作者承认提供的财政支持荷兰科学研究组织（NWO ECHO-STIP格兰特717.013.005，NWO VIDI格兰特723.014.006）。

1.核壳型二氧化硅颗粒的合成 注意:二氧化硅颗粒根据以下程序，这是基于STOBER方法24,25合成。 <ol><li> 荧光硅种子的合成 <ol><li>溶解荧光素异硫氰酸酯在5毫升乙醇中的105毫克（0.27毫摩尔）。 </li><li>加入100微升（3-氨基丙基）三乙氧基硅烷（APTES，0.43毫摩尔）到先前溶液中。 </li><li> 5分钟内超声处理溶液，并让它在室温下在氩气气氛下反应过夜，同时搅拌。染料 - 官能APTES复合使用，无需纯化。 </li><li>在一个1升圆底烧瓶中混合2.5毫升用25ml氨水（在水中25％）和250毫升乙醇的染料官能APTES的。 </li><li>上述反应混合物的弯液面下加入10 mL硅酸四乙酯（TEOS）的用玻璃吸管控制而的帮助e为磁搅拌器搅拌。 </li><li>同样地，5小时后，添加另外1.75 TEOS中并在氩气氛下过夜搅拌该混合物。 </li><li>倒入分散成几个45毫升管。 </li><li>离心管（350 XG，30分钟），除去上清液，并添加30毫升新鲜乙醇在每个管。再次超声处理3分钟的新的分散体，和离心机以除去上清液。重复这些步骤洗涤3次。 </li><li>保持在乙醇荧光种子在约13.6毫克/毫升的浓度，并在黑暗中（避免暴露于光）。 </li><li>制备非荧光种子按照相同的程序省略了除荧光染料。 注意:在此之后的步骤，获得在半径约100nm的种子。 </li></ol></li><li> 核壳型二氧化硅颗粒的合成 <ol><li>补的1L圆底烧瓶用51毫升乙醇，17个毫升去离子水，3.4氨毫升（在水中25％）和4-毫升种子分散体（54.4毫克荧光种子约）。 </li><li>填充塑料注射器用5ml的TEOS和10ml乙醇。 </li><li>补的第二塑料注射器1.34毫升氨（在水中25％），3.4毫升去离子水10.25毫升乙醇。 </li><li>两个注射器连接到圆底烧瓶用塑料管。 </li><li>装备用氩流量和磁力搅拌器的烧瓶中。氩入口具有被旁边的第二注射器，以避免从TEOS液滴氨气之间的接触，以防止二次成核的出口。 </li><li>在同一时间同时添加注射器的内容在使用蠕动泵同时搅拌该混合物1.7毫升/小时。确保获得自由下落的液滴，以避免滑翔墙壁，因此二次核上。 </li><li>停止加入后7小时以获得约300nm的核 - 壳粒子在半径。 </li><li>倒入烧瓶内容分成几个45毫升管中。 </li><li>离心管（350 XG，30分钟），除去上清液，并添加30毫升新鲜乙醇在每个管。再次超声处理3分钟的新的分散性，和离心机以除去上清液。重复这些步骤洗涤3次。 </li><li>保持核 - 壳粒子在乙醇中，在黑暗中（避免暴露于光）。 </li><li>准备按照相同的程序，但使用的非荧光种子非荧光二氧化硅颗粒。 </li></ol></li></ol> 2.二氧化硅胶体的功能化<ol><li> NVOC功能化胶体的合成 <ol><li>分散10毫克核壳型二氧化硅颗粒在1ml乙醇与12在50毫升圆底烧瓶硬脂醇的NVOC-C11-OH分子的毫克（0.03毫摩尔）和31毫克（0.11毫摩尔）（所得一起在20/80 NVOC-C11-OH /硬脂醇的摩尔比）。 </li><li>超声处理该混合物10分钟，以确保所有的分子被溶解和颗粒是很好dispeRSED。 </li><li>添加到该混合物磁力搅拌棒并用在室温下的氩源源不断蒸发乙醇。在继续之前，确保没有乙醇左，否则它会与粒子的硅烷醇基团反应。检查乙醇是否完全蒸发讲究烧瓶底部的温度。如果感觉冷，乙醇尚未完全蒸发。 </li><li>加热在连续搅拌下和在氩气下22源源不断烧瓶至180℃6小时。 </li><li>让烧瓶冷却到室温。 </li><li>添加3毫升三氯甲烷的到烧瓶中，并超声处理5分钟（或直到所有的固体成分已溶解或分散）。 </li><li>离心分散（2600 XG，4分钟），除去上清液，加入新鲜氯仿 。再次超声处理3分钟的新的分散性，和离心机以除去上清液。重复这些步骤洗6次。 </l我&gt; <li>干燥在70℃下在真空中粒子过夜，并将它们存储在一个干燥器中。 </li></ol></li><li> BTA-胶体的合成 <ol><li>分散10毫克在3ml 氯仿的NVOC-C11-OH /硬脂醇的20/80摩尔比官能化粒子。 </li><li>照射在UV烘箱（λ 最大 = 354纳米）的分散体1小时，以裂解NVOC基。确保该脱保护是在颗粒的表面上均匀通过用磁力搅拌器温和地搅拌该分散液的同时脱保护。这产生了胺官能化粒子（ 图1a）。 </li><li>溶解9毫克苯-1,3,5- tricarboxamide衍生物（BTA，0.01毫摩尔），8.7微升的N，N-二异丙基乙胺（DIPEA，0.05毫摩尔）和5.2毫克（苯并三唑-1-基氧基）三吡咯烷基六氟磷酸盐的（加入PyBOP，0.01毫摩尔）在1毫升氯仿中。 </li><li>该解决方案添加到胺官能p制品的分散性和在室温下和在氩气氛下搅拌过夜。 </li><li>离心分散（2600 XG，4分钟），除去上清液，加入3毫升新鲜氯仿的。再次超声处理3分钟的新的分散性，和离心机以除去上清液。重复这些步骤洗6次。 </li><li>干燥在70℃下该颗粒在真空中进行48小时，并把它们存储在一个干燥器中。 </li></ol></li></ol> 3.静态光散射测量（SLS） 注意:使用非荧光颗粒，由于荧光芯吸收波长相同的常规的光散射设备入射激光的光。 <ol><li>官能10毫克非荧光二氧化硅颗粒与硬脂醇只（无NVOC-C11-OH）以下在2.1节中描述的方法。 </li><li>制备500微升0.033毫克/毫升的非官能化粒子的分散液的水和一个的2毫克/毫升的环己烷硬脂涂覆醇颗粒的另一个。 </li><li>超声处理两分散体为至少20分钟，以确保颗粒被很好地分散。 </li><li>同时测量分散体的散射强度，将溶剂和从30° ​​至120°5°步骤基准溶剂。 </li><li>画出样品（Ⅰ 样品 ）的强度作为q的函数 （公式1）Q =4πñ 溶剂罪（θ/ 2）/λ0 与散射角θ，溶剂Ñ 溶剂的折射率和激光λ0的波长。 </li><li>利用软件将数据装配到下面的公式（ 例如 ，起源） （式2）I 采样 = CP（QR） 其中，C是由下式给出一个恒定和形式因数P（QR） （等式3）&lt;IMG ALT ="等式3"SRC ="/文件/ ftp_upload / 53934 / 53934eq3.jpg"/&gt; 其中球形胶体的平均半径为R。 </li><li>从适合每个分散提取R上 。 </li><li>计算瑞利比（Rθ），这是对于散射光的强度的绝对度量，根据以下等式，针对每个θ。 （公式4） <img alt="公式4" src="/files/ftp_upload/53934/53934eq4.jpg" /> 与样本的强度，溶剂和参考， 我 样 ， 我 溶剂 和I分别引用 ，溶剂的折射率和参考Ñ 溶剂和n 参考 ，相应地，与参考R 参考的瑞利比。在这里使用甲苯作为参考，使得n 水 = 1.332，N 甲苯 = 1.497，N = 环己烷 1.426; R 甲苯 = 2.74x10 -3米-1 26。 </li><li>计算自Rθ和等式5的胶体（ 正胶体 ）的平均折射率。 （式5） <img alt="公式5" src="/files/ftp_upload/53934/53934eq5.jpg" /> 与每体积N，用V 粒子发出的粒子v 颗粒的体积的颗粒数= 4/3πR3，并假设该结构系数S（q）的〜1，这是无相互作用颗粒的限制。 </li></ol> 4.定量活性中心每个粒子的数注意:在半径使用13纳米的小颗粒（具有较大的表面，以-volume比）。 <ol><li>功能化与/硬脂以下2.1节中描述的步骤酒精NVOC-C11-OH的20/80摩尔比小市售颗粒。 </li><li>分散20毫克小，官能化粒子在1ml CHCl 3中，照射在UV烘箱（λ 最大 = 354纳米）的分散体1小时，以裂解NVOC基。用磁力搅拌棒轻轻搅拌分散体，同时脱保护。以这种方式，胶体不沉降和它们的表面保持暴露于UV光，从而确保均匀的脱保护。 </li><li>降速所得胺官能颗粒（3400 xg离心，10分钟），去除上清。 </li><li>干燥的颗粒在70℃下2小时。 </li><li>溶解0.50毫克琥珀酰亚胺基3-（2-吡啶基）丙酸酯（SPDP，0.0016毫摩尔）在200微升二甲基甲酰胺（DMF）中的。 </li><li>的SPDP溶液添加到20毫克的干燥胺官能颗粒和涡流的系统30分钟。在这段时间内，对胶体所有可用伯胺已与SPDP反应。 </li><li>用1毫升DMF中的6次洗涤颗粒（或直到无游离的SPDP在上清液在λ= 375纳米的检测通过UV-Vis光谱）。在最后的洗涤步骤尝试去除尽可能多的上清液越好。 </li><li>在50μlDMF中溶解0.53毫克二硫苏糖醇（DTT，0.0034毫摩尔）。添加DTT溶液的颗粒和涡分散30分钟。在这段时间内的吡啶-2-硫酮基团被裂解。 </li><li>确定自由上清液中释放的吡啶-2-硫酮的在λ= 293纳米用微量紫外可见分光光度计的吸光度。 </li><li>构建一个校准曲线通过测定系列稀释的不同的已知量的SPDP的吸光度与过量的DTT，以确定在DMF吡啶-2-硫酮的消光系数ɛ（〜12.1x10 3 M -1 -1） 。 </li><li&gt;计算吡啶-2-硫酮，C P2T，它是从使用朗伯-比尔定律颗粒裂解的浓度: （公式6）ABS = C P2Tε升 用吡啶-2-硫酮çP2T的摩尔浓度，消光系数ɛ和路径长度l。 </li><li>计算每个颗粒的活性位点（胺）的数量用下面的方程 （式7） <img alt="公式7" src="/files/ftp_upload/53934/53934eq7.jpg" /> 与一种粒子M 粒子的质量 这是M 粒子 = 4 /3πR3ρ，用ρ= 1.295克/厘米3，颗粒M1 总 （20毫克）和总体积V 总 （50微升）的总加权质量。该公式假设所有可用胺与SPDP的反应和DTT减少附着在颗粒所有SPDP的分子。 </li></ol> 5.显示器胶体大会激光共聚焦显微镜注意:使用的核壳型二氧化硅颗粒（用荧光芯和非荧光壳）。 <ol><li>制备400μl的在环己烷BTA-官能化粒子的0.1％（重量）的分散体和超声处理的样品20分钟。 </li><li>照射在UV炉样品瓶（λ 最大 = 354纳米）切割掉BTA的邻硝基组。采取25微升等分试样在照射不同的时间，例如从0到30分钟，以监测聚类过程。 </li><li>放置在与间隔的帮助不同载玻片的不同等分试样，并用盖玻片封闭腔室（腔室尺寸为13mm直径×0.12毫米高度）。关闭室后，打开盖玻片倒置，让颗粒泥沙及adsorb到玻璃，这便于成像。 </li><li>每次照射时间为样品制备后尽快取每个样品的若干图片包含共焦显微镜。 </li></ol> 6.图像分析<ol><li> 用ImageJ的单峰的数目的量化 注:用于编写脚本在ImageJ的手册中介绍的所有命令: http://imagej.nih.gov/ij/docs/guide/user-guide.pdf <ol><li>平滑的共聚焦图像从边缘去除孤立像素并填写运行"平滑"功能小孔。 </li><li>鉴于只有芯是荧光，扩张明亮区域，直到属于同一群集的触摸和颗粒合并颗粒的边缘。为此，使用"扩张"过滤器。与约180纳米壳厚度的颗粒，并用0.02微米/像素的分辨率照片拍摄，两人扩张步骤是不够的。 </li><li>将图像转换进入运行"使二元"功能的二进制图像。 </li><li>通过运行工具"，"缩放设置..."，距离= 1称为= 0.02像素= 1单位=嗯""对于例如0.02微米/像素的分辨率拍摄的照片设置比例。 </li><li>应用阈值大小，从在焦粒子区分噪声和失焦颗粒。例如，用0.02微米/像素的分辨率拍摄的照片，所有区域小于0.2像素被排除。为此，使用"分析颗粒..."，"大小= 0.2-∞"命令。 </li><li>创建all.jpg图像，并与所有明亮区域的图像（集群和单峰）通过使用命令"，"结果"，在大小的文件全部.txt，_all.txt""和""JPEG"，"全" "。 </li><li>假设0.2和0.7像素之间，所有的明亮区域的大小和一个圆（圆=π4面积/周长2）0.7和1.0之间运行命令单线"分析颗粒..."，"圆= 0.7-1.0。" </li><li>创建singlets.jpg形象，与那些通过使用命令"，"结果"，_singlets.txt""和""JPEG"，"单峰"，"单线所有明亮区域的信息singlets.txt文件。 </li></ol></li><li> 处理用Matlab信息 <ol><li>阅读单.txt文件，并计算出每一个画面单（ 单线 ）的平均规模。 </li><li>使用一个单峰的平均大小来计算每个群集的粒子数（A 双峰 = 2A 单峰 ，一个三胞胎 = 3A 单峰 ...）和颗粒在与其它全部.txt文件的图像的总数。 </li><li>计算颗粒部分中的每个曝光时间为单峰:F 汗衫 =号码单峰/总颗粒</li><li>计算的双峰，三胞胎等分数:F 双峰 = 2 *双重数/总颗粒等 </li></ol></li></ol>

