Name: controlled synthesis and fluorescence tracking of highly uniform poly(n-isopropylacrylamide) microgels
Uploaded: 2016-09-08T14:00:00
Description: Watch this Scientific Journal Video about Controlled Synthesis and Fluorescence Tracking of Highly Uniform PolyN-isopropylacrylamide Microgels at JoVE.com

The Deutsche Forschungsgemeinschaft (DFG) is acknowledged for financial support within the Sonderforschungsbereich SFB 985 "Functional Microgels and Microgel Systems".

1.マイクロゲルの合成注：N -isopropylacrylamide（NIPAM）をn-ヘキサンから再結晶しました。受信した他の試薬を使用しました。 <ol><li>ポリ（NIPAM）マトリックスミクロゲルの従来のバッチ合成<ol><li>濾過245 ml中に1.8グラムのNIPAMと24ミリグラムのN、N &#39;-bisacrylamide（BIS）を溶解（0.2μmの再生セルロース（RC）メンブレンフィルター）還流冷却器を備えた500mlの三首?...

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官能性コモノマーの少量の添加は、PNIPAMミクロゲル由来の粒子サイズおよび構造に大きな影響を持つことができます。同時小規模試験管重合は、このような変化を考慮するための良い方法であり、急速に必要に応じて反応をアップスケーリングするための目標粒径のための右の反応組成物を見つけるのに役立ちます。粒子の質量?...

刺激応答性ポリ（N -isopropylacrylamide）（PNIPAM）マイクロゲル1,2は、さまざまなスマートアプリケーションでの電位に起因する過去20年間連続の関心を集めています。実証されたユースケースは、低分子量化合物と他の生物医学的用途の12のために切り替え可能なエマルジ ​​ョン安定剤3-8、マイクロレンズ9、細胞培養簡単細胞収穫10,11のための基質、およびスマート担体を含みます。ビューの基礎研究の観点から、これらの粒子は、コロイドの相互作用13-15およびポリマー-溶媒相互作用16-18として被験体を調査するために有用であることが証明されています。 任意のアプリケーションでPNIPAMミクロゲルおよびそれらの誘導体の使用の成功は、典型的には、粒度分布の平均粒径と幅に関する知識を必要とします。 PNIPAMマイクロを含む実験結果の正しい解釈のためのゲルは、官能性コモノマーの影響を受けることができる粒子構造は、知らなければなりません。動的および静的光散乱（DLSそれぞれSLSは、）は、これらの方法は、高速で使用するのが比較的容易であるため、この情報を取得するための一意に適しています。そして彼らは彼らのネイティブ環境（分散）で非侵襲的に粒子特性を調べます。 DLSおよびSLSはまた、顕微鏡法のための典型的な小さなサンプルサイズから生じるバイアスを回避する粒子の膨大な数のデータを収集します。したがって、この研究の最初の目的は、コロイド特性評価への新たな実務家のための光散乱に関するグッドプラクティスを導入することです。 一般的に、沈殿重合は、実験室規模で行われ、特定の粒子特性のための右の反応条件を見出すことは面倒であると合成の多くの繰り返しを必要とすることができます。大きなバッチ合成とは対照的に、非撹拌沈殿重合19,20は、ARであります異なる反応体組成物のバッチは、狭いサイズ分布の粒子を得、同時に重合することができるAPID手順。同時重合実験変動を最小限にし、大きな出力が正しい反応条件は、反応をア​​ップスケーリングするための高速見つけることができることを意味します。したがって、私たちの第二の目的は、プロトタイピングで、製品を大量に必要としないアプリケーションで非撹拌沈殿重合の有用性を実証することです。 合成と特性評価のさまざまな側面は​​、コロイドの相互作用の研究における蛍光標識されたPNIPAMマイクロゲルの応用例で一緒に来ます。ここでは、広いマトリックス濃度範囲にわたって非標識行列ミクロゲルの分散液中の標識トレーサーのミクロゲルの拡散を調査し、濃縮コロイド分散液中のケージの効果を解決するために、高精度の単一粒子追跡を使用します。広視野蛍光顕微鏡法は、FO適していますrをそれとして、この目的は、潜在的に異なるマトリックス種の多数の中から、いくつかのトレーサー分子の特定の動作を特徴づけることができます。これは、システムのアンサンブル平均特性を測定するため、大規模なシステムでは、プローブ粒子の数が少ないの問題を解決することができないようなDLS、SLSおよびレオロジーなどの技術とは対照的です。また、この具体例では、従来の光散乱法は、任意の標準的な分析を無効に強い多重散乱をもたらす高粒子濃度に起因利用することができません。自動データ処理及び統計的方法の使用は、大きなサンプルサイズにわたって平均単一粒子追跡のために、全体的なシステム挙動の分析を可能にします。

