应用低相干动态光散射法测量悬浮液中的颗粒粒径分布

利用低相干动态光散射法测量不同浓度悬浮液中的颗粒粒径分布。由低相干光源和迈克尔逊干涉仪,结合传统的动态光散射技术组成低相干动态光散射装置,通过检测单次背散射光的能谱分布,利用CONTIN算法得到不同浓度悬浮液中颗粒的粒径分布。结果表明,对于1%～10%体积浓度范围内的单分散悬浮液羊品测量得到的颗粒粒径精确度在4%以内。     

利用低相干光纤动态光散射法测量浓悬浮液中多分散颗粒粒径分布

本文针对高浓度散射介质,用低相干光纤动态光散射技术测量浓悬浮液中多分散颗粒系的粒径及其粒径分布。利用迭代CONTIN算法对实验数据进行反演运算,得到多分散颗粒系的粒径分布结果。结果表明,浓悬浮液中多分散颗粒系的峰值粒径测量值与给定的两种标准粒径值相吻合,其误差在4%之内,粒径分布曲线中各散射颗粒所反映的散射体光强分布与根据Mie散射计算得到的理论值相吻合。实验结果证明低相干光纤动态光散射实验系统能准确测量浓悬浮液中多分散颗粒粒径及粒径分布。     

多模光纤式动态光散射实验研究

介绍了多模光纤在动态光散射中的应用,搭建了基于多模光纤的动态光散射实验系统,并用该系统测量了单分散、多分散以及不同浓度的标准聚苯乙烯乳胶球悬浮液.结果表明,该系统可准确地测量浓度达4.5%的聚苯乙烯乳胶球溶液中悬浮颗粒的粒径分布.     

应用动态光散射和透射电镜研究热力学不相容条件下果胶与乳清蛋白混合体系的微观结构

应用动态光散射、透射电镜和粘度-剪切模型3种方法互相配合,研究了果胶与乳清分离蛋白的混合体系在热力学不相容条件下的微观结构。在90℃及pH7.4条件下,向5%蛋白浓度的乳清蛋白溶液中加入带有负电的果胶分子,可导致热变性乳清蛋白分子之间发生损耗聚集,并引发混合体系内的相分离现象。确切地说,当果胶与乳清蛋白的混合重量比小于0.08时,溶液内可观察到粒径小于300nm的聚集颗粒,体系呈现牛顿流体特征;而当混合重量比大于0.08时,体系粘度上升,切稀特征逐渐明显,聚集集团粒径接近700nm。     

基于偏振门的动态光散射颗粒测量法的研究

为了解决动态光散射纳米颗粒测量技术无法测量高浓度颗粒粒径的难题,提出了一种基于偏振门的动态光散射测量法。从动态光散射和Mie理论出发,理论分析了在高浓度溶液下多重散射效应对散射光偏振态和颗粒粒度测量结果的影响。根据散射光偏振特点,结合偏振门检测技术,改进了传统的动态光散射光学系统。实验研究了在低浓度和高浓度溶液时,不同偏振角度下的散射光强和粒度测量值,完善了散射光的偏振理论。采用90°偏振门检偏,通过各种浓度下的实验,证明了方法的可行性。该方法较之目前同类方法具有原理和结构简单,系统易于维护的特点。     

核酸适配体纳米金共振散射光谱检测血清中钾离子

在pH7.0的Na2HPO4-NaH2PO4缓冲溶液中,纳米金与适配体(aptamer)结合形成较稳定的aptamer-Au复合物,且不被NaCl聚集。在85℃水浴中,K+与aptamer作用后折叠形成稳定的G-四分体结构复合物且释放出纳米金。在高浓度盐作用下,纳米金聚集成较大粒径的纳米金颗粒,导致体系563nm处的共振散射强度增大,其平均粒径为120nm。文章研究了K+ -随机单链DNA1(ssDNA1)-纳米金、K+ -ssD-NA2-纳米金和K+ -aptamer-纳米金体系的共振散射光谱特性,并用圆二色光谱技术证明了核酸适配体结构的变化。考察了pH、NaCl浓度、aptamer浓度、纳米金用量以及Cu2+、Mg2+、Pb2+、Ca2+、Al3+、Zn2+Fe3+等常见重金属离子等对测定K+的影响,结果显示这些离子不干扰测定,该法具有较好的选择性。在选定条件下,K+浓度在0.67～3350μmol·L-1范围与共振散射峰值ΔI呈良好的线性关系,回归方程、相关系数、检出限分别为ΔI=0.167c-0.7,0.9932,0.3μmol·L-1 K+。该法用于血清样品分析,结果与离子选择电极法一致。     