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B. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Magnetic+assembly+of+colloidal+superstructures+with+multipole+symmetry.">Magnetic assembly of colloidal superstructures with multipole symmetry.</a> Nature. 457 (7232), 999-1002 (2009).</li><li>Vutukuri, H. R., 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=Colloidal+analogues+of+charged+and+uncharged+polymer+chains+with+tunable+stiffness.">Colloidal analogues of charged and uncharged polymer chains with tunable stiffness.</a> Angew. Chem. Int. Edit. 51 (45), 11249-11253 (2012).</li><li>De Greef, T. F. A., Meijer, E. W. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Materials+science:+Supramolecular+polymers.">Materials science: Supramolecular polymers.</a> Nature. 453 (7192), 171-173 (2008).</li><li>De Feijter, I., Albertazzi, L., Palmans, A. R. A., Voets, I. K. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Stimuli-responsive+colloidal+assembly+driven+by+surface-grafted+supramolecular+moieties.">Stimuli-responsive colloidal assembly driven by surface-grafted supramolecular moieties.</a> Langmuir. 31 (1), 57-64 (2015).</li><li>Celiz, A. D., Lee, T. C., Scherman, O. A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Polymer-mediated+dispersion+of+cold+nanoparticles:+using+supramolecular+moieties+on+the+periphery.">Polymer-mediated dispersion of cold nanoparticles: using supramolecular moieties on the periphery.</a> Adv. Mater. 21 (38-39), 3937-3940 (2009).</li><li>Cantekin, S., De Greef, T. F. A., Palmans, A. R. A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Benzene-1,3,5-tricarboxamide:+A+versatile+ordering+moiety+for+supramolecular+chemistry.">Benzene-1,3,5-tricarboxamide: A versatile ordering moiety for supramolecular chemistry.</a> Chem. Soc. Rev. 41 (18), 6125-6137 (2012).</li><li>Mes, T., Van Der Weegen, R., Palmans, A. R. A., Meijer, E. W. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Single-chain+polymeric+nanoparticles+by+stepwise+folding.">Single-chain polymeric nanoparticles by stepwise folding.</a> Angew. Chem. Int. Edit. 50 (22), 5085-5089 (2011).</li><li>van Blaaderen, A., Vrij, A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Synthesis+and+characterization+of+monodisperse+colloidal+organo-silica+spheres.">Synthesis and characterization of monodisperse colloidal organo-silica spheres.</a> J. Colloid Interf. Sci. 156 (1), 1-18 (1993).</li><li>Van Helden, A. K., Jansen, J. 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Sci. 81 (2), 354-368 (1981).</li><li>Israelachvili, J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Intermolecular+and+Surface+Forces.">Intermolecular and Surface Forces.</a> Van der Waals forces between particles and surfaces. , 253-289 (2011).</li><li>van Blaaderen, A., Vrij, A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Synthesis+and+characterization+of+colloidal+dispersions+of+fluorescent,+monodisperse+silica+spheres.">Synthesis and characterization of colloidal dispersions of fluorescent, monodisperse silica spheres.</a> Langmuir. 8 (12), 2921-2931 (1992).</li><li>Giesche, H. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Synthesis+of+monodispersed+silica+powders+II.+Controlled+growth+reaction+and+continuous+production+process.">Synthesis of monodispersed silica powders II. Controlled growth reaction and continuous production process.</a> J. Eur. Ceram. Soc. 14 (3), 205-214 (1994).</li><li>Wu, H. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Correlations+between+the+Rayleigh+ratio+and+the+wavelength+for+toluene+and+benzene.">Correlations between the Rayleigh ratio and the wavelength for toluene and benzene.</a> Chem. Phys. 367 (1), 44-47 (2010).</li></ol>

当环己烷，具有1.426的折射率，被用作溶剂以分散BTA-胶体，范德华相互作用非常弱，由于胶体的折射率和溶剂几乎相同。注意，相比于在水中的裸二氧化硅胶体用于在环己烷中的SLS实验官能胶体的浓度要高得多。这是必要的，以获得足够强的散射，由于低对比度的折射率几乎匹配。立即检测出的环己烷样品中的痕量的水，尽管是间接地通过不可忽略的聚类由于毛细管力。因此，它是最重要的，以?...

