A validated spectrofluorometric method for the determination of celecoxib in capsules

A rapid, selective, sensitive and simple fluorescence method was developed for the direct determination of celecoxib in capsules. The capsules were emptied, pulverized and dissolved in either ethanol or acetonitrile, sonicated and filtered. Direct fluorescence emission was measured at 355±5 nm (exciting at 272 nm). The method was fully validated and the recoveries were excellent, even in presence of excipients.     

Effect of Oxalic Acid on Stabilization and Property of Sb-Doped Tin Oxide Sol

Zeta potential studies show that the ATO nanoparticle surface is positively charged in pH range from 2 to 5 without oxalic acid. The addition of oxalic acid brings a charge reversal on the surface of ATO particle in a wide pH range. The interaction of oxalic acid with surface of ATO nanoparticle was studied by FTIR and indicates that the most probable mechanism is the formation of Sn-O-C bonds via the condensation reaction between the oxalic acid and surface hydroxyl groups. TEM, X-ray diffraction and UV-Vis-Near IR spectra were used to characterize the nanocrystalline ATO sol and thin gel film.     

Metal components analysis of metallothionein-III in the brain sections of metallothionein-I and metallothionein-II null mice exposed to mercury vapor with HPLC/ICP-MS

Mercury vapor is effectively absorbed via inhalation and easily passes through the blood–brain barrier; therefore, mercury poisoning with primarily central nervous system symptoms occurs. Metallothionein (MT) is a cysteine-rich metal-binding protein and plays a protective role in heavy-metal poisoning and it is associated with the metabolism of trace elements. Two MT isoforms, MT-I and MT-II, are expressed coordinately in all mammalian tissues, whereas MT-III is a brain-specific member of the MT family. MT-III binds zinc and copper physiologically and is seemed to have important neurophysiological and neuromodulatory functions. The MT functions and metal components of MTs in the brain after mercury vapor exposure are of much interest; however, until now they have not been fully examined. In this study, the influences of the lack of MT-I and MT-II on mercury accumulation in the brain and the changes of zinc and copper concentrations and metal components of MTs were examined after mercury vapor exposure by using MT-I, II null mice and 129/Sv (wild-type) mice as experimental animals. MT-I, II null mice and wild-type mice were exposed to mercury vapor or an air stream for 2 h and were killed 24 h later. The brain was dissected into the cerebral cortex, the cerebellum, and the hippocampus. The concentrations of mercury in each brain section were determined by cold vapor atomic absorption spectrometry. The concentrations of mercury, copper, and zinc in each brain section were determined by inductively coupled plasma mass spectrometry (ICP-MS). The mercury accumulated in brains after mercury vapor exposure for MT-I, II null mice and wild-type mice. The mercury levels of MT-I, II null mice in each brain section were significantly higher than those of wild-type mice after mercury vapor exposure. A significant change of zinc concentrations with the following mercury vapor exposure for MT-I, II null mice was observed only in the cerebellum analyzed by two-way analysis of variance. As for zinc, the copper concentrations only changed significantly in the cerebellum. Metal components of metal-binding proteins of soluble fractions in the brain sections were analyzed by size-exclusion high-performance liquid chromatography (HPLC) connected with ICP-MS. From the results of HPLC/ICP-MS analyses, it was concluded that the mercury components of MT-III and high molecular weight metal-binding proteins in the cerebellum of MT-I, II null mice were much higher than those of wild-type mice. It was suggested that MT-III is associated with the storage of mercury in conditions lacking MT-I, and MT-II. It was also suggested that the physiological role of MT-III and some kind of high molecular weight proteins might be impaired by exposure to mercury vapor and lack of MT-I and MT-II.     

聚乙烯单晶的退火效应

用混合晶红外光谱法和ＳＡＸＳ、ＤＳＣ和ＬＡＭ等方法研究了聚乙烯单晶在７５℃、９０℃和１０５℃退火前后的结构变化，发现在９０℃以下和１０５℃以上退火，遵循不同的退火机制     

(4S)-4-羧基杂氮硅三环的合成

利用L-N,N-双(β-羟乙基)丝氨酸及L-N,N-双(β-羟乙基)苏氨酸与三乙氧基硅烷或氯烷基三乙氧基硅烷反应合成了具有手性的(4S)-4-羧基杂氮硅三环(1～5),并运用IR、~1HNMR、EI-MS等手段表征了结构。证据显示存在着贯穿笼状结构的N→Si配键。     

（±）—Salvinolone的全合成研究

以２－（３，４－环己基类二氧－５－异丙基）苯基乙醇（２）和３－异丙氧基－５，５－二甲基－１，３－环己烯酮（４）为原料，利用羰基α－位的烷基化反应和分子内的Ｆｒｉｅｄｅｌ－Ｃａｒｆｔｓ反应为关键步骤，经９步反应，合成了多氧芳香型三环二萜类天然产物Ｓａｌｖｉｎｏｌｏｎｅ。     

付里叶变换红外光谱仪的操作参数对光谱的影响

本文以二苯基甲酮的ＫＢｒ压片为标样，在Ｂｒｕｋｅｒ ＩＦＳ １２０ＨＲ付里叶变换红外光谱仪上系统考察了该仪器折一些重要操作参数（光源光栏、切趾函数、扫描速度）对光谱质量（信噪比，分辨率）的影响。从而获得了测样时的优化操作条件。     

硅氧化合物化学蒸气沉积法精细调变沸石分子筛

本文报告了用化学蒸气沉积法精细调变沸石孔径的结果，着重考察了正硅酸乙酯和六甲基硅醚沉积条件的关系。间二甲苯和均三甲苯的吸附动力学实验表明，用Ｓｉ－（ＯＥｔ）４制得的ＳｉＨβ和ＳｉＨＺＳＭ－５上的吸附速率及吸附量明显下降，证实沸石的孔口得到了调变。正己烷的吸附等温线和异丙醇探针反应，沸石孔容和孔道内酸性未受孔口调变的影响。结果还表明Ｓｉ（ＯＥｔ）４未进入沸石孔道，而六甲基硅醚分子则进入Ｈβ沸石孔道，