Name: advanced compositional analysis of nanoparticle-polymer composites using direct fluorescence imaging
Uploaded: 2016-07-19T14:00:00.000+00:00
Duration: 7 min 41 s
Description: Watch this Scientific Journal Video about Advanced Compositional Analysis of Nanoparticle-polymer Composites Using Direct Fluorescence Imaging at JoVE.com

C.R.C. would like to acknowledge the Ramsay Memorial Trust for funding.

1.硒化镉/ ZnS核/壳量子点的制备<ol><li> 在三辛基的制备（TOP）-Se解决方案 <ol><li>通过在氮气下或者在手套箱硒适量混入TOP的Schlenk烧瓶（每个反应8需要毫升，通常为0.4克浓度在10毫升的TOP）制备硒的TOP中的0.5M的溶液。 </li><li>搅拌该混合物以溶解硒1小时，从而在TOP-硒复合物的灰色溶液。 </li><li>确保溶液然后冷冻 - 泵 - 解冻脱气5次。将所得储备溶液可以在氮气下储存3个月。 </li></ol></li><li> 在核心的CdSe的制备 <ol><li>称出镉氧化物（51毫克，0.4毫摩尔），顶部氧化物（3.7克，9.6毫摩尔），十六烷基胺（1.93克，8毫摩尔）和1-十二烷基膦酸（0.22克，0.88毫摩尔）和结合成一个三颈250毫升圆底烧瓶中。添加搅拌棒。 </li><li>关闭两个颈部用隔膜和保证第三附连到长回流冷凝器和氮气/真空的Schlenk线。通过一个隔膜插入一个加热罩温度探头直接到混合物中。泵/用氮气再填充烧瓶五次。 </li><li>加热烧瓶至320℃，并在氮气氛下搅拌1小时熔化。 </li><li>降低壁炉的至270℃的温度，然后用大的注射器和大口径针（20毫升为3mm孔）脱气用氮气5次。 </li><li>采取了8个毫升TOP-硒溶液（步骤1.1）的，并仔细但迅速注入到三颈烧瓶中，通过隔膜。 </li><li>搅拌在270℃下进行30秒分钟之间和10，以控制产生的颗粒的大小的反应。对于红光（〜600纳米），7-9分钟为宜。 </li><li>制备沸水（大到足以浸没在反应容器的一半）下向反应混合物和地点的碗。反应时间结束后，迅速冷却在boili反应纳克水漩。 小心:冷却可导致烧瓶破裂。以极大的关怀和穿着厚厚的防渗透手套。 </li><li>一旦冷却，注入10ml氯仿入烧瓶以溶解所有产品，并划分两个50毫升离心管之间的混合物。 </li><li>顶端的每个管高达50毫升EtOH中并离心在3,600×g的10分钟以沉淀颗粒。弃去上清液，并在总共10毫升正己烷的再分散的粒料。 </li></ol></li><li> 在CdSe核的ZnS，脱壳: <ol><li>的己烷添加芯到100毫升圆底烧瓶中含有锌二乙基二（0.5克，1.4毫摩尔），油胺（3毫升，9.12毫摩尔），三辛基膦（3毫升，6.73毫摩尔）和1-十八碳烯（10毫升）中。添加搅拌棒。交换反应气氛氮气。 </li><li>热在部分真空下3.3℃/分钟的加热板，搅拌器的反应，直至70℃，并使用的Schlenk线去除己烷。 </li&gt; <li>气氛切换为氮气，继续加热以这样的速率到120℃。搅拌在120℃下进行2小时。 </li><li>让反应冷却，并分成2×50毫升离心管之间的混合物。确保将管加满至50ml用EtOH在3,600×g下使粒子沉淀，离心10分钟。 </li><li>弃去上清液，并在总共10毫升正己烷的再分散的粒料。 </li><li>离心该溶液（3 600 XG，10分钟）再次以除去任何不溶性杂质，被倾入一个样品管之前，并储存在冰箱（4℃）在氮气氛下长达三个月。 </li></ol></li></ol> 2.纳米颗粒的封装肿胀到PDMS <ol><li> 肿胀液的配制: <ol><li>通过混合36毫升正己烷用4ml的CdSe量子点分散体（如合成）制备的CdSe量子点的储备溶液和磁力搅拌该溶液中。