介孔胶体材料发现在科学和技术的广泛应用，如用在原子和分子的物质1,2-基础研究的模型系统，因为光子材料3,4，作为药物递送系统5,6，用作涂料7和光刻表面图案形成8,9。由于疏液胶体，最终不可逆地聚集由于无所不在范德华相互作用亚稳材料，其操作成特定的靶结构是非常困难的。许多策略已经被开发，以控制胶体自组装包括使用添加剂以调整静电10,11或耗竭的相互作用12,13，或外部触发，如磁14或电动15字段。一个成熟的替代策略，以实现对结构的控制，这些系统的动力学和力学及其功能的机智^ h分子通过特定和定向力的相互作用。超分子化学提供小分子呈现位点特异性，定向性强但可逆的相互作用，其可以在强度由溶剂的极性，温度和光16进行调制的综合工具箱。因为它们的性能进行了散装和溶液中广泛的研究，这些分子是有吸引力的候选构造软材料进外来阶段以可预测的方式。尽管有这样的综合方法的潜在明确通过超分子化学编排胶体组装，这些学科很少接口裁缝介孔胶体材料17,18的属性。 超分子的胶体一个坚实的平台必须满足三个主要需求。首先，超分子结构部分的耦合应该温和条件下进行，以防止降解。其次，表面力在sepa​​rati组件不是直接接触大应该由栓系基序，这意味着未涂覆胶体应当几乎完全通过排除容积相互作用相互作用支配。因此，该胶体的物理 - 化学特性应适合于抑制在胶体体系，如范德华力或静电引力固有的其他相互作用。第三，表征应该允许大会的明确归属的超分子部分的存在。为了满足这些三个前提，超分子胶体健壮两步合成被开发（ 图1a）。在第一步骤中，疏水NVOC官能化的二氧化硅颗粒是在环己烷中分散的准备。该NVOC组能够容易地切割，从而产生胺官能化的颗粒。胺的反应性高可进行直接的后官能化，使用范围广的温和的反应条件所需的超分子结构部分。在此，我们公关通过用硬脂醇和苯-1,3,5- tricarboxamide（BTA）衍生物20的硅石珠粒官能epare超分子胶体。十八烷醇几个起着重要的作用:它使胶体亲有机并介绍这有助于降低胶体21,22之间的非特异性相互作用短程立体排斥。范德华力，因为胶体的折射率和溶剂23之间的紧密匹配的进一步降低。光及温敏短程吸引力表面力被保护双边贸易20的邻硝基掺入产生的。 邻硝基苄基部分是一个光可切割组块的相邻双边贸易间的氢键时在discotics酰胺掺入形成（ 图1b）。经紫外光光切割的BTA溶液中能够识别并具有相同的BTA分子相互作用通过3倍ħydrogen债券阵，与强烈依赖于温度17粘结强度。由于范德华吸引力是最小为环己烷硬脂涂覆的二氧化硅粒子以及轻型和温度无关，所观察到的刺激响应胶体组件必须BTA-介导的。 这种详细的视频演示了如何合成和表征超分子胶体以及如何通过共聚焦显微镜，研究在紫外线照射他们的自我组装。此外，简单图像分析协议从聚集胶体区分胶体汗衫及确定每簇报道胶体的量。的合成策略的多功能性允许容易地变化的粒径，表面覆盖率以及引入的结合部分，这对于一个大家族介孔高级材料的胶态积木的发展开辟了新的途径。