<table border="0" cellpadding="0" cellspacing="0" width="741">
	<tbody>
		<tr height="20">
			<td height="20" style="height:20px;width:259px;">Acetone</td>
			<td style="width:199px;">VWR Chemicals</td>
			<td style="width:155px;">KRAF13455</td>
			<td style="width:129px;"></td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;width:259px;">Bisacrylamid</td>
			<td style="width:199px;">AppliChem</td>
			<td style="width:155px;">A3636</td>
			<td style="width:129px;"></td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;width:259px;">n-Hexane</td>
			<td style="width:199px;">Merck</td>
			<td style="width:155px;">104374</td>
			<td style="width:129px;"></td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;width:259px;">N-Isopropylacrylamide</td>
			<td style="width:199px;">Fisher Scientific</td>
			<td style="width:155px;">AC412785000</td>
			<td>recrystallized from n-hexane</td>
		</tr>
		<tr height="40">
			<td height="40" style="height:40px;width:259px;">Methacryloxyethyl thiocarbamoyl rhodamine B</td>
			<td style="width:199px;">Polysciences</td>
			<td style="width:155px;">23591</td>
			<td style="width:129px;"></td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;width:259px;">Potassium peroxodisulfate</td>
			<td style="width:199px;">Merck</td>
			<td style="width:155px;">105091</td>
			<td style="width:129px;"></td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;width:259px;">Silicone oil 47 V 350</td>
			<td style="width:199px;">VWR Chemicals</td>
			<td style="width:155px;">83851</td>
			<td style="width:129px;"></td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;width:259px;">Toluene</td>
			<td style="width:199px;">Sigma Aldrich</td>
			<td style="width:155px;">244511</td>
			<td style="width:129px;"></td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;">F12 Refrigerated/heating circulator</td>
			<td style="width:199px;">Julabo</td>
			<td>9116612</td>
			<td style="width:129px;"></td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;">Microscope</td>
			<td>Olympus</td>
			<td>IX83</td>
			<td></td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;">XY(Z) Piezo System</td>
			<td>Physik Instrumente</td>
			<td>P-545.3R7</td>
			<td></td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;">100x Oil immersion objective</td>
			<td>Olympus</td>
			<td>UPLSAPO</td>
			<td></td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;">QuadLine Beamsplitter</td>
			<td>AHF Analysentechnik</td>
			<td>F68-556T</td>
			<td></td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;">&#160;Cobolt Jive 150 laser</td>
			<td>Cobolt</td>
			<td>0561-04-01-0150-300</td>
			<td></td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;">Multimode Fiber</td>
			<td>Thorlabs</td>
			<td>UM22-600</td>
			<td></td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;">iXON Ultra 897 EMCCD camera</td>
			<td>Andor</td>
			<td>DU-897U-CS0-BV</td>
			<td></td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;">Laser goniometer</td>
			<td>SLS Systemtechnik</td>
			<td>Mark III</td>
			<td></td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;">CF40 Cryo-compact circulator</td>
			<td>Julabo</td>
			<td>9400340</td>
			<td></td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;">Laser goniometer system&#160;</td>
			<td>ALV GmbH</td>
			<td>ALV / CGS-8F</td>
			<td></td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;">Multi-tau corretator</td>
			<td>ALV GmbH</td>
			<td>ALV-7004</td>
			<td></td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;">Light scattering electronics</td>
			<td>ALV GmbH</td>
			<td>ALV / LSE 5004</td>
			<td></td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;">Photon counting module</td>
			<td>PerkinElmer</td>
			<td>SPCM-CD2969</td>
			<td>2 units in pseudo cross-correlation mode</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">633 nm HeNe Laser</td>
			<td>JDS Uniphase</td>
			<td>1145P</td>
			<td></td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;">F32 Refrigerated/heating circulator</td>
			<td>Julabo</td>
			<td>9312632</td>
			<td></td>
		</tr>
	</tbody>
</table>

controlled synthesis and fluorescence tracking of highly uniform poly(n-isopropylacrylamide) microgels