电解质对浓悬浮液中胶体颗粒扩散特性的影响

本文利用相位调制光纤低相干动态光散射装置, 研究了不同物质量浓度下电解质 (NaCl及 BaCl₂) 对浓悬浮液中聚苯乙烯胶体颗粒扩散特性的影响. 实验结果表明, 当电解质浓度低于0.01 mol/L 时, 恒温条件下浓悬浮液中聚苯乙烯胶体颗粒扩散系数随电解质离子浓度以及离子化合价的增大而增大, 实验测量得到的扩散系数与Stern模型所得到的扩散系数符合较好. 关键词： 测量 电解质 浓悬浮液 低相干动态光散射     

基于动态光散射的SiO_2/H_2O纳米流体分散稳定性初探

基于动态光散射法,采用同差探测实现了纳米流体分散体系的粒度测量。对体积分数为0.005%和0.0025%浓度的SiO_2/H_2O纳米流体颗粒粒径进行了测量,粒径的实验值的平均偏差分别为1.37%和1.39%,可以满足纳米颗粒粒径的高精度测量要求。两种浓度的SiO_2/H_2O纳米流体的平均粒径基本一致,偏差在实验的不确定度以内,且随时间无明显变化,证明了颗粒分散的稳定性,本方法可以用于纳米流体分散稳定性的评价。     

基于单模光纤的DLS粒径测量研究

动态光散射技术是一种测量纳米颗粒粒径分布的最有效方法。为了克服高浓度样品溶液中存在的多重散射效应, 本文基于单模光纤搭建了一套DLS实验系统, 传输光纤的输出端与接收光纤的接收端都作了抛光磨平处理。在模拟复杂工业环境下, 分别用低浓度单分散、不同浓度单分散以及高浓度多分散性标准聚苯乙烯乳胶球悬浮液检测了该系统的适用性。实验结果表明, 利用该系统可快速准确的测量体积分数达40%的聚苯乙烯乳胶球悬浮液中的纳米颗粒粒径及其分布。     

丙酮酸脱氢酶的光子相关动态光散射研究

本文利用动态光散射技术研究丙酮酸脱氢酶,得到其微观结构方面的若干信息.测量出其PDC结构及E_2-X-K结构的半径;发现在较低浓度下,聚集现象可以忽略,尺寸分布是单分散性分布,动态光散射谱的线宽Γ与散射波矢q分别呈Γ∝q~2及Γ∝q~3关系.而在较高浓度下,Γ∝qα,α为分数,这时尺寸分布里多分散性分布.     

Phase separation in dilute solutions of poly (N-isopropylacrylamide)

The appearance of spherical particles resulting from phase separation in dilute solutions of poly(N-isopropylacrylamide) has been observed by dynamic light scattering (DLS). The particles have a relatively narrow size distribution. The size of particles increases with increasing concentration of polymer, and decreasing heating speed. Electron microscopy confirms the existence of spherical particles with size and polydispersity in agreement with DLS.     

Characterisation of silica nanoparticles prior to in vitro studies: from primary particles to agglomerates

The size, surface charge and agglomeration state of nanoparticles under physiological conditions are fundamental parameters to be determined prior to their application in toxicological studies. Although silica-based materials are among the most promising candidates for biomedical applications, more systematic studies concerning the characterisation before performing toxicological studies are necessary. This interest is based on the necessity to elucidate the mechanisms affecting its toxicity. We present here TEM, SAXS and SMPS as a combination of methods allowing an accurate determination of single nanoparticle sizes. For the commercial material, Ludox TM50 single particle sizes around 30 nm were found in solution. DLS measurements of single particles are rather affected by polydispersity and particles concentration but this technique is useful to monitor their agglomeration state. Here, the influence of nanoparticle concentration, ionic strength (IS), pH and bath sonication on the agglomeration behaviour of silica particles in solution has been systematically investigated. Moreover, the colloidal stability of silica particles in the presence of BSA has been investigated showing a correlation between silica and protein concentrations and the formation of agglomerates. Finally, the colloidal stability of silica particles in standard cell culture medium has been tested, concluding the necessity of surface modification in order to preserve silica as primary particles in the presence of serum. The results presented here have major implications on toxicity investigations because silica agglomeration will change the probability and uptake mechanisms and thereby may affect toxicity.     