<table border="0" cellpadding="0" cellspacing="0" width="1805">
	<tbody>
		<tr height="21">
			<td height="21" style="height:21px;width:524px;">APTES</td>
			<td style="width:128px;">Sigma-Aldrich</td>
			<td style="width:119px;"></td>
			<td style="width:1035px;"></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:524px;">FTIC</td>
			<td style="width:128px;">Sigma-Aldrich</td>
			<td style="width:119px;"></td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:524px;">TEOS</td>
			<td style="width:128px;">Sigma-Aldrich</td>
			<td style="width:119px;"></td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:524px;">LUDOX AS-40</td>
			<td style="width:128px;">Sigma-Aldrich</td>
			<td style="width:119px;"></td>
			<td>Silica particles of 13 nm in radius</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:524px;">MilliQ</td>
			<td style="width:128px;">---</td>
			<td style="width:119px;">---</td>
			<td style="width:1035px;">18.2 M&#937;&#183;cm at 25 &#176;C</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:524px;">Ethanol</td>
			<td style="width:128px;">SolvaChrom</td>
			<td style="width:119px;"></td>
			<td style="width:1035px;">---</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:524px;">Ammonia (25% in water)</td>
			<td style="width:128px;">Sigma-Aldrich</td>
			<td style="width:119px;"></td>
			<td style="width:1035px;">---</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:524px;">Chloroform</td>
			<td style="width:128px;">SolvaChrom</td>
			<td style="width:119px;"></td>
			<td style="width:1035px;">---</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:524px;">Cyclohexane</td>
			<td style="width:128px;">Sigma-Aldrich</td>
			<td style="width:119px;"></td>
			<td style="width:1035px;">---</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:524px;">Dimethylformamide (DMF)</td>
			<td style="width:128px;">Sigma-Aldrich</td>
			<td style="width:119px;"></td>
			<td style="width:1035px;">---</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:524px;">Stearyl alcohol</td>
			<td style="width:128px;">Sigma-Aldrich</td>
			<td style="width:119px;"></td>
			<td style="width:1035px;">---</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">N,N-Diisopropylethylamine (DIPEA)</td>
			<td style="width:128px;">Sigma-Aldrich</td>
			<td style="width:119px;"></td>
			<td style="width:1035px;">---</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Benzotriazol-1-yl-oxytripyrrolidinophosphonium hexafluorophosphate (PyBOP)</td>
			<td style="width:128px;">Sigma-Aldrich</td>
			<td style="width:119px;"></td>
			<td style="width:1035px;">---</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Succinimidyl 3-(2-pyridyldithio)propionate (SPDP)</td>
			<td style="width:128px;">Sigma-Aldrich</td>
			<td style="width:119px;"></td>
			<td style="width:1035px;">---</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Dithiothreitol (DTT)&#160;</td>
			<td style="width:128px;">Sigma-Aldrich</td>
			<td style="width:119px;"></td>
			<td style="width:1035px;">---</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:524px;">NVOC-C11-OH</td>
			<td style="width:128px;">Synthesized</td>
			<td style="width:119px;">---</td>
			<td style="width:1035px;">I. de Feijter, 2014 Responsive materials from adaptive supramolecular constructs, Doctoral thesis, Technical University of Eindhoven, The Netherlands</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:524px;">BTA</td>
			<td style="width:128px;">Synthesized</td>
			<td style="width:119px;">---</td>
			<td style="width:1035px;">I. de Feijter, 2014 Responsive materials from adaptive supramolecular constructs, Doctoral thesis, Technical University of Eindhoven, The Netherlands</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:524px;">Centrifuge</td>
			<td style="width:128px;">Thermo Scientific</td>
			<td style="width:119px;"></td>
			<td>Heraeus Megafuge 1.0</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:524px;">Ultrasound bath</td>
			<td style="width:128px;">VWR</td>
			<td style="width:119px;"></td>
			<td>Ultrasonic cleaner</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Peristaltic pumps</td>
			<td>Harvard Apparatus</td>
			<td></td>
			<td>PHD Ultra Syringe Pump</td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;width:524px;">UV-oven</td>
			<td style="width:128px;">Luzchem</td>
			<td style="width:119px;"></td>
			<td>LZC-a V UV reactor equipped with 8x8 UVA light bulbs (&#955;max=354 nm)</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:524px;">Stirrer-heating plate</td>
			<td style="width:128px;">Heidolph</td>
			<td style="width:119px;"></td>
			<td>MR-Hei Standard</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:524px;">Light Scattering</td>
			<td style="width:128px;">ALV</td>
			<td style="width:119px;"></td>
			<td>CGS-3 MD-4 compact goniometer system, equipped with a Multiple Tau digital real time correlator (ALV-7004) and a solid-state laser (&#955;=532 nm, 40 mW)</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">UV-Vis spectrophotometer</td>
			<td style="width:128px;">Thermo Scientific</td>
			<td style="width:119px;"></td>
			<td>NanoDrop 1000 Spectrophotometer</td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;">Confocal microscope</td>
			<td style="width:128px;">Nikon</td>
			<td style="width:119px;"></td>
			<td>Ti Eclipse with an argon laser with &#955;excitation=488 nm</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:524px;">Slide spacers</td>
			<td style="width:128px;">Sigma-Aldrich</td>
			<td style="width:119px;"></td>
			<td>Grace BioLabs Secure seal imaging spacer (1 well, diam. &#215; thickness 13 mm &#215; 0.12 mm)</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:524px;">Syringes</td>
			<td style="width:128px;">BD Plastipak</td>
			<td style="width:119px;"></td>
			<td>20 mL syringe</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:524px;">Plastic tubing</td>
			<td style="width:128px;">SCI</td>
			<td style="width:119px;">BB31695-PE/5</td>
			<td>Ethylene oxide gas sterilizable micro medical tubing</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:524px;">Pulsating vortex mixer</td>
			<td style="width:128px;">VWR</td>
			<td style="width:119px;"></td>
			<td>Electrical: 120V, 50/60Hz, 150W Speed Range: 500&#8211;3000 rpm</td>
		</tr>
	</tbody>
</table>

synthesis and characterization of supramolecular colloids

Control over colloidal assembly is of utmost importance for the development of functional colloidal materials with tailored structural and mechanical properties for applications in photonics, drug delivery and coating technology. Here we present a new family of colloidal building blocks, coined supramolecular colloids, whose self-assembly is controlled through surface-functionalization with a benzene-1,3,5-tricarboxamide (BTA) derived supramolecular moiety. Such BTAs interact via directional, strong, yet reversible hydrogen-bonds with other identical BTAs. Herein, a protocol is presented that describes how to couple these BTAs to colloids and how to quantify the number of coupling sites, which determines the multivalency of the supramolecular colloids. Light scattering measurements show that the refractive index of the colloids is almost matched with that of the solvent, which strongly reduces the van der Waals forces between the colloids. Before photo-activation, the colloids remain well dispersed, as the BTAs are equipped with a photo-labile group that blocks the formation of hydrogen-bonds. Controlled deprotection with UV-light activates the short-range hydrogen-bonds between the BTAs, which triggers the colloidal self-assembly. The evolution from the dispersed state to the clustered state is monitored by confocal microscopy. These results are further quantified by image analysis with simple routines using ImageJ and Matlab. This merger of supramolecular chemistry and colloidal science offers a direct route towards light- and thermo-responsive colloidal assembly encoded in the surface-grafted monolayer.

鉴于用于合成在室温下和在温和的反应条件下的第二步骤中的超分子胶体（ 图1a），耦合BTA-衍生物（ 图1b）的两个步骤，其稳定性得到保证。 <img alt="图1" src="/files/ftp_upload/53934/53934fig1.jpg" /> 图1.超分子胶体的合成的方案。一 ）硬脂醇和NVOC保护烷基链与二氧化硅胶体的耦合，照射时随...

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Synthesis and Characterization of Supramolecular Colloids

A protocol for the synthesis and characterization of colloids coated with supramolecular moieties is described. These supramolecular colloids undergo self-assembly upon the activation of the hydrogen-bonds between the surface-anchored molecules by UV-light.

超分子胶体的合成与表征

Control over colloidal assembly is of utmost importance for the development of functional colloidal materials with tailored structural and mechanical ...

