Determination of ranolazine in human plasma by liquid chromatographic-tandem mass spectrometric assay

A highly sensitive liquid chromatographic-tandem mass spectrometric method (LC-MS-MS) is developed to quantitate ranolazine in human plasma. The analyte and internal standard tramadol are extracted from plasma by liquid-liquid extraction using diethyl ether-dichloromethane (60:40 v/v), and separated on a Zorbax extend C(18) column using methanol-10mM ammonium acetate (60:40 v/v, pH 4.0) at a flow of 1.0 mL/min. Detection is carried out by multiple reaction monitoring on a QtrapTM LC-MS-MS system with an electrospray ionization interface. The assay is linear over the range 10-5000 ng/mL with a limit of quantitation of 10 ng/mL and a lower limit of detection (S/N > 3) of 1 ng/mL. Intra- and inter-day precision are < 3.1% and < 2.8%, respectively, and the accuracy is in the range 96.7-101.6%. The validated method is successfully used to analyze the drug in samples of human plasma for pharmacokinetic studies.     

From metal-organic framework to nanoporous carbon: toward a very high surface area and hydrogen uptake

In this work, with a zeolite-type metal-organic framework as both a precursor and a template and furfuryl alcohol as a second precursor, nanoporous carbon material has been prepared with an unexpectedly high surface area (3405 m(2)/g, BET method) and considerable hydrogen storage capacity (2.77 wt % at 77 K and 1 atm) as well as good electrochemical properties as an electrode material for electric double layer capacitors. The pore structure and surface area of the resultant carbon materials can be tuned simply by changing the calcination temperature.     

2-[1-(4-甲酰氨基苯基乙酰氧)烷基]-1,4-二羟基-9,10-蒽醌类衍生物的 合成及其抗肿瘤作用研究

为寻找抗肿瘤作用强、毒性低并且对癌细胞具有靶向性的新蒽醌类化合物, 合成了未见报道的12个2-[1-(4-甲酰氨苯基乙酰氧)烷基]-1,4-二羟基-9,10-蒽醌类衍生物, 分别用L1210癌细胞进行细胞毒性实验及小鼠S180腹水癌做了体内抗肿瘤实验. 实验结果表明, 蒽醌侧链中引入对甲酰氨基苯乙酰基后细胞毒性增强. 随着侧链碳链数的增加细胞毒性随之逐渐减小, 当烷基侧链中的碳数超过7以上时, 细胞毒性消失. 当侧链R基为苯环时与脂肪烃链或环己基相比细胞毒性更大, 说明芳香环对癌细胞具有更强的抑制作用. S180小鼠抗肿瘤实验结果表明, 蒽醌侧链中引入对甲酰氨基苯甲酰基后活性无显著性变化.     

Optimization on fabrication and performance of A-site-deficient La0.58Sr0.4Co0.2Fe0.8O3-δ cathode for SOFC

A-site-deficient perovskite cathode material La_0.58Sr_0.4Co_0.2Fe_0.8O_3 − δ (L58SCF) is coated on the yttria-stabilized zirconia electrolyte by screen-printing technique. Several key fabrication parameters including selection of additives (binder and pore former), effect of coating thickness, sintering temperature and time on the microstructure, and electrochemical performance of cathode are investigated by scanning electron microscopy and electrochemical impedance spectroscopy. We study the microstructure and the electrochemical property of the cathode with different kinds of additives. Results show that the cathode possesses fine microstructure, enough porosity, and ideal electrochemical property when polyvinyl butyral serves as both binder and pore former in the cathode. The cathode with three screen-printing coats (thickness 28 ± 7 μm, weight 6.07 ± 0.72 mg cm⁻²) sintering at 1,000 °C for 2 h shows lower polarization resistance of 0.183 Ω cm² at 800 °C. Based on the optimized parameters, the polarization resistances of the L58SCF–Ce_0.8Gd_0.2O_{1.9 – δ} composite cathode display the R _p values of 0.067 Ω cm² at 800 °C, 0.106 Ω cm² at 750 °C, 0.225 Ω cm² at 700 °C, and 0.550 Ω cm² at 650 °C.     