&lt;/ LI&gt; <li>预留每个由9毫升原液作为指定肿胀溶液两小瓶。 </li><li>使用的原液的不同QD浓度的进一步肿胀方案编制的剩余部分。通过稀释原液，得到66％（体积/体积）溶液，50％溶液和33％的溶液制备降低QD浓度三个肿胀的解决方案。 <ol><li>通过混合6毫升所述的CdSe QD原液用3毫升正己烷制备66％（体积/体积）溶液。搅拌溶液磁，以确保完全混合。 </li><li>通过混合4.5毫升所述的CdSe QD原液用4.5毫升正己烷制备50％（体积/体积）溶液。搅拌溶液磁，以确保完全混合。 </li><li>通过混合将3ml的CdSe QD原液用6ml正己烷制备33％（体积/体积）溶液。搅拌溶液磁，以确保完全混合。 </li></ol></li><li>存储所有黑暗的条件下，QD的解决方案，在室温下。&lt;/ LI&gt; </ol></li><li> 聚合物的制备和QD融合-在改变肿胀液的浓度QD: <ol><li>剪下用一个新的手术刀刀片四家医疗级硅胶广场（11毫米×11毫米）。 </li><li>在每个不同％QD浓度的四个溶胀溶液的浸入医用级硅氧烷正方形:储备溶液，66％（V / V），50％（体积/体积）和33％（体积/体积）。允许聚合物样品溶胀黑暗条件下24小时，并在室温下。 </li><li> 48小时，在此期间中的残留溶剂蒸发，聚合物收缩回其初始尺寸除去黑暗条件下从相应的溶胀溶液和空气干燥溶胀的聚合物样品。 </li><li>用去离子水彻底清洗QD-掺入样品以除去任何表面结合的材料。 </li></ol></li><li> 聚合物的制备和QD融合-改变聚合物曝光时间去肿解决方案: </strong&gt;的<ol><li>制备四种多医用级硅氧烷正方形（11毫米×11毫米），如在2.2.1说明。 </li><li>沉浸在股票溶胀溶液的医用级硅酮平方用于改变时间周期:1小时，3小时，6小时和24小时。 </li><li>从溶胀溶液除去后，空气干燥黑暗条件下溶胀的聚合物样品48小时，使得样品收缩回其以前的尺寸。 </li><li>用去离子水彻底清洗QD-掺入样品以除去任何表面结合材料或残余溶剂。 </li></ol></li></ol> 3.纳米可视化骤升到封装PDMS <ol><li> 硅胶试样制备: <ol><li>切出两个硅氧烷广场用新鲜的手术刀刀片（5.5毫米×11毫米）。确保此公开硅氧烷样品的内表面。 </li></ol></li><li> 荧光成像: <ol><li>将硅样品上microsco用于成像的pe滑动，确保聚合物的新切割面，使与载玻片完全接触。按硅氧烷部分轻轻向下，以确保与载玻片平滑的接触。将样品在显微镜的阶段。 </li><li>完整寿命荧光测量使用488nm的光谱滤光的激光线在20MHz或类似的速率包含5皮秒脉冲。23使用一个声光调谐滤光器系统中，可直接联接到激光输出，以生成488纳米激光线。用一个定制的激光扫描单元（参见补充信息），它是由二向色镜（488纳米）转换成10X物镜的后孔径反射，然后到样品聚焦的​​激光束。 <ol><li>收集具有相同目标的荧光发射，这之后，通过相同的分色镜。这直接朝着光的雪崩光电二极管单光子计数模式下工作。流程lifeti<html>我23测量使用时间相关单光子计数（TCSPC）板。 </li></ol></li><li>记录在开头的仪器响应函数（IRF）和各实验会话结束23 注意:在TCSPC实验中的记录的信号应显示在检测器的光子到达和生产随后的激光脉冲之间的时间延迟。这个时间延迟然而，应与测量装置的IRF进行卷积。因此，在IRF被作为仪器至100nM金胺O，从而具有相对于仪器响应一个显著寿命较短（约100皮秒）的反应测定。 </li><li>提取由荧光强度的指数衰减的非线性拟合的寿命和使用最大似然估计（MLE）算法25-27从IRF解卷积此。最大似然估计（γj）的计算为 eq1.jpg"/&gt; 其中，n i是在信道i光子计数的数目，k是信道（或容器）的每个荧光衰变的数目，P I（j）是一组的光子会落在信道，如果我的颗粒具有的概率一生j和N是数为给定的衰减的总数量。 </li><li>记录每个样品的荧光强度和寿命数据5分钟，创造了连续扫描由264的图像的大小为512×512像素。结合这提供二维荧光强度，寿命和强度加权终身地图，计算MLE拥有150光子阈值，这个过程用MATLAB。 </li></ol></li></ol>