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9.6K 次观看.  Eindhoven University of Technology. A protocol for the synthesis and characterization of colloids coated with supramolecular moieties is described. These supramolecular colloids undergo self-assembly upon the activation of the hydrogen-bonds between the surface-anchored molecules by UV-light.

视频: Synthesis and Characterization of Supramolecular Colloids

Split-and-pool Synthesis and Characterization of Peptide Tertiary Amide Library

Peptidomimetics are great sources of protein ligands. The oligomeric nature of these compounds enables us to access large synthetic libraries on solid phase by using combinatorial chemistry. One of the most well studied classes of peptidomimetics is peptoids. Peptoids are easy to synthesize and have been shown to be proteolysis-resistant and cell-permeable. Over the past decade, many useful protein ligands have been identified through screening of peptoid libraries. However, most of the ligands identified from peptoid libraries do not display high affinity, with rare exceptions. This may be due, in part, to the lack of chiral centers and conformational constraints in peptoid molecules. Recently, we described a new synthetic route to access peptide tertiary amides (PTAs). PTAs are a superfamily of peptidomimetics that include but are not limited to peptides, peptoids and N-methylated peptides. With side chains on both &#945;-carbon and main chain nitrogen atoms, the conformation of these molecules are greatly constrained by sterical hindrance and allylic 1,3 strain. (Figure 1) Our study suggests that these PTA molecules are highly structured in solution and can be used to identify protein ligands. We believe that these molecules can be a future source of high-affinity protein ligands. Here we describe the synthetic method combining the power of both split-and-pool and sub-monomer strategies to synthesize a sample one-bead one-compound (OBOC) library of PTAs.

Peptide tertiary amides (PTAs) are a superfamily of peptidomimetics that include but are not limited to peptides, peptoids and N-methylated peptides. Here we describe a synthetic method which combines&#160;both split-and-pool and sub-monomer strategies to synthesize a one-bead one-compound library of PTAs.

分裂和池合成及肽叔酰胺图书馆表征

Peptidomimetics are great sources of protein ligands. The oligomeric nature of these compounds enables us to access large synthetic libraries on solid ...

科研

化学

Nucleoside Triphosphates - From Synthesis to Biochemical Characterization

The traditional strategy for the introduction of chemical functionalities is the use of solid-phase synthesis by appending suitably modified phosphoramidite precursors to the nascent chain. However, the conditions used during the synthesis and the restriction to rather short sequences hamper the applicability of this methodology. On the other hand, modified nucleoside triphosphates are activated building blocks that have been employed for the mild introduction of numerous functional groups into nucleic acids, a strategy that paves the way for the use of modified nucleic acids in a wide-ranging palette of practical applications such as functional tagging and generation of ribozymes and DNAzymes. One of the major challenges resides in the intricacy of the methodology leading to the isolation and characterization of these nucleoside analogues.
	
	In this video article, we present a detailed protocol for the synthesis of these modified analogues using phosphorous(III)-based reagents. In addition, the procedure for their biochemical characterization is divulged, with a special emphasis on primer extension reactions and TdT tailing polymerization. This detailed protocol will be of use for the crafting of modified dNTPs and their further use in chemical biology.

The protocol described herein aims to explain and abridge the numerous obstacles in the way of the intricate route leading to modified nucleoside triphosphates. Consequently, this protocol facilitates both the synthesis of these activated building-blocks and their availability for practical applications.

核苷三磷酸 - 从合成到生化特征

The  traditional strategy for the introduction of chemical functionalities is the  use of solid-phase synthesis by appending suitably modified ...

Synthesis and Characterization of Functionalized Metal-organic Frameworks

Metal-organic frameworks have attracted extraordinary amounts of research attention, as they are attractive candidates for numerous industrial and technological applications. Their signature property is their ultrahigh porosity, which however imparts a series of challenges when it comes to both constructing them and working with them. Securing desired MOF chemical and physical functionality by linker/node assembly into a highly porous framework of choice can pose difficulties, as less porous and more thermodynamically stable congeners (e.g., other crystalline polymorphs, catenated analogues) are often preferentially obtained by conventional synthesis methods. Once the desired product is obtained, its characterization often requires specialized techniques that address complications potentially arising from, for example, guest-molecule loss or preferential orientation of microcrystallites. Finally, accessing the large voids inside the MOFs for use in applications that involve gases can be problematic, as frameworks may be subject to collapse during removal of solvent molecules (remnants of solvothermal synthesis). In this paper, we describe synthesis and characterization methods routinely utilized in our lab either to solve or circumvent these issues. The methods include solvent-assisted linker exchange, powder X-ray diffraction in capillaries, and materials activation (cavity evacuation) by supercritical CO2 drying. Finally, we provide a protocol for determining a suitable pressure region for applying the Brunauer-Emmett-Teller analysis to nitrogen isotherms, so as to estimate surface area of MOFs with good accuracy.

Synthesis, activation, and characterization of intentionally designed metal-organic framework materials is challenging, especially when building blocks are incompatible or unwanted polymorphs are thermodynamically favored over desired forms. We describe how applications of solvent-assisted linker exchange, powder X-ray diffraction in capillaries and activation via supercritical CO2 drying, can address some of these challenges.

功能化的合成与表征金属 - 有机骨架

Metal-organic frameworks have attracted extraordinary amounts of research attention, as they are attractive candidates for numerous industrial and ...