刺激応答性ポリ（N -isopropylacrylamide）（PNIPAM）マイクロゲルは、様々な将来の実用的なアプリケーションを持っており、基礎研究に使用しています。本研究では、迅速な非撹拌沈殿重合法によってチューニングミクロゲルサイズのためのショーケースとしての蛍光標識したPNIPAMマイクロゲルを追跡する単一粒子を使用しています。このアプローチは、新しい反応組成物および条件を試作するため、または製品を大量に必要としないアプリケーションに適しています。動的および静的光散乱によってミクロゲル合成、粒子サイズ及び構造決意は、プロトコルに詳述されています。官能性コモノマーの添加は、粒子の核生成及び構造に大きな影響を持つことができることが示されています。広視野蛍光顕微鏡による単一粒子追跡を容易にすることによって調査されないシステム、非標識ミクロゲルの濃縮マトリックス中の標識トレーサーマイクロゲルの拡散の調査を可能にしますこのような動的光散乱などの他の方法。

バッチ内PNIPAMミクロゲル粒子の数、および、最終的な粒子の体積は、チオカルバモイルローダミンBは、バッチ内の粒子数密度を減少させることによって、核形成に影響を与える核形成段階20疎水性コモノマー色素メタクリロキシエチル中に早期反応で決定されます。二つの異なる初期NIPAM濃度について粒子濃度の?...

Watch this Scientific Journal Video about Controlled Synthesis and Fluorescence Tracking of Highly Uniform PolyN-isopropylacrylamide Microgels at JoVE.com

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

非撹拌沈殿重合は、狭いサイズ分布の刺激応答性ポリ（N -isopropylacrylamide）ミクロゲルの合成への迅速な、再現性のプロトタイピング手法を提供します。このプロトコル合成では、光散乱特性評価および広視野顕微鏡のセットアップでこれらのミクロゲルの単一粒子蛍光追跡が実証されています。