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C., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Doping+Group+IIB+Metal+Ions+into+Quantum+Dot+Shells+via+the+One-Pot+Decomposition+of+Metal-Dithiocarbamates.">Doping Group IIB Metal Ions into Quantum Dot Shells via the One-Pot Decomposition of Metal-Dithiocarbamates.</a> Adv. Opt. Mater. 3 (5), 704-712 (2015).</li><li>Li, L., Hu, J., Yang, W., Alivisatos, A. P. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Band+Gap+Variation+of+Size-+and+Shape-Controlled+Colloidal+CdSe+Quantum+Rods.">Band Gap Variation of Size- and Shape-Controlled Colloidal CdSe Quantum Rods.</a> Nano Letters. 1 (7), 349-351 (2001).</li></ol>

The authors have nothing to disclose.

Cross-sectional fluorescence imaging allows for direct visualization of nanoparticles during swell encapsulation. The kinetics of encapsulation has been shown, with the drive toward a high nanoparticle surface concentration demonstrated. The extent of nanoparticle incorporation is shown to vary with swell encapsulation time (described in section 2.3), with the total amount of incorporated nanoparticles increasing as this time is extended, with the particle concentration localized at the surface if the polymer samples are...

纳米材料的应用曾长期担任增加对新技术感兴趣的一个领域。1-3这包括越来越多地使用的日常用品，包括化妆品，服装，包装，电子纳米粒子的4-6倾向于使用纳米颗粒的主要驱动器在功能性材料从较高相对于材料它们的反应性茎，除了在颗粒尺寸的能力来调整属性由变异7另一个优点是容易地形成的复合材料的能力，引入关键属性的基质，如催化功能材料的强化和电性能的调优。8-12 其中最简单的纳米颗粒-聚合物复合材料可通过一系列的技术来实现，是基质的制造过程中直接整合所需的纳米粒子。13,14该Results在均质材料均匀间距的纳米材料贯穿始终。然而，许多应用仅仅要求活性物质存在于纳米复合材料的外部接口。其结果是，直接掺入不导致有效地使用有时昂贵纳米材料作为存在通过散装的材料的多纳米颗粒废物。15,16为了实现直接掺入，纳米颗粒还必须与主体基质形成兼容。这可能是具有挑战性的，尤其是在要求多面的反应，如在通常由可以由高活性的纳米颗粒的影响金属配合物催化剂的机制促进热固性聚合物的情况下合成。14 聚合物合成过程中直接​​纳米粒子掺入相关联的相当大的缺点，已导致的技术旨在限制纳米颗粒incorporati发展到表面层。17-21胀大封装是在文献中报道的最成功的策略之一，以实现高的表面的纳米粒子的浓度，与在聚合物本体有限浪费。17-19该技术利用聚合物的溶剂从动溶胀矩阵，允许分子种类和纳米颗粒的侵入。在除去溶胀溶剂，在基质内的物种成为固定到位，以在表面局部物种的浓度最高。迄今为止，大多数膨胀包封的报道使用均朝向抗微生物聚合物的制造中，在那里它是关键的活性剂是在该材料的表面上。虽然许多这些报告显示增强的抗菌活性，精确的表面的纳米颗粒组合物进行详细很少探测。克里克等人最近证明为纳米粒子侵入的直接可视化的方法，提供了重要的INSIGHT成涌浪封装实现动力学和表面的纳米颗粒的浓度。22 这个工作详细硒化镉量子点（QD），其溶胀封装到聚二甲基硅氧烷（PDMS），并使用荧光成像它们掺入的直接可视化的合成。变溶胀封装时间和纳米粒子的浓度在溶胀溶液的效果进行了探索。荧光可视化技术允许纳米粒子侵入的直接成像到PDMS并表明量子点的最高浓度是在该材料的表面上。