The Synthesis, Characterization and Reactivity of a Series of Ruthenium N-triphosPh Complexes

Herein we report the synthesis of a tridentate phosphine ligand N(CH2PPh2)3 (N-triphosPh) (1) via a phosphorus based Mannich reaction of the hydroxylmethylene phosphine precursor with ammonia in methanol under a nitrogen atmosphere. The N-triphosPh ligand precipitates from the solution after approximately 1 hr of reflux and can be isolated analytically pure via simple cannula filtration procedure under nitrogen. Reaction of the N-triphosPh ligand with [Ru3(CO)12] under reflux affords a deep red solution that show evolution of CO gas on ligand complexation. Orange crystals of the complex [Ru(CO)2{N(CH2PPh2)3}-&#954;3P] (2) were isolated on cooling to RT. The 31P{1H} NMR spectrum showed a characteristic single peak at lower frequency compared to the free ligand. Reaction of a toluene solution of complex 2 with oxygen resulted in the instantaneous precipitation of the carbonate complex [Ru(CO3)(CO){N(CH2PPh2)3}-&#954;3P] (3) as an air stable orange solid. Subsequent hydrogenation of 3 under 15 bar of hydrogen in a high-pressure reactor gave the dihydride complex [RuH2(CO){N(CH2PPh2)3}-&#954;3P] (4), which was fully characterized by X-ray crystallography and NMR spectroscopy. Complexes 3 and 4 are potentially useful catalyst precursors for a range of hydrogenation reactions, including biomass-derived products such as levulinic acid (LA). Complex 4 was found to cleanly react with LA in the presence of the proton source additive NH4PF6 to give [Ru(CO){N(CH2PPh2)3}-&#954;3P{CH3CO(CH2)2CO2H}-&#954;2O](PF6) (6).

The Synthesis, Characterization and Reactivity of a Series of Ruthenium N-triphosPh Complexes

Ruthenium phosphine complexes are widely used for homogeneous catalytic reactions such as hydrogenations. The synthesis of a series of novel tridentate ruthenium complexes bearing the N-triphos ligand N(CH2PPh2)3 is reported. Additionally, the stoichiometric reaction of a dihydride Ru&#8211;N-triphos complex with levulinic acid is described.

一系列钌的合成，表征和反应<em&gt;Ñ</em&gt; -triphos<sup&gt;博士</sup&gt;配合

Herein we report the synthesis of a tridentate phosphine ligand N(CH2PPh2)3 (N-triphosPh) (1) via a phosphorus based Mannich reaction of the ...

Synthesis, Characterization, and Functionalization of Hybrid Au/CdS and Au/ZnS Core/Shell Nanoparticles

Plasmonic nanoparticles are an attractive material for light harvesting applications due to their easily modified surface, high surface area and large extinction coefficients which can be tuned across the visible spectrum. Research into the plasmonic enhancement of optical transitions has become popular, due to the possibility of altering and in some cases improving photo-absorption or emission properties of nearby chromophores such as molecular dyes or quantum dots. The electric field of the plasmon can couple with the excitation dipole of a chromophore, perturbing the electronic states involved in the transition and leading to increased absorption and emission rates. These enhancements can also be negated at close distances by energy transfer mechanism, making the spatial arrangement of the two species critical. Ultimately, enhancement of light harvesting efficiency in plasmonic solar cells could lead to thinner and, therefore, lower cost devices. The development of hybrid core/shell particles could offer a solution to this issue. The addition of a dielectric spacer between a gold nanoparticles and a chromophore is the proposed method to control the exciton plasmon coupling strength and thereby balance losses with the plasmonic gains. A detailed procedure for the coating of gold nanoparticles with CdS and ZnS semiconductor shells is presented. The nanoparticles show high uniformity with size control in both the core gold particles and shell species allowing for a more accurate investigation into the plasmonic enhancement of external chromophores.

The synthesis of uniform gold nanoparticles coated with semiconductor shells of CdS or ZnS is performed. The semiconductor coating is conducted by first depositing a silver sulfide shell and exchanging the silver cations for zinc or cadmium cations.

合成，表征和混合金/硫化镉和Au / ZnS核/壳纳米颗粒功能化

Plasmonic nanoparticles are an attractive material for light harvesting applications due to their easily modified surface, high surface area and large ...

Preparation of Carbon Nanosheets at Room Temperature

Amphiphilic molecules equipped with a reactive, carbon-rich "oligoyne" segment consisting of conjugated carbon-carbon triple bonds self-assemble into defined aggregates in aqueous media and at the air-water interface. In the aggregated state, the oligoynes can then be carbonized under mild conditions while preserving the morphology and the embedded chemical functionalization. This novel approach provides direct access to functionalized carbon nanomaterials. In this article, we present a synthetic approach that allows us to prepare hexayne carboxylate amphiphiles as carbon-rich siblings of typical fatty acid esters through a series of repeated bromination and Negishi-type cross-coupling reactions. The obtained compounds are designed to self-assemble into monolayers at the air-water interface, and we show how this can be achieved in a Langmuir trough. Thus, compression of the molecules at the air-water interface triggers the film formation and leads to a densely packed layer of the molecules. The complete carbonization of the films at the air-water interface is then accomplished by cross-linking of the hexayne layer at room temperature, using UV irradiation as a mild external stimulus. The changes in the layer during this process can be monitored with the help of infrared reflection-absorption spectroscopy and Brewster angle microscopy. Moreover, a transfer of the carbonized films onto solid substrates by the Langmuir-Blodgett technique has enabled us to prove that they were carbon nanosheets with lateral dimensions on the order of centimeters.

We present the synthesis of an amphiphilic hexayne and its use in the preparation of carbon nanosheets at the air-water interface from a self-assembled monolayer of these reactive, carbon-rich molecular precursors.

碳纳米片在室温下准备

Amphiphilic molecules equipped with a reactive, carbon-rich "oligoyne" segment consisting of conjugated carbon-carbon triple bonds self-assemble into ...

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 ...

Synthesis and Characterization of Fe-doped Aluminosilicate Nanotubes with Enhanced Electron Conductive Properties

