Evaluation of copper-1,3,5-benzenetricarboxylate metal-organic framework (Cu-MOF) as a selective sorbent for Lewis-base analytes

The metal-organic framework copper-1,3,5-benzenetricarboxylate (Cu-BTC) was evaluated for its ability to selectively interact with Lewis-base analytes by examining retention on gas-chromatographic columns packed with Chromosorb W HP that contained 3.0% SE-30 along with various loadings of Cu-BTC. Scanning electron microscopy images of the support material showed the characteristic Cu-BTC crystals embedded in the SE-30 coating on the diatomaceous support. The results indicated that the Cu-BTC-containing stationary phase had limited thermal stability (220 °C) and strong general retention for analytes. Kováts index calculations showed selective retention (amounting to about 300 Kováts units) relative to n-alkanes for many small Lewis-base analytes on a column that contained 0.75% Cu-BTC compared with an SE-30 control. Short columns that contained lower loadings of Cu-BTC (0.10%) allowed elution of nitroaromatics; however, selectivity was not observed for aromatic compounds (including nitroaromatics) or nitroalkanes. Observed retention characteristics are discussed.     

Stability evaluation of tramadol enantiomers using a chiral stability-indicating capillary electrophoresis method and its application to pharmaceutical analysis

In this study, a chiral stability-indicating CE assay was developed for the stability evaluation of tramadol (TR) enantiomers in commercial tablets using maltodextrin as chiral selector. To investigate the stability-indicating power of the analytical method as well as stability evaluation of TR enantiomers, active pharmaceutical ingredient and TR tablets were subjected to photolysis, heat, oxidation and hydrolysis to conduct stress testing. Best separation for the TR enantiomers was achieved on an uncoated fused-silica capillary at 20 °C using borate buffer (50 mM, pH 10.2) containing 10% m/v maltodextrin. All determinations were performed by a UV detector at 214 nm. A constant voltage of 20 kV was applied to obtain the separation. The range of quantitation for both enantiomers was 5-100 μg/mL (R>0.996). Intra- and inter-day RSD (n=6) were less than 10%. The percent relevant errors were obtained to be less than 4.0 for both enantiomers. The limits of quantitation and detection for both enantiomers were 5 and 1.5 μg/mL, respectively. Degradation products resulting from the stress studies were the same for both enantiomers and did not interfere with the detection of the enantiomers.     

利用样本成分耗散物的非线性化学指纹图谱原理及相似度计算与评价

在恒温恒压条件下,以丙酮和样本中底物作为主要耗散物的不同成分的样本对非线性化学反应机理产生不同影响,从而引起反应体系电位-时间曲线形状不同变化为特征的B-Z化学振荡体系为例,就非线性化学指纹图谱原理进行了详细研究和讨论,并提出了计算非线性化学指纹图谱系统相似度的通用方法.利用系统相似度和欧氏距离、相关系数及夹角余弦对不同生产批次古汉养生精和18种其他样本的非线性化学指纹图谱的相似度进行了计算与分析.结果表明,相关系数和夹角余弦都不能用来作为评价非线性化指纹图谱相似度的指标.利用欧氏距离公式计算指纹图谱的非参数型相似度时,能正确反映指纹图谱的特征差异,但用其计算参数型相似度时,则有时不能正确反映样本非线性化学指纹图谱特征差异的相对程度.系统相似度能最真实反映样本指纹图谱之间差异程度,是4种相似度计算方法中最好的,可用于非线性化学指纹图谱相似度计算与评价.成功提出了一种经济、简便、易行和有效的鉴别样本真伪与评价其质量的科学方法.     

利用样本成分耗散物的非线性化学指纹图谱的检测方法、条件、特点和应用

分析了适用于测定样本非线性化学指纹图谱的热力学体系和动力学模型,结果表明,在远离平衡的封闭体系和无耗散物补充的敞开体系中,阻尼非线性化学反应对样本化学成分的群集表征和整体含量分析具有重要作用．以丙酮和葡萄糖等为耗散物的阻尼B—Z振荡非线性化学反应为例,研究了反应物种及其浓度、电极类型、温度、搅拌速率、样本种类及用量等影响非线性化学指纹图谱的因素,并对指纹图谱中样本化学成分的定量信息、指纹图谱的特点和应用等进行了研究．成功提出了用于鉴别和评价样本的非线性化学指纹图谱的检测条件和方法．     

Bernstein-type operators on a triangle with all curved sides

We construct and analyze Bernstein-type operators on triangles with curved sides, their product and Boolean sum. We study the interpolation properties and approximation accuracy. Using the modulus of continuity we also study the remainders of the corresponding approximation formulas. Finally, there are given some particular cases and numerical examples.     