荧光性胱氨酸聚集纳米团簇的制备及其应用研究

基于碱性胱氨酸水溶液在恒温水浴条件下可形成荧光性分子聚集体的特性,发展一种荧光光谱直接检测胱氨酸含量的新方法。实验结果表明,将pH 9.0的0.01 mol·L-1的胱氨酸溶液,于90 ℃恒温水浴热处理12 h后,胱氨酸分子可形成大小为12.5nm粒径的荧光分子聚集纳米团簇（FANC）结构,并发射蓝绿色荧光。采用荧光光谱（FL）、透射扫描电镜（TEM）和质谱（MS）对FANC的荧光性能和结构进行表征,并初步探讨光致发光机理。FANC在410 nm最佳激发波长条件下,于508 nm处具有最佳的荧光发射信号,体系的平均荧光寿命为6.028 ns,荧光量子产率为8.48%。FANC在水溶液中具有稳定的光漂白性、酸碱稳定性和光谱不依赖性质,粒子的Zeta电位为-57 mV,结合150 nm的水合粒径结果,表明形成的团簇表面亲水且带负电荷。质谱结果显示体系中存在多种胱氨酸分子间脱水形成的分子碎片,因此推测FANC是胱氨酸分子在水溶液环境中因分子间作用力形成分子聚集体。基于FANC的荧光强度和原料胱氨酸的浓度在1.0×10-5～6.0×10-4 mol·L-1范围内呈良好的线性关系,可将该方法用于胱氨酸片中含量的测定,结果与中国药典中记载的滴定比色法相吻合。相比于其他检测方法,该方法具有操作简便,检测限低,精确度高等优点。     

Phosphorylcholine functionalized dendrimers for the formation of highly stable and reactive gold nanoparticles and their glucose conjugation for biosensing

Phosphorylcholine (PC)-functionalized poly(amido amine) (PAMAM) dendrimers were prepared and used as both reducing and stabilizing agents for synthesis of highly stable and reactive gold nanoparticles (Au NPs). Biomimetic PC-functionalized PAMAM dendrimers-stabilized gold nanoparticles (Au DSNPs) were formed by simply mixing the PC modified amine-terminated fifth-generation PAMAM dendrimers (G5-PC) with AuCl₄ ⁻ ions by controlling the pH, no additional reducing agents or other stabilizers were needed. The obtained Au DSNPs were shown to be spherical, with particle diameters ranging from 5 to 12 nm, the sizes and growth kinetics of Au DSNPs could be tuned by changing the pH and the initial molar ratio of dendrimers to gold as indicated by transmission electron microscopy (TEM) and UV–Vis data. The prepared Au DSNPs showed excellent stability including: (1) stable at wide pH (7–13) values; (2) stable at high salt concentrations up to 2 M NaCl; (3) non-specific protein adsorption resistance. More importantly, surface functionalization could be performed by introducing desired functional groups onto the remained reactive amine groups. This was exemplified by the glucose conjugation. The glucose conjugated Au DSNPs showed bio-specific interaction with Concanavalin A (Con A), which induced aggregation of the Au NPs. Colorimetric detection of Con A based on the plasmon resonance of the glucose conjugated Au DSNPs was realized. A limit of detection (LOD) for Con A was 0.6 μM, based on a signal-to-noise ratio (S/N) of 3. These findings demonstrated that the PC modified Au DSNPs could potentially serve as a versatile nano-platform for the biomedical applications.     

Optimization of salt concentration in PEG-based crystallization solutions

Although polyethylene glycol (PEG) is the most widely used precipitant in protein crystallization, the concentration of co-existing salt in the solution has not been well discussed. To determine the optimum salt concentration range, several kinds of protein were crystallized in a 30% PEG 4000 solution at various NaCl concentrations with various pH levels. It was found that, if crystallization occurred, the lowest effective salt concentration depended on the pH of the protein solution and the pI of the protein molecule; that is, higher salt concentrations were required for crystal growth if the difference between pH and pI was increasing. The linear relationship between the charge density of the protein and the ionic strength of the crystallization solution was further verified. These results suggested that the lowest effective concentration of salt in a crystallization solution can be predicted before performing a crystallization experiment. Our results can be a tip for tuning crystallization conditions by the vapor-diffusion method.     

