Quantification of Structural Integrity and Stability Using Nanograms of Protein by Flow-Induced Dispersion Analysis

In the development of therapeutic proteins, analytical assessment of structural stability and integrity constitutes an important activity, as protein stability and integrity influence drug efficacy, and ultimately patient safety. Existing analytical methodologies solely rely on relative changes in optical properties such as fluorescence or scattering upon thermal or chemical perturbation. Here, we present an absolute analytical method for assessing protein stability, structure, and unfolding utilizing Taylor dispersion analysis (TDA) and LED-UV fluorescence detection. The developed TDA method measures the change in size (hydrodynamic radius) and intrinsic fluorescence of a protein during in-line denaturation with guanidinium hydrochloride (GuHCl). The conformational stability of the therapeutic antibody adalimumab and human serum albumin were characterized as a function of pH. The simple workflow and low sample consumption (40 ng protein per data point) of the methodology make it ideal for assessing protein characteristics related to stability in early drug development or when having a scarce amount of sample available.     

Complications in the Use of the Taylor Dispersion Method for Ternary Diffusion Measurements: Methanol + Acetone + Water Mixtures

The Taylor dispersion technique is used to measure the ternary mutual diffusion coefficients of aqueous nonelectrolyte solutions at 25°C. The dispersion of the injected solutes is recorded by a differential refractometer and an ultraviolet-visible detector. The diffusion coefficients are calculated directly by fitting the theoretical dispersion equations to about six experimental curves simultaneously. If the ternary diffusion effects in the measured dispersion profiles are not confused by the inaccuracy of the experimental method or an unfavorable relative detector sensitivity, the diffusion coefficients are precise. For the system methanol + acetone + water, it is shown that the Taylor dispersion method is unsuitable for the determination of all the diffusion coefficients if the methanol mole fraction is less than 0.45 or the acetone mole fraction if more than 0.001.     

分散第二相Al_2O_3对高分子固体电解质电性能的影响

于固体电解质PEO＿NaSCN络合物中加入Al2O3绝缘体作为第二相,分别研究了Al2O3的粒径,含量对该固体电解质电性能的影响.发现当Al2O3的粒径小于1μm时,离子电导率比纯的固体电解质的电导率高,大于1μm时,则比纯样品的低,即临界粒径约为1μm.当Al2O3的含量达到约25%时,电导率达到极大值.此外,样品的高频极化和低频极化也随Al2O3的粒径的增大而越显著.     

Pharmaceutical performance of solid dispersions containing poly(ethylene) glycol 6000 and diazepam or temazepamInfluence of grinding

The effect of grinding on the physical properties and pharmaceutical performance of solid dispersions made of poly(ethylene) glycol 6000 (PEG6000) and temazepam or diazepam was studied using differential scanning calorimetry (DSC), X-ray powder diffraction and dissolution experiments. DSC-analysis of flash-cooled dispersions revealed that amorphous PEG present immediately after grinding crystallised upon aging mainly into the twice folded modification and to a small extent into the extended form. DSC-analysis of dispersions kept in the slab form for 1 month and subsequently ground, revealed that in the abscence of the grinding impulse crystallisation of PEG6000 takes place in the same way as in dispersions ground immediately after preparation and then aged for 1 month. Grinding solid dispersions immediately after preparation resulted in superior dissolution properties compared with solid dispersions kept in the monolith-slab form and subsequently ground. This difference in dissolution properties was found to be attributed to the drug and not to the polymer, more precisely, it was suggested that the drug particle size in ground dispersions was smaller than in dispersions kept in the slab form and subsequently ground. These findings suggest that grinding of solid dispersions immediately after preparation is the preparation method of choice instead of liquid filling of hard gelatin capsules resulting in monoliths. This revised version was published online in July 2006 with corrections to the Cover Date.     