<table><tbody><tr><td>Polydimethylsiloxane sheets</td><td>NuSil</td><td>-</td><td>Medical Grade</td></tr><tr><td>Oleylamine</td><td>Sigma Aldrich</td><td>O7805</td><td>Technical Grade</td></tr><tr><td>Trioctylphosphine</td><td>Sigma Aldrich</td><td>117854</td><td>Technical Grade</td></tr><tr><td>Trioctylphosphine oxide</td><td>Sigma Aldrich</td><td>346187</td><td>Technical Grade</td></tr><tr><td>1-Octadecene</td><td>Sigma Aldrich</td><td>O806</td><td>Technical Grade</td></tr><tr><td>Zinc diethyldithiocarbamate</td><td>Sigma Aldrich</td><td>329703</td><td>-</td></tr><tr><td>Oleic acid</td><td>Sigma Aldrich</td><td>364525</td><td>Technical Grade</td></tr><tr><td>Triethylamine</td><td>Sigma Aldrich</td><td>471283</td><td>-</td></tr><tr><td>Cadmium oxide</td><td>Alfa Aesar</td><td>33235</td><td>-</td></tr><tr><td>Hexadecylamine</td><td>Alfa Aesar</td><td>B22459</td><td>Technical Grade</td></tr><tr><td>1-Dodecylphosphonic acid</td><td>Alfa Aesar</td><td>H26259</td><td>-</td></tr><tr><td>Selenium powder</td><td>Acros</td><td>19807</td><td>-</td></tr><tr><td>Chloroform</td><td>Sigma Aldrich</td><td>366919</td><td>-</td></tr><tr><td>n-Hexane</td><td>Sigma Aldrich</td><td>208752</td><td>-</td></tr><tr><td>Microscope slides</td><td>VWR</td><td>631-0137</td><td>Thickness No. 1</td></tr></tbody></table>

advanced compositional analysis of nanoparticle-polymer composites using direct fluorescence imaging

The fabrication of polymer-nanoparticle composites is extremely important in the development of many functional materials. Identifying the precise composition of these materials is essential, especially in the design of surface catalysts, where the surface concentration of the active component determines the activity of the material. Antimicrobial materials which utilize nanoparticles are a particular focus of this technology. Recently swell encapsulation has emerged as a technique for inserting antimicrobial nanoparticles into a host polymer matrix. Swell encapsulation provides the advantage of localizing the incorporation to the external surfaces of materials, which act as the active sites of these materials. However, quantification of this nanoparticle uptake is challenging. Previous studies explore the link between antimicrobial activity and surface concentration of the active component, but this is not directly visualized. Here we show a reliable method to monitor the incorporation of nanoparticles into a polymer host matrix via swell encapsulation. We show that the surface concentration of CdSe/ZnS nanoparticles can be accurately visualized through cross-sectional fluorescence imaging. Using this method, we can quantify the uptake of nanoparticles via swell encapsulation and measure the surface concentration of encapsulated particles, which is key in optimizing the activity of functional materials.

量子点表现出红色荧光，与λ最大值的大约600纳米。22,28的红色发射是由于激子由量子棒，其大小尺寸的强约束状态中的限制。 Li等人表明，量子棒，发射移动到与增加宽度或所述杆的长度降低能源。他们进一步发现，发射主要由横向限制，即使当杆是很长的，特别是当宽度小于有问题，因为它是在强约束状态的材料的玻尔半径起着重要的作用来确定。29...

