Method development for the quantitation of ABT-578 in rabbit artery tissue by 96-well liquid-liquid extraction and liquid chromatography/tandem mass spectrometric detection

Quantitative determination of drug concentrations in tissue samples can provide critical information for drug metabolism, kinetics, and toxicity evaluations. For analysis of tissue samples using liquid chromatography/tandem mass spectrometric (LC/MS/MS) detection, homogenization is a critical step in achieving good assay performance. Assay performance can be closely evaluated by spiking the drug directly into tissue samples prior to homogenization. It is especially important to include this assay evaluation for the analysis of artery tissue samples because artery tissue is very elastic, making it quite a challenge to develop an effective procedure for homogenization. An LC/MS/MS assay in 96-well format using liquid-liquid extraction was developed for analyzing ABT-578 in rabbit artery samples. Tissue quality control samples were prepared by spiking ABT-578 stock solutions directly into the tissue before homogenization. The usage of the tissue control samples gives a thorough evaluation of the sample preparation process that includes both homogenization and sample extraction. A 20% blood in saline solution was used as a homogenization solution. Calibration standards were made by spiking ABT-578 into rabbit whole blood. Blood quality control samples were also prepared by spiking ABT-578 into rabbit whole blood. These blood QC samples were used to confirm the validity of the calibration curve. A lower limit of quantitation of 0.050 ng/mL was achieved. The linear dynamic range of blood standards was from 0.050-30.3 ng/mL with the correlation coefficient (r) ranging from 0.9969-0.9996. Overall %CV was between 1.3 and 7.0%, and analytical recovery was between 98.2 and 105.8% for blood QC samples. The %CVs for tissue QC samples were between 6.7 and 13.0%, and analytical recovery after correction was between 93.5 and 114.3%.     

A light-driven rotaxane molecular shuttle with dual fluorescence addresses

[reaction: see text] A molecular shuttle containing an alpha-CD macrocycle, an azobenzene unit, and two different fluorescent naphthalimide units was synthesized. The cis-trans photoisomerization of the azobenzene unit resulted in the motion of the CD macrocycle on the track. Because of the easy regulation and full reversibility of the fluorescence change of the two stopper units, the molecular shuttle could be used as a molecular storage medium or switch with all-optical inputs and outputs.     

我国古代的炭黑生产及法家科学家的贡献

炭黑是现代石油化工重要产品之一。我们伟大的祖国,是世界上生产炭黑最早的国家。远在原始公社时期,我们的祖先在长期的生产实践中已掌握了在不完全燃烧的情况下产生炭黑(烟炱)的操作技术,用来熏染陶坯,生产精美的黑陶。炭黑生产技术的发展,与我国古代文字的产生、纸的发明及印刷术的发展等辉煌成就有着密切的联系。上古时期制墨,以天然石墨为主,后来就被更为优越的松烟炭黑所代替。汉朝时曾有过许多关于墨的记载。公元100年出版的我国最早的一本字典《说文     

Identification of differentially expressed proteins between human hepatoma and normal liver cell lines by two-dimensional electrophoresis and liquid chromatography-ion trap mass spectrometry

In the previous study, the proteomes of the human hepatoma cell line BEL-7404 and the normal human liver cell line L-02 were separated by high resolution two-dimensional electrophoresis (2-DE). Image analysis revealed that 99 protein spots showed quantitative and qualitative variations that were significant (P < 0.01) and reproducible. Here we report the identification results of some of these protein spots. Protein spots excised from 2-D gels were subjected to in-gel digestion with trypsin, and the resulting peptides were measured by microbore high performance liquid chromatography - ion trap - mass spectrometry (LC-IT-MS) to obtain the tandem mass (MS/MS) spectra. Twelve protein spots were identified with high confidence using SEQUEST with uninterpreted MS/MS raw data. Besides inosine-5'-monophosphate dehydrogenase 2, heat shock 27 kDa protein, calreticulin and calmodulin, whose expression was elevated in hepatoma cells, glutathione-S-transferase P was identified from hepatoma cells in which its level was 18-fold higher compared to human liver cells. Two spots were identified as the homologs of reticulocalbin for the first time in hepatoma cells and their expression increased compared to liver cells. However, tubulin beta-1 chain and natural killer cell enhancing factor B were downregulated in hepatoma cells. A tumor suppressing serpin, maspin precursor, was identified from one spot whose quantity was much higher in the normal liver cell line. More interestingly, epidermal fatty acid-binding protein (E-FABP) and fatty acid-binding protein, adipocyte-type (A-FABP), were detected in liver cells but not in hepatoma cells. The functional implication of the identified proteins was discussed.     