Accurate evaluation of a polynomial in Chebyshev form

This paper presents a compensated algorithm to accurately evaluate a polynomial expressed in Chebyshev basis of the first and second kind with floating-point coefficients. The principle is to apply error-free transformations to improve the traditional Clenshaw algorithm. The new algorithm is as accurate as the Clenshaw algorithm performed in twice the working precision. Forward error analysis and numerical experiments illustrate the accuracy and properties of the proposed algorithm.     

CdZnTe像素阵列探测器成像评价模型及实验

考虑载流子陷获效应建立了碲锌镉(CdZnTe)像素阵列探测器感应电荷分布模型,并从非平衡载流子连续方程出发,推导了晶体内部陷获载流子数密度分布,得到了CdZnTe探测器成像调制传递函数评价模型。数值计算结果表明:随入射光子能量的增加,探测器成像质量明显下降;当电子载流子与空穴载流子迁移寿命积范围分别为0.510-3 to 5.010-3 cm2/V,2.010-5 to 7.510-5 cm2/V时,电子载流子感应信号是探测器响应信号的主要来源,而空穴迁移寿命积变化对探测器成像性能的影响有限,所建立模型的载流子收集特性与实际探测器载流子收集特性相符。搭建了40 mm40 mm的CdZnTe成像探测系统,探测并获得了系统预采样调制传递函数。实验结果表明:模型理论值与实验数据相符合,实际CdZnTe晶体中存在的固有深能级缺陷、实验所采用的非单色性X射线源及较大的实际像素间隙是造成理论值与实验结果存在一定偏差的主要原因。     

离轴抛物面反射镜模拟空间环境镜面变形分析

在卫星红外多光谱扫描仪模拟空间环境辐射定标试验中,环境模拟器舱内的稳、瞬态温度场会给光学系统成像质量带来影响.以试验中的实测温度变化作为温度载荷,借助有限元软件,分析了定标系统中通光孔径为φ400mm的离轴抛物面主镜的温度场分布和热弹性变形.选用在单位圆内正交的Zernike多项式为拟合基函数,通过坐标变换,将抛物镜表...     

基于微粒群区域搜索和小波评价的差分式自动聚焦

为进一步提高图像法自动聚焦的性能,提出了一种差分式提取图像边缘的方法,并构造了图像清晰度的小波评价函数,同时利用微粒群(PSO)算法对聚焦区域进行快速搜索。首先,介绍了差分式边缘提取方法及其优势,给出了一种评价区域的选取判据以及基于PSO的高效搜索方法;然后,对小波评价函数参数进行了比较分析和优选;最后,与传统方法进行了对比实验。结果表明,由于采用了差分式提取方法以及新的自适应聚焦窗口和评价函数,聚焦曲线较传统方法具有更高的调焦分辨率,PSO算法的使用使聚焦速度提高了约170 ms,聚焦精度约为2.3μm,同时调焦效果不受初始位置的影响。     

Synthesis and antitumor evaluation of fluoroquinolone C3 fused heterocycles(Ⅱ):From triazolothiadiazines to pyrazolotriazoles

To further expand an effective modified route for the shift from an antibacterial fluoroquinolone（FQ） to an antitumor FQ,two series of title compounds based on an isostere of the FQ C3 carboxylic group with two fused heterocyclic rings,[1,2,4]triazolo[3,4- b][1,3,4]thiadiazine and pyrazolo[5,1-c][1,2,4]triazole,respectively,were designed and synthesized starting from the current antibacterial FQs,and their in vitro antitumor activity against L1210,CHO cell lines were evaluated via their respective IC₅₀ values.