Watch this Scientific Journal Video about Advanced Compositional Analysis of Nanoparticle-polymer Composites Using Direct Fluorescence Imaging at JoVE.com

Advanced Compositional Analysis of Nanoparticle-polymer Composites Using Direct Fluorescence Imaging

Here we present a reliable method to monitor the incorporation of nanoparticles into a polymer host matrix via swell encapsulation. We show that the surface concentration of cadmium selenide quantum dots can be accurately visualized through cross-sectional fluorescence imaging.

纳米粒子 - 聚合物复合材料使用直接荧光成像的先进成分分析

The fabrication of polymer-nanoparticle composites is extremely important in the development of many functional materials. Identifying the precise ...

advanced-compositional-analysis-nanoparticle-polymer-composites-using

Research

JoVE Journal

Engineering

7.7K 次观看.  Imperial College London. Here we present a reliable method to monitor the incorporation of nanoparticles into a polymer host matrix via swell encapsulation. We show that the surface concentration of cadmium selenide quantum dots can be accurately visualized through cross-sectional fluorescence imaging.

视频: Advanced Compositional Analysis of Nanoparticle-polymer Composites Using Direct Fluorescence Imaging

Confocal Imaging of Confined Quiescent and Flowing Colloid-polymer Mixtures

The behavior of confined colloidal suspensions with attractive interparticle interactions is critical to the rational design of materials for directed assembly1-3, drug delivery4, improved hydrocarbon recovery5-7, and flowable electrodes for energy storage8. Suspensions containing fluorescent colloids and non-adsorbing polymers are appealing model systems, as the ratio of the polymer radius of gyration to the particle radius&#160;and concentration of polymer control the range and strength of the interparticle attraction, respectively. By tuning the polymer properties and the volume fraction of the colloids, colloid fluids, fluids of clusters, gels, crystals, and glasses can be obtained9.&#160;Confocal microscopy, a variant of fluorescence microscopy, allows an optically transparent and fluorescent sample to be imaged with high spatial and temporal resolution in three dimensions. In this technique, a small pinhole or slit blocks the emitted fluorescent light from regions of the sample that are outside the focal volume of the microscope optical system. As a result, only a thin section of the sample in the focal plane is imaged. This technique is particularly well suited to probe the structure and dynamics in dense colloidal suspensions at the single-particle scale: the particles are large enough to be resolved using visible light and diffuse slowly enough to be captured at typical scan speeds of commercial confocal systems10. Improvements in scan speeds and analysis algorithms have also enabled quantitative confocal imaging of flowing suspensions11-16,37.&#160;In this paper, we demonstrate confocal microscopy experiments to probe the confined phase behavior and flow properties of colloid-polymer mixtures. We first prepare colloid-polymer mixtures that are density- and refractive-index matched. Next, we report a standard protocol for imaging quiescent dense colloid-polymer mixtures under varying confinement in thin wedge-shaped cells. Finally, we demonstrate a protocol for imaging colloid-polymer mixtures during microchannel flow.

Confocal microscopy is used to image quiescent and flowing colloid-polymer mixtures, which are studied as model systems for attractive suspensions. Image analysis algorithms are used to calculate structural and dynamic metrics for the colloidal particles that measure changes due to geometric confinement.

密闭静态和流动胶体聚合物混合物的共聚焦成像

The behavior of confined colloidal suspensions with attractive interparticle interactions is critical to the rational design of materials for directed ...

科研

化学

Combinatorial Synthesis of and High-throughput Protein Release from Polymer Film and Nanoparticle Libraries