测量不确定度在分析化学实验教学质量控制中的应用

本文根据CNAL/AG07:2002指南评定程序,对武汉大学主编《分析化学实验》(第4版)有代表性的基础定量实验进行了测量不确定度的详细评估;确定了有关参数的不同分量对合成标准不确定度的影响程度大小,对实验教学质量控制(SPC)中的异因诊断具有一定的指导作用。     

认真学习毛主席哲学著作 努力搞好毕业实践

遵照毛主席关于“教育必须为无产阶级政治服务,必须同生产劳动相结合”的教导,我们化学系无机专业34名工农兵学员和11名教师,从1974年2月起,分赴长岭炼油厂、大冶有色金属公司、武汉无机盐厂和校办九·一二化工厂等单位进行毕业实践。经过五个月,在毛主席革命路线指引下,在批林批孔的推动下,在实践中,通过学习毛主席的哲学著作《实践论》和《矛盾论》,使我们的马列主义水平不断提高,分析问题和解决问题的能力也有显著的增强,在科学试验上取得了一些可喜的成果。据初步统计,在我们毕业实践的十一个项目中,已用于工业生产的有两项,即将投入生产或中试的有两项,取得阶段成果的有三项,其他几项也为以后的实验提供了有用的资料。这些成果表明,毛主席的哲学思想是指导科学试验的锐利武器,无产阶级文化大革命和批林批孔运动是推动教育革命的强     

光谱成像技术无损鉴别西洋参饮片的研究

应用电可控液晶光谱成像装置,测定不同市售来源的西洋参饮片,以期为其质量控制提供新的方法。系统光谱分辨率5nm,光谱覆盖范围为405～680nm,空间分辨率50lp·mm-1。从成像光谱立方体中提取特征光谱曲线,构建饮片指纹图谱;采用主成分等聚类分析方法解析其指纹图谱,用于饮片真伪鉴别与质量判定。结果与性状,显微及理化鉴定结果相吻合。表明光谱成像分析技术可用于中药指纹图谱的构建和质量评价,操作方法简便、快速、无损。     

硫砷玻璃光存储记录材料

早在四十年代,就有人对硫砷玻璃的透红外性能进行过研究。但是作为激光全息记录介质来研究还仅仅是近几年来的事情。我们全组同志遵照伟大领袖毛主席关于“中国人民有志气,有能力,一定要在不远的将来,赶上和超过世界先进水平”的教导,在批林批孔运动的推动下,坚持走“独立自主、自力更生”的道路,经过一年多的努力,终于在1974年10月份成功地在硫砷玻璃介质上实现了激光全息存储。在直径约1mm的点子内存储了《在社会主义大道上前进》的一页文字(见图1)。再现后文字清晰,黑白分明,至今已有半年,尚未发现明显变化。     

长磁聚焦电偏转图象加强管

本文介绍西安光机所自行设计和研制的一种磁聚焦静电偏转象加强器。光电阴极有,S11和S20二种,电子倍增膜采用Al₂O₃—Al—KCl膜,萤光屏为K₉萤光粉制作;象增强器光增益1～5×10⁴倍,分弁率15～20线对/毫米,扫描时间4微秒,线性偏转面积10×20平方毫米。本象加强器被有关单位用于测量爆炸物的爆轰压力取得了良好结果。