Quantitative analysis of MWCNT agglomeration in polymeric‐based membranes using atomic force microscope

In this work, we performed an analysis on the surface properties of polyethersulfone (PES)‐based ultrafiltration membranes that were prepared by incorporating acid functionalized multiwalled carbon nanotube (f‐MWCNT) and polyvinylpyrrolidone into membrane matrix via simple blending method. The bonding‐chemistry of the nanocomposites implanted within the PES membrane was investigated by Fourier transform infrared spectrometer while atomic force microscope was employed to observe the distribution of f‐MWCNT in the membrane matrix and further measured its agglomeration quantitatively. The resultant 3D atomic force microscope images provided the most satisfactory way to examine the distribution of nanomaterials in the membranes, and with the help of ‘point profile data’ the maximum height and width of the agglomerated cluster could be quantitatively calculated. Moreover, the surface profile studies of the membrane surface provided the information about the length, volume, area, perimeter, radius and diameter of grains. It was observed that PES/nanocomposite blended membranes were held together via strong hydrogen bonding, but poor dispersion of MWCNT in the membrane matrix reduced the membrane performance in terms of protein (pepsin and bovine albumin serum) rejection and increased the surface roughness. Copyright © 2016 John Wiley & Sons, Ltd.     

富缺陷BN负载的高分散Cu催化乙醇脱氢制乙醛

生物乙醇作为平台分子通过催化转化的方法可以制备烯烃、乙醛、丁醇和芳香化学品等,其中乙醛是生产乙酸、季戊四醇、三氯乙醛、山梨酸等重要化学品的原料.随着乙醛的需求量逐年增加,发展以乙醇直接脱氢生成乙醛的工艺,具有联产氢气、原子经济性高、产物易分离的优点,符合国际绿色低碳发展战略要求,有望替代当前乙烯氧化法生产工艺.乙醇分子...     

Time domain measurement of dispersion in optical fibres

A time domain dispersion measurement apparatus was successfully built and tested at the Indian Institute of Technology, Madras. This instrument can measure directly the pulse broadening in a multimode optical fibre. The basic dispersion mechanisms in optical fibres and the design details of the system are discussed.     

Formation of Ultrafine Apatite Fibers by Sol-gel/Electrospinning

Ultrafine apatite fibers were prepared by electrospinning of sol-gel precursor/poly（ vinyl pyrrolidone） （PVP） solutions followed by subsequent calcination. The as-electrospun and calcinated fibers were observed under a scanning electron microscope and an optical polarizing microscope. Results show that the morphology and the diameter of as-electrospun fibers strongly depend on the viscosity and the surface tension of sol-gel precursor/PVP solutions. After calcination, the smooth as-electrospun fibers shrink and the fiber diameter decreases because of the removal of the polymer. The chemical evolution upon the transformation of the precursor from a gel to the final apatite fibers was investigated by thermogravimetric-differenfial thermal analysis, X-ray diffraction, and Fourier transform infrared spectroscopy. It is thus suggested that the crystalline structure of the calcined fibers is largely influenced by the calcination temperature. After being calcined at 600 ℃, the apatite fibers with a diameter of about 280 nm containing β-tricalcium phosphate were obtained.     

高峰值功率大模场全光纤脉冲放大器

报道了一种由纤芯直径分别为15 μm和25 μm的大模场光纤组成的全光纤脉冲放大器模块。当注入脉冲宽度为10 ns,重复频率为1 Hz,光谱宽度为0.3 nm,脉冲能量为80 nJ的激光脉冲时,经过两级放大输出的激光脉冲峰值功率为30 kW,单脉冲能量为300 μJ。此外,实验研究了该放大器模块输出的时间特性。研究发现：由于受激布里渊散射（SBS）效应,限制了单纵模光纤激光在光纤中的高能量放大,采用宽带激光脉冲可以有效地抑制SBS效应,提高光纤放大器的SBS阈值。     

激光点火系统用高功率光纤光开关

仿真和实验研究了一种控制Nd:YAG脉冲激光能量通断的光纤直接连接型光开关。建立光纤耦合模型,分析了光纤对准误差中对耦合效率的影响,其中横向偏移的影响最显著。采用微机电系统V型槽固定光纤,微小型凸轮作为制动器,步进电机驱动凸轮旋转,微小型凸轮与移动光纤相切,带动光纤移动,实现两光纤的错开和对准。制造了这种高功率直接连接型光纤光开关原理样机,并进行了主要性能测试。测试结果表明,这种光开关能够满足激光点火系统的大容量、高隔离度的要求。