Polyanhydrides are a class of biomaterials with excellent biocompatibility and drug delivery capabilities. While they have been studied extensively with conventional one-sample-at-a-time synthesis techniques, a more recent high-throughput approach has been developed enabling the synthesis and testing of large libraries of polyanhydrides1. This will facilitate more efficient optimization and design process of these biomaterials for drug and vaccine delivery applications. The method in this work describes the combinatorial synthesis of biodegradable polyanhydride film and nanoparticle libraries and the high-throughput detection of protein release from these libraries. In this robotically operated method (Figure 1), linear actuators and syringe pumps are controlled by LabVIEW, which enables a hands-free automated protocol, eliminating user error. Furthermore, this method enables the rapid fabrication of micro-scale polymer libraries, reducing the batch size while resulting in the creation of multivariant polymer systems. This combinatorial approach to polymer synthesis facilitates the synthesis of up to 15 different polymers in an equivalent amount of time it would take to synthesize one polymer conventionally. In addition, the combinatorial polymer library can be fabricated into blank or protein-loaded geometries including films or nanoparticles upon dissolution of the polymer library in a solvent and precipitation into a non-solvent (for nanoparticles) or by vacuum drying (for films). Upon loading a fluorochrome-conjugated protein into the polymer libraries, protein release kinetics can be assessed at high-throughput using a fluorescence-based detection method (Figures 2 and 3) as described previously1. This combinatorial platform has been validated with conventional methods2 and the polyanhydride film and nanoparticle libraries have been characterized with 1H NMR and FTIR. The libraries have been screened for protein release kinetics, stability and antigenicity; in vitro cellular toxicity, cytokine production, surface marker expression, adhesion, proliferation and differentiation; and in vivo biodistribution and mucoadhesion1-11. The combinatorial method developed herein enables high-throughput polymer synthesis and fabrication of protein-loaded nanoparticle and film libraries, which can, in turn, be screened in vitro and in vivo for optimization of biomaterial performance.

This method describes the combinatorial synthesis of biodegradable polyanhydride film and nanoparticle libraries and the high-throughput detection of protein release from these libraries.

组合合成和高通量的蛋白质释放的聚合物薄膜和纳米粒子库

Polyanhydrides are a class of biomaterials with excellent biocompatibility and drug delivery capabilities. While they have been studied extensively with ...

生物工程

Electroactive Polymer Nanoparticles Exhibiting Photothermal Properties

A method for the synthesis of electroactive polymers is demonstrated, starting with the synthesis of extended conjugation monomers using a three-step process that finishes with Negishi coupling. Negishi coupling is a cross-coupling process in which a chemical precursor is first lithiated, followed by transmetallation with ZnCl2. The resultant organozinc compound can be coupled to a dibrominated aromatic precursor to give the conjugated monomer. Polymer films can be prepared via electropolymerization of the monomer and characterized using cyclic voltammetry and ultraviolet-visible-near infrared (UV-Vis-NIR) spectroscopy. Nanoparticles (NPs) are prepared via emulsion polymerization of the monomer using a two-surfactant system to yield an aqueous dispersion of the polymer NPs. The NPs are characterized using dynamic light scattering, electron microscopy, and UV-Vis-NIR-spectroscopy. Cytocompatibility of NPs is investigated using the cell viability assay. Finally, the NP suspensions are irradiated with a NIR laser to determine their effectiveness as potential materials for photothermal therapy (PTT).

A protocol is presented for the synthesis and preparation of nanoparticles consisting of electroactive polymers.

电活性聚合物纳米粒子参展光热特性

A method for the synthesis of electroactive polymers is demonstrated, starting with the synthesis of extended conjugation monomers using a three-step ...

工程学

Controlled Synthesis and Fluorescence Tracking of Highly Uniform Poly(N-isopropylacrylamide) Microgels

Stimuli-sensitive poly(N-isopropylacrylamide) (PNIPAM) microgels have various prospective practical applications and uses in fundamental research. In this work, we use single particle tracking of fluorescently labeled PNIPAM microgels as a showcase for tuning microgel size by a rapid non-stirred precipitation polymerization procedure. This approach is well suited for prototyping new reaction compositions and conditions or for applications that do not require large amounts of product. Microgel synthesis, particle size and structure determination by dynamic and static light scattering are detailed in the protocol. It is shown that the addition of functional comonomers can have a large influence on the particle nucleation and structure. Single particle tracking by wide-field fluorescence microscopy allows for an investigation of the diffusion of labeled tracer microgels in a concentrated matrix of non-labeled microgels, a system not easily investigated by other methods such as dynamic light scattering.