Simultaneous determination of naphazoline and pyridoxine in eye drops using excitation–emission matrix fluorescence coupled with second-order calibration method based on alternating trilinear decomposition algorithm

A novel method is developed for the direct determination of naphazoline hydrochloride(NAP) and pyridoxine hydrochloride(VB6) in commercial eye drops. By using excitation–emission matrix(EEM)fluorescence coupled with second-order calibration method based on the alternating trilinear decomposition(ATLD) algorithm, the proposed approach can achieve quantitative analysis successfully even in the presence of unknown and uncalibrated interferences. The method shows good linearity for NAP and VB6 with correlation coefficients greater than 0.99. The results were in good agreement with the labeled contents. To further confirm the feasibility and reliability of the proposed method, the same batch samples were analyzed by multiple reaction monitoring(MRM) based on LC–MS/MS method.T-test demonstrated that there are no significant differences between the prediction results of the two methods. The satisfactory results obtained in this work indicate that the use of the second-order calibration method coupled with the EEM is a promising tool for industrial quality control and pharmaceutical analysis due to its advantages of high sensitivity, low-cost and simple implementation.     

Application of XPS imaging analysis in understanding interfacial delamination and X‐ray radiation degradation of PMMA

The recent development of X‐ray Photoelectron Spectroscopy (XPS) instrumentation with spatial resolution down to several microns has advanced the capability of elemental and chemical state imaging. XPS imaging analysis has been applied in understanding the delamination problems of siloxane coatings on polymethyl‐methacrylate (PMMA) polymer. It was found that delamination occurred by interfacial failure, and the coating suffered complete delamination from a PMMA substrate. This example offered an opportunity for the investigation of X‐ray damage on polymers encountered in XPS imaging analysis. This paper also demonstrated how to construct a constrained peak model with the aid of chemical knowledge and supporting evidence of the sample. Monte Carlo error analysis was used to determine the validity of the peak fit models used. Copyright © 2013 John Wiley & Sons, Ltd.     

MOF-808/Bi2MoO6复合材料的构筑及其光催化性能

采用简单的两步水热法制备出了锆基金属有机骨架和钼酸铋的复合材料MOF-808/Bi₂MoO₆。通过X射线粉末衍射、傅里叶红外光谱、扫描电子显微镜、透射电子显微镜、X射线光电子能谱、紫外可见漫反射光谱、N₂吸附-脱附测试和电化学测试对所制备材料的组成、微观结构、光学性质以及光生载流子的复合效率进行了分析。与纯Bi₂MoO₆和MOF-808相比,0.5%-MOF-808/Bi₂MoO₆复合材料展示出了较高的光催化活性,在可见光照射120 min时对抗生素环丙沙星(CIP)的降解率达89.7%。通过自由基捕获实验,证明了·O₂^-是主要活性物种,基于此我们提出了可能的光催化降解机理。     

Cd2(Te6O13)][Cd2Cl6] and Cd7Cl8(Te7O17): novel tellurium(IV) oxide slabs and unusual cadmium chloride architectures

Initial attempts to prepare new Ln-Cd-Te-O-Cl compounds led to the isolation of two novel cadmium tellurium(IV) oxychlorides with two different types of structures, namely, [Cd(2)(Te(6)O(13))][Cd(2)Cl(6)] and Cd(7)Cl(8)(Te(7)O(17)). Both compounds feature novel polymeric tellurium(IV) oxide anions and unusual cadmium chloride substructures. The structure of [Cd(2)(Te(6)O(13))][Cd(2)Cl(6)] is composed of 1D [Cd(2)Cl(6)](2)(-) double chains and (002) [Cd(2)(Te(6)O(13))](2+) layers. The 1D Te(6)O(13)(2)(-) slab of the [Cd(2)(Te(6)O(13))](2+) layer is formed by TeO(3), TeO(4), and TeO(5) groups via corner- and edge-sharing, and it contains six- and seven-membered tellurium(IV) polyhedral rings. The structure of Cd(7)Cl(8)(Te(7)O(17)) features a 3D network with long-narrow tunnels along the b axis. The two types of structural building blocks are 1D [Te(7)O(17)](6)(-) anions and unusual corrugated [Cd(7)Cl(8)](6+) layers based on "cyclohexane-like" Cd(3)Cl(3) rings.