Increasing the sensitivity of cryoprobe protein NMR experiments by using the sole low-conductivity arginine glutamate salt

Decrease in experimental sensitivity of cryoprobe experiments for salty samples, attributed to increased sample conductivity, has been a long-standing issue in protein NMR. Salt concentration can not be simply reduced as this often leads to protein aggregation. A simple and inexpensive solution to this problem is demonstrated here. We show that even for proteins prone to aggregation, the traditional solubilizing salt, 100mM NaCl, can be completely replaced by 50mM l-Arg and l-Glu. This replacement simultaneously reduces the sample conductivity and improves protein solubility. Up to a 6-fold overall increase in experimental sensitivity was achieved, in comparison with the traditional salty buffer. At constant protein concentration up to 2-fold increase in sensitivity was observed. The lengths of the proton pi/2 pulses were also significantly decreased, up to the level typical for non-salty samples in water.     

Fabrication of silk sericin/alginate microparticles by electrohydrodynamic spraying technique for the controlled release of silk sericin

Silk sericin has been recently investigated for many biological roles. This study aimed to develop the new delivery system to control the release of silk sericin. The alginate microparticles encapsulating silk sericin were fabricated by electrospraying technique. Concentrations of silk sericin and alginate polyelectrolyte solutions were investigated. All microparticles had an average size of 264–284 μm and could entrap silk sericin with high entrapment efficiency (84–89%). The microparticles could deliver silk sericin in a rate-controlled manner. This study would show a promising controlled release application of silk sericin protein from alginate microparticles fabricated by the means of electrostatic forces.     

Molecular mobility of confined phases in model mesoporous (MCM-41) and microporous (AlPO4-5 zeolite) host materials

This paper discusses the self-assembly of block copolymers into vesicular morphology. After a brief state of art of the field, a system based on an amphiphilic poly(butadiene)-b-poly(-L-glutamic acid) (PB-b-PGA) diblock copolymer in aqueous solution is discussed in detail. The aggregation behavior of this block copolymer has been investigated by means of fluorescence spectroscopy, dynamic (DLS) and static (SLS) light scattering as well as transmission electron microscopy (TEM). The diblock copolymer was found to form well-defined vesicles in water. The size of these so-called polymersomes or peptosomes could be reversibly manipulated as a function of both pH and ion strength. Depending on the pH of the aqueous solution, the hydrodynamic radii of these vesicles were found to vary from 100 nm to 150 nm. By cross-linking the 1,2-vinyl double bonds present in the polybutadiene block, the ability to transform a transient supramolecular self-organized aggregate into a permanent “shape-persistent stimuli-responsive nanoparticle” has been demonstrated. Received 25 June 2002 and Received in final form 22 October 2002 Published online: 11 March 2003     

Mechanisms of structure formation in particulate gels of β-lactoglobulin formed near the isoelectric point

Particulate gels are known to be formed by bovine β-lactoglobulin near the isoelectric point when partial unfolding is allowed to occur under heating. The aggregation process of the protein has been investigated within the context of a nucleation and growth process by preparing gels under precisely controlled thermal histories. This was achieved using a Differential Scanning Calorimeter (DSC) to provide controlled heating rates, and known final temperatures and incubation times. The resulting particulate gels were characterized by their particle size and polydispersity using Environmental Scanning Electron Microscopy (ESEM), which permits hydrated samples to be observed. Particle size was found to decrease with increasing final temperature, with the aggregation taking longer to reach completion for lower temperatures. Particle size was also found to decrease with increasing heating rate. This system could be modelled as evolving via nucleation and growth by taking into account the fact that the concentration of the aggregating species was varying as a function of temperature as well as time. The intrinsic tryptophan fluorescence as a function of temperature was used as a guide to the fraction of unfolded protein in solution, thereby permitting successful comparisons between the model predictions and the particle sizes to be made.-1     

Silk peptide production from whole silkworm cocoon using ultrasound and enzymatic treatment and its suppression of solar ultraviolet-induced skin inflammation

Silk fibroin, which is derived from sericin through degumming, is mainly used as a biomaterial. However, interest in functional verification and industrial applications of sericin has been growing for several years. We used ultrasonication to simplify the extraction process of the silk peptide under low salt conditions at 20 °C, instead of using the conventional conditions of high salt and temperature. The concentration of the silk peptide was measured to determine the optimized extraction time and solvent, which were 4 h and 0.1 N NaOH, respectively. The molecular weight of the enzyme-treated silk peptide was measured using SDS-PAGE and GPC. Silk peptide treated with papain after ultrasound had a molecular weight of less than 5 kDa, and the papain treated-silk peptide reduced solar ultraviolet-induced COX-2 expression through inhibition of ERK phosphorylation. This is the first study investigating simultaneous extraction of fibroin and sericin, which can be used for mass production of food materials.