Controlled Synthesis and Fluorescence Tracking of Highly Uniform PolyN-isopropylacrylamide Microgels

Non-stirred precipitation polymerization provides a rapid, reproducible prototyping approach to the synthesis of stimuli-sensitive poly(N-isopropylacrylamide) microgels of narrow size distribution. In this protocol synthesis, light scattering characterization and single particle fluorescence tracking of these microgels in a wide-field microscopy setup are demonstrated.

可控合成和高度统一聚荧光追踪（<em&gt;ñ</em&gt; -isopropylacrylamide）微凝胶

Stimuli-sensitive poly(N-isopropylacrylamide) (PNIPAM) microgels have various prospective practical applications and uses in fundamental research. In this ...

Synthesis of Cyclic Polymers and Characterization of Their Diffusive Motion in the Melt State at the Single Molecule Level

We demonstrate a method for the synthesis of cyclic polymers and a protocol for characterizing their diffusive motion in a melt state at the single molecule level. An electrostatic self-assembly and covalent fixation (ESA-CF) process is used for the synthesis of the cyclic poly(tetrahydrofuran) (poly(THF)). The diffusive motion of individual cyclic polymer chains in a melt state is visualized using single molecule fluorescence imaging by incorporating a fluorophore unit in the cyclic chains. The diffusive motion of the chains is quantitatively characterized by means of a combination of mean-squared displacement (MSD) analysis and a cumulative distribution function (CDF) analysis. The cyclic polymer exhibits multiple-mode diffusion which is distinct from its linear counterpart. The results demonstrate that the diffusional heterogeneity of polymers that is often hidden behind ensemble averaging can be revealed by the efficient synthesis of the cyclic polymers using the ESA-CF process and the quantitative analysis of the diffusive motion at the single molecule level using the MSD and CDF analyses.

A protocol for the synthesis and characterization of diffusive motion of cyclic polymers at the single molecule level is presented.

环状聚合物的合成及其在熔融状态扩散运动的表征在单分子水平

We demonstrate a method for the synthesis of cyclic polymers and a protocol for characterizing their diffusive motion in a melt state at the single ...

Performing Spectroscopy on Plasmonic Nanoparticles with Transmission-Based Nomarski-Type Differential Interference Contrast Microscopy

Differential interference contrast (DIC) microscopy is a powerful imaging tool that is most commonly employed for imaging microscale objects using visible-range light. The purpose of this protocol is to detail a proven method for preparing plasmonic nanoparticle samples and performing single particle spectroscopy on them with DIC microscopy. Several important steps must be followed carefully in order to perform repeatable spectroscopy experiments. First, landmarks can be etched into the sample substrate, which aids in locating the sample surface and in tracking the region of interest during experiments. Next, the substrate must be properly cleaned of debris and contaminants that can otherwise hinder or obscure examination of the sample. Once a sample is properly prepared, the optical path of the microscope must be aligned, using Kohler Illumination. With a standard Nomarski style DIC microscope, rotation of the sample may be necessary, particularly when the plasmonic nanoparticles exhibit orientation-dependent optical properties. Because DIC microscopy has two inherent orthogonal polarization fields, the wavelength-dependent DIC contrast pattern reveals the orientation of rod-shaped plasmonic nanoparticles. Finally, data acquisition and data analyses must be carefully performed. It is common to represent DIC-based spectroscopy data as a contrast value, but it is also possible to present it as intensity data. In this demonstration of DIC for single particle spectroscopy, the focus is on spherical and rod-shaped gold nanoparticles.

The goal of this protocol is to detail a proven approach for the preparation of plasmonic nanoparticle samples and for performing single particle spectroscopy on them with differential interference contrast (DIC) microscopy.

基于传输的野武学型差分干涉对比显微镜对等离子体纳米粒子的光谱处理

Differential interference contrast (DIC) microscopy is a powerful imaging tool that is most commonly employed for imaging microscale objects using ...

