剂热处理等方法更为简易,为多级材料制备提供了一条新路径。

负载二茂铁的富勒烯C_(60)六边形片晶的制备及表征

利用液-液界面析出法在富勒烯C60和二茂铁(Fc)的甲苯-异丙醇体系中,成功地制备了负载Fc的富勒烯C60/Fc片晶。通过偏光显微镜(POM)、扫描电子显微镜(SEM)、红外光谱(IR)和拉曼光谱(Raman)、能谱(EDS)和X射线衍射分析(XRD)等对C60/Fc片晶的形貌结构、组分与元素分布以及晶型进行了表征。POM观察结果表明,C60/Fc片晶的形状近似于六边形,尺寸均匀,粒径约为10μm。SEM-EDS的观察分析结果发现,Fe元素均匀地分布在C60片晶的表面。IR和拉曼光谱分析表明,C60/Fc片晶中C60和Fc之间各自分别以分子状态存在。XRD结果表明,C60/Fc片晶为单斜晶型。