制御された合成および均一性の高いポリの蛍光トラッキング（<em&gt; N</em&gt; -isopropylacrylamide）ミクロゲル

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

The overall goal of this work is to investigate the dynamic behavior and interaction of soft colloidal particles in dispersions of various particle densities in the vicinity of glass transition. Microgels are soft objects that can adapt their size, shape, and mobility according to their environments. In contrast to rigid colloidal particles, there are many open questions concerning the behavior of soft microgels.The main advantage of wide field fluorescence microscopy is the possibility to localize single microgels with high accuracy, directly follow their motion in C2, and to analyze the amounts of diffusion. To investigate the dynamics of single microgels in dense systems, only a small number of microgels must be fluorescently labeled. Non-stirred precipitation polymerization allows for parallel synthesis of microgel with variable reaction conditions to conveniently match the size of labeled and unlabeled microgels.Dynamic light-scattering provides the average hydrodynamic radii of the microgels within an accuracy of a few nanometers. Dissolve 1.8 grams of NIPAM and 24 milligrams of BIS in 245 milliliters of filtered double-distilled water in a 500 milliliter, three-neck round bottom flask equipped with reflux condenser, a stirrer, and a rubber septum. Insert a thermometer and a 120-millimeter needle for the nitrogen input through the septum.Heat the solution to 60 degrees Celsius while stirring. Then, deoxygenate the solution by purging with nitrogen for 40 minutes. Simultaneously prepare an initiator solution of 155 milligrams of potassium persulfate, or KPS, in five milliliters of filtered double-distilled water, and bubble the solution with nitrogen to remove oxygen.Next, wash a syringe with nitrogen, and transfer the complete five milliliter KPS solution to a nitrogen-washed syringe equipped with a 120-millimeter needle. Lift the nitrogen needle above the solution level in the three-neck flask, and add the KPS solution rapidly through the rubber septum into the reactor. Let the polymerization proceed for one hour under nitrogen flow and slow stirring at 60 degrees Celsius.Use a Buchner funnel and filter paper to filter the hot reaction solution, and discard any big aggregates. After letting the dispersion cool down, centrifuge and redisperse the dispersion three times for 40 minutes at 257, 000 times G.Finally, redisperse the sediment in a minimum viable amount of double-distilled water before lyophilizing the dispersion for storing. Weigh 257.7 milligrams of NIPAM, 3.5 milligrams of BIS, and 1.5 milligrams of methacryloxyethyl thiocarbamoyl rhodamine B dye in a glass vessel, and add 10 milliliters of filter double-distilled water.Prepare the same solution without the dye in a separate glass vessel. Ultrasonicate the dye solution for 15 minutes to dissolve the dye in water. Prepare various dilutions of the monomer solution with the dye to obtain a concentration series.Here, dye in the concentration range of 02 to 0.1 millimole per liter is used. Next, dissolve 8.4 milligrams of KPS in 10 milliliters of filtered double-distilled water to get the initiator solution. Transfer 0.5 milliliters of the concentration series and 05 milliliters of the KPS solution to test tubes with a 10 millimeter diameter to obtain the final reaction solutions.Seal the tubes with rubber septa. Preheat an oil bath in a double-walled glass vessel connected to a heating circulator to 63 degrees Celsius. Deoxygenize the reaction solutions by purging with nitrogen through 120-millimeter needles for 20 minutes.Then, insert the tubes into a floating platform, and immerse the platform in the pre-heated oil bath. Set the temperature to 60 degrees Celsius. For high-precision particle size tuning, the temperature control during the initial reaction has to be rigorous, typically plus or minus 0.1 degrees Celsius.Let the reaction proceed for an appropriate amount of time. Typically, one hour is enough. Following the reaction, transfer the reaction tubes rapidly to an oven at 60 degrees Celsius.Put one drop of the hot dispersion in 10 milliliters of filtered double-distilled water, pre-heated over the poly-NIPAM volume phase transition temperature in order to measure the hydrodynamic radii of the particles in the collapsed state. Let the rest of the dispersions cool down to room temperature, and transfer them into centrifuge tubes. After centrifuging the solution, dilute the microgels in two milliliters of filtered double-distilled water to use as tracer particles.For hydrodynamic radius determination in the collapsed state by dynamic light scattering, first wash the cuvettes and glassware with acetone vapor. Transfer approximately one milliliter of diluted particle dispersion to a measurement cuvette. Temper the dynamic light-scattering goniometer index match bath to 50 degrees Celsius, and transfer the sample to the instrument without letting it cool down.Insert the sample cuvette, and move the detector arm to the small scattering angle. After checking the beam profile and count range as described in the text protocol, move the goniometer arm to the highest scattering angle. Check that the count rate is still high enough for the measurement.If the intensity is too low, move the arm to a lower scattering angle. Then, check the beam visually through the toluene bath glass at the lowest scattering angle. If glow around the incident beam is observed, multiple scattering takes place.Acquire 20 correlograms between the minimum and maximum scattering angle with a minimum acquisition time of 60 seconds. Increase the acquisition time for weak intensity large-scattering angles if necessary. Use an appropriate objective lens of the desired magnification and aperture for excitation of the tracers and simultaneous fluorescence collection from the sample.In this work, a 100X, 1.3 numerical aperture oil-immersion objective lens is used. Place the moisture chamber onto an XYZ pi-SO table that fits into a microscope. To prevent the sample from drying, place a plasma-cleaned cover slip into the moisture chamber, and pipette 10 microliters of the desired concentration of poly-NIPAM dispersion.Depending on the excitation and emission spectra of the fluorescent dye, use a suitable laser for excitation, and adjust the laser power appropriately. A 561-nanometer diode-pump solid state laser is used here at a constant laser power of 16 milliwatts. To obtain homogeneous sample illumination, couple the laser into a multimode fiber, shake the fiber using a vortexer to temporarily average out laser speckles, and project the fiber end into the sample plane.Calibrate the Z-distance from the back reflection of the cover slip, and focus several micrometers into the sample by moving the objective slightly up, and fix the Z-position using a Z-compensator. This avoids any interface effects with the cover slip. Adjust the detector parameters, such as exposure time, to the strength of the fluorescent signal.In this case, an EMCCD camera is used with an exposure time of 0.1 seconds in electron-multiplying mode and a gain of 50. Acquire several movies with the appropriate number of frames to obtain adequate lag time to calculate the mean-squared displacement of the microgels in different regions of the sample. Eight labeled microgel batches were synthesized.For six batches, correlogram decay rates linear rise against the square of the scattering vector magnitude, which indicates narrow size distribution. A fit through the origin indicates only translational diffusion. For two batches, nonlinear behavior is observed.The deviation is caused by broad size distribution and a particle form factor minimum, which coincides with the scattering vector range. To obtain a better estimate for the mean diffusion coefficient of the particles, exclude these points from the fit. High signal to noise ratio enables tracking of fluorescent microgels.Their diffusion is restricted by the the unlabeled microgel matrix. Higher concentrations of unlabeled microgel matrix on the right leads to a pronounced cage effect, where the fluorescent microgels are trapped in an unlabeled matrix of microgels. At low concentrations of unlabeled mircogel matrix, the tracer microgels exhibit normal diffusion, which is inferred from the linear increase of mean-square displacement with lag time.However, at high concentrations close to the colloidal glass transition, they exhibit nonlinear diffusion, depicted by nonlinear temporal evolution of mean-square displacements. At higher concentration of unlabeled microgel matrix, the tracer microgels are trapped by unlabeled neighbors into transient cages, as illustrated by clustered tracks for 12 microgels. Parallel small-scale synthesis enables fast experimentation with different reaction parameters.This also minimizes any undesired experimental variation due to reaction temperature differences. In combination with the careful dynamic light-scattering characterization, the reaction conditions for the right microgel size can be found fast. In this video, we demonstrate how controlled microgel synthesis allows us to investigate the diffusion of single microgels in concentrated microgel solutions by wide field fluorescence microscopy.Following this procedure, it will be possible to understand how the structure of microgels controls their properties. This will open the door to designing new soft interactive matter.