通过纳米级红外光谱探索多相聚合物系统

Advances in Nanoscale Infrared Spectroscopy to Explore Multiphase Polymeric Systems

Multiphase polymeric systems encompass local domains with dimensions that can vary from a few tens of nanometers to several micrometers. Their composition is commonly assessed using infrared spectroscopy, which provides an average fingerprint of the various materials contained in the volume probed. However, this approach does not offer any details on the arrangement of the phases in the material. Interfacial regions between two polymeric phases, often in the nanoscale range, are also challenging to access. Photothermal nanoscale infrared spectroscopy monitors the local response of materials excited by infrared light with the sensitive probe of an atomic force microscope (AFM). While the technique is suitable for interrogating small features, such as individual proteins on pristine gold surfaces, the characterization of three-dimensional multicomponent materials is more elusive. This is due to a relatively large volume of material undergoing photothermal expansion, defined by the laser focalization onto the sample and by the thermal properties of the polymeric constituents, compared to the nanoscale region probed by the AFM tip. Using a polystyrene (PS) bead and a polyvinyl alcohol (PVA) film, we evaluate the spatial footprint of photothermal nanoscale infrared spectroscopy for surface analysis as a function of the position of PS in the PVA film. The effect of the feature position on the nanoscale infrared images is investigated, and spectra are acquired. Some perspectives on the future advances in the field of photothermal nanoscale infrared spectroscopy are provided, considering the characterization of complex systems with embedded polymeric structures.

作者聚焦:探索多相聚合物系统的纳米级红外光谱进展  

This protocol describes the application of atomic force microscopy and nanoscale infrared spectroscopy to evaluate the performance of photothermal nanoscale infrared spectroscopy in the characterization of three-dimensional multi-polymeric samples.

纳米级红外光谱探索多相聚合物体系的进展

Multiphase polymeric systems encompass local domains with dimensions that can vary from a few tens of nanometers to several micrometers. Their composition ...

A Quantitative Fluorescence Microscopy-based Single Liposome Assay for Detecting the Compositional Inhomogeneity Between Individual Liposomes

Most research employing liposomes as membrane model systems or drug delivery carriers relies on bulk read-out techniques and thus intrinsically assumes all liposomes of the ensemble to be identical. However, new experimental platforms able to observe liposomes at the single-particle level have made it possible to perform highly sophisticated and quantitative studies on protein-membrane interactions or drug carrier properties on individual liposomes, thus avoiding errors from ensemble averaging. Here we present a protocol for preparing, detecting, and analyzing single liposomes using a fluorescence-based microscopy assay, facilitating such single-particle measurements. The setup allows for imaging individual liposomes in a massive parallel manner and is employed to reveal intra-sample size and compositional inhomogeneities. Additionally, the protocol describes the advantages of studying liposomes at the single liposome level, the limitations of the assay, and the important features to be considered when modifying it to study other research questions.

This protocol describes the fabrication of liposomes and how these can be immobilized on a surface and imaged individually in a massive parallel manner using fluorescence microscopy. This allows for the quantification of the size and compositional inhomogeneity between single liposomes of the population.

定量荧光显微镜为基础的单脂体测定，用于检测单个脂质体之间的成分不均匀性

Most research employing liposomes as membrane model systems or drug delivery carriers relies on bulk read-out techniques and thus intrinsically assumes ...

纳米粒子 - 聚合物复合材料使用直接荧光成像的先进成分分析

摘要

探索更多视频

此视频中的章节

密闭静态和流动胶体聚合物混合物的共聚焦成像

组合合成和高通量的蛋白质释放的聚合物薄膜和纳米粒子库

电活性聚合物纳米粒子参展光热特性

可控合成和高度统一聚荧光追踪（

环状聚合物的合成及其在熔融状态扩散运动的表征在单分子水平

基于传输的野武学型差分干涉对比显微镜对等离子体纳米粒子的光谱处理

纳米级红外光谱探索多相聚合物体系的进展

纳米级红外光谱探索多相聚合物体系的进展

纳米级红外光谱探索多相聚合物体系的进展

定量荧光显微镜为基础的单脂体测定，用于检测单个脂质体之间的成分不均匀性