The goal of the protocol is to synthesize Fe-doped aluminosilicate nanotubes of the imogolite type with the formula (OH)3Al2-xFexO3SiOH. Doping with Fe aims at lowering the band gap of imogolite, an insulator with the chemical formula (OH)3Al2O3SiOH, and at modifying its adsorption properties towards azo-dyes, an important class of organic pollutants of both wastewater and groundwater.
Fe-doped nanotubes are obtained in two ways: by direct synthesis, where FeCl3 is added to an aqueous mixture of the Si and Al precursors, and by post-synthesis loading, where preformed nanotubes are put in contact with a FeCl3&#8226;6H2O aqueous solution. In both synthesis methods, isomorphic substitution of Al3+ by Fe3+ occurs, preserving the nanotube structure. Isomorphic substitution is indeed limited to a mass fraction of ~1.0% Fe, since at a higher Fe content (i.e., a mass fraction of 1.4% Fe), Fe2O3 clusters form, especially when the loading procedure is adopted. The physicochemical properties of the materials are studied by means of X-ray powder diffraction (XRD), N2 sorption isotherms at -196 &#176;C, high resolution transmission electron microscopy (HRTEM), diffuse reflectance (DR) UV-Vis spectroscopy, and &#950;-potential measurements. The most relevant result is the possibility to replace Al3+ ions (located on the outer surface of the nanotubes) by post-synthesis loading on preformed imogolite without perturbing the delicate hydrolysis equilibria occurring during nanotube formation. During the loading procedure, an anionic exchange occurs, where Al3+ ions on the outer surface of the nanotubes are replaced by Fe3+ ions. In Fe-doped aluminosilicate nanotubes, isomorphic substitution of Al3+ by Fe3+ is found to affect the band gap of doped imogolite. Nonetheless, Fe3+ sites on the outer surface of nanotubes are able to coordinate organic moieties, like the azo-dye Acid Orange 7, through a ligand-displacement mechanism occurring in an aqueous solution.

Here, we present a protocol to synthesize and characterize Fe-doped aluminosilicate nanotubes. The materials are obtained by either sol-gel synthesis upon addition of FeCl3&#8226;6H2O to the mixture containing the Si and Al precursors or by post-synthesis ionic exchange of preformed aluminosilicate nanotubes.

以增强电子导电性能的合成与表征Fe掺杂碳纳米管硅铝的

The goal of the protocol is to synthesize Fe-doped aluminosilicate nanotubes of the imogolite type with the formula (OH)3Al2-xFexO3SiOH. Doping with Fe ...

Phase Behavior of Charged Vesicles Under Symmetric and Asymmetric Solution Conditions Monitored with Fluorescence Microscopy

Phase-separated giant unilamellar vesicles (GUVs) exhibiting coexisting liquid-ordered and liquid-disordered domains are a common biophysical tool to investigate the lipid raft hypothesis. Numerous studies, however, neglect the impact of physiological solution conditions. On that account, the current work presents the effect of high-salinity buffer and trans-membrane solution asymmetry on liquid-liquid phase separation in charged GUVs grown from dioleylphosphatidylglycerol, egg sphingomyelin, and cholesterol. The effects were studied under isothermal and varying temperature conditions.
We describe equipment and experimental strategies applicable for monitoring the stability of coexisting liquid domains in charged vesicles under symmetric and asymmetric high-salinity solution conditions. This includes an approach to prepare charged multicomponent GUVs in high-salinity buffer at high temperatures. The protocol entails the option to perform a partial exchange of the external solution by a simple dilution step while minimizing the vesicle dilution. An alternative approach is presented utilizing a microfluidic device that allows for a complete external solution exchange. The solution effects on phase separation were also studied under varying temperatures. To this end, we present the basic design and utility of an in-house built temperature control chamber. Furthermore, we reflect on the assessment of the GUV phase state, pitfalls associated with it and how to circumvent them.

Experiments on phase separated giant unilamellar vesicles (GUVs) frequently neglect physiological solution conditions. This work presents approaches to study the effect of high-salinity buffer on liquid-liquid phase separation in charged multicomponent GUVs as a function of trans-membrane solution asymmetry and temperature.

用荧光显微镜监测对称和非对称溶液条件下带电泡的相行为

Phase-separated giant unilamellar vesicles (GUVs) exhibiting coexisting liquid-ordered and liquid-disordered domains are a common biophysical tool to ...

Protocol for the Solid-phase Synthesis of Oligomers of RNA Containing a 2'-O-thiophenylmethyl Modification and Characterization via Circular Dichroism

Solid-phase synthesis has been used to obtain canonical and modified polymers of nucleic acids, specifically of DNA or RNA, which has made it a popular methodology for applications in various fields and for different research purposes. The procedure described herein focuses on the synthesis, purification, and characterization of dodecamers of RNA 5&#39;-[CUA CGG AAU CAU]-3&#39; containing zero, one, or two modifications located at the C2&#39;-O-position. The probes are based on 2-thiophenylmethyl groups, incorporated into RNA nucleotides via standard organic synthesis and introduced into the corresponding oligonucleotides via their respective phosphoramidites. This report makes use of phosphoramidite chemistry via the four canonical nucleobases (Uridine (U), Cytosine (C), Guanosine (G), Adenosine (A)), as well as 2-thiophenylmethyl functionalized nucleotides modified at the 2&#39;-O-position; however, the methodology is amenable for a large variety of modifications that have been developed over the years. The oligonucleotides were synthesized on a controlled-pore glass (CPG) support followed by cleavage from the resin and deprotection under standard conditions, i.e., a mixture of ammonia and methylamine (AMA) followed by hydrogen fluoride/triethylamine/N-methylpyrrolidinone. The corresponding oligonucleotides were purified via polyacrylamide electrophoresis (20% denaturing) followed by elution, desalting, and isolation via reversed-phase chromatography (Sep-pak, C18-column). Quantification and structural parameters were assessed via ultraviolet-visible (UV-vis) and circular dichroism (CD) photometric analysis, respectively. This report aims to serve as a resource and guide for beginner and expert researchers interested in embarking in this field. It is expected to serve as a work-in-progress as new technologies and methodologies are developed. The description of the methodologies and techniques within this document correspond to a DNA/RNA synthesizer (refurbished and purchased in 2013) that uses phosphoramidite chemistry.

Protocol for the Solid-phase Synthesis of Oligomers of RNA Containing a 2'-O-thiophenylmethyl Modification and Characterization via Circular Dichroism

This article provides a detailed procedure on the solid-phase synthesis, purification, and characterization of dodecamers of RNA modified at the C2&#39;-O-position. UV-vis and circular dichroism photometric analyses are used to quantify and characterize structural aspects, i.e., single-strands or double-strands.

用于固相合成含有2&#39;-<em&gt; 0</em通过圆二色性修饰和表征

Solid-phase synthesis has been used to obtain canonical and modified polymers of nucleic acids, specifically of DNA or RNA, which has made it a popular ...