Research

JoVE Journal

Chemistry

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

Synthesis of Poly(N-isopropylacrylamide) Janus Microhydrogels for Anisotropic Thermo-responsiveness and Organophilic/Hydrophilic Loading Capability

Synthesis of PolyN-isopropylacrylamide Janus Microhydrogels for Anisotropic Thermo-responsiveness and Organophilic/Hydrophilic Loading Capability

ポリの合成（<em&gt; N</em&gt; -isopropylacrylamide）異方性熱応答性および有機性/親水性ローディング機能のためのヤヌスMicrohydrogels

Janus microparticles are compartmentalized particles with differing molecular structures and/or functionality on each of their two sides. Because of this ...

化学

Highly Stereoselective Synthesis of 1,6-Ketoesters Mediated by Ionic Liquids: A Three-component Reaction Enabling Rapid Access to a New Class of Low Molecular Weight Gelators

イオン液体によって媒介1,6-ケトエステルの高立体選択的合成：低分子ゲル化剤の新しいクラスへの迅速なアクセスを有効にする三成分の反応

In organic chemistry ionic liquids (ILs) have emerged as safe and recyclable reaction solvents. In the presence of a base ILs can be deprotonated to form ...

A Simple Method for the Size Controlled Synthesis of Stable Oligomeric Clusters of Gold Nanoparticles under Ambient Conditions

周囲条件下での金ナノ粒子の安定オリゴマークラスターのサイズ制御された合成のための簡単​​な方法

Reducing dilute aqueous HAuCl4 with sodium thiocyanate (NaSCN) under alkaline conditions produces 2 to 3 nm diameter nanoparticles. Stable grape-like ...

Synthesis and Characterization of Supramolecular Colloids

超分子コロイドの合成とキャラクタリゼーション

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

Hydroquinone Based Synthesis of Gold Nanorods

金ナノロッドのヒドロキノンベースの合成

Gold nanorods are an important kind of nanoparticles characterized by peculiar plasmonic properties. Despite their widespread use in nanotechnology, the ...

Scale-up Chemical Synthesis of Thermally-activated Delayed Fluorescence Emitters Based on the Dibenzothiophene-S,S-Dioxide Core

スケール アップ ジベンゾチオフェン S、S 二酸化コアに基づく熱重合遅延蛍光体の化学合成

We report a procedure to linearly scale-up the synthesis of 2,8-bis(3,6-di-tert-butyl-9H-carbazol-9-yl)dibenzothiophene-S,S-dioxide (compound 4) and ...

Synthesis and Mass Spectrometry Analysis of Oligo-peptoids

合成とオリゴ ペプチドの質量分析

Peptoids are sequence-controlled peptide-mimicking oligomers consisting of N-alkylated glycine units. Among many potential applications, peptoids have ...

Synthesis of Substrate-Bound Au Nanowires Via an Active Surface Growth Mechanism

アクティブな表面の成長メカニズムを介して基質結合 Au ナノワイヤの作製

Advancing synthetic capabilities is important for the development of nanoscience and nanotechnology. The synthesis of nanowires has always been a ...

Synthesis and Characterization of Amphiphilic Gold Nanoparticles

親和性金ナノ粒子の合成と特性化

Gold nanoparticles covered with a mixture of 1-octanethiol (OT) and 11-mercapto-1-undecane sulfonic acid (MUS) have been extensively studied because of ...

Hierarchical and Programmable One-Pot Oligosaccharide Synthesis

階層的でプログラム可能なワンポットオリゴ糖合成

This article presents a general experimental protocol for programmable one-pot oligosaccharide synthesis and demonstrates how to use Auto-CHO software for ...