Name: synthesis of hydrogels with antifouling properties as membranes for water purification
Uploaded: 2017-04-07T14:00:00.000+00:00
Duration: 7 min 32 s
Description: Watch this Scientific Journal Video about Synthesis of Hydrogels with Antifouling Properties As Membranes for Water Purification at JoVE.com

We gratefully acknowledge the financial support of this work by the Korean Carbon Capture and Sequestration R&amp;D Center (KCRC).

プレポリマー溶液の調製<ol><li> 調製溶媒として水を使用して <ol><li>磁気撹拌棒をガラスボトルに脱イオン（DI）水の10.00グラムを追加します。 </li><li> SBMAの2.00グラムを測定し、水を含むガラスびんに移します。 SBMAが完全に溶解するまで、30分間溶液を撹拌しました。 </li><li>別個の瓶に、（M、N = 700グラム/モル）PEGDAの20.00グラムを加えます。 </li><li> PEGDA溶液に、1-ヒドロキシシクロヘキシルフェニルケトン（HCPK）の20.0 mgの、光開始剤を加えます。少なくとも30分間溶液を撹拌してみましょう。 </li><li>使い捨てピペットを用いて、SBMA水溶液にPEGDA-HCPK溶液8.00グラムを転送します。溶液が均一になるまで継続し、混合物を攪拌。 </li></ol></li><li> 溶媒として水/エタノール混合物を用いて調製 <ol><li> DI水の6.00グラムと、磁気攪拌棒を備えたアンバー・グラスボトルにエタノール4.00グラムを追加します。徹底的な混合を可能にするソリューションをかき混ぜます。 </li><li>水/エタノール混合物にSBMAの2.00グラムを追加します。ソリューションを攪拌し、SBMAが完全に溶解することができます。 </li><li> SBMA混合物にPEGDA-HCPK溶液8.00グラムを転送するためにピペットを使用。溶液を十分に混合するために攪拌します。 </li></ol></li></ol>自立フィルムの調製<ol><li>きれいな石英ディスク上の既知の厚さを持つ2つのスペーサを置きます。スペーサの厚さは、得られたポリマーフィルム19の厚さを制御します。 </li><li>使い捨てピペットを用いて石英ディスクにプレポリマー溶液の少量（〜1.0 ml）を転送します。 </li><li>液体の上に別の石英ディスクを置き、液体膜に気泡が存在しないことを確認してください。 </li><li>紫外線（UV）架橋剤中のサンプルを置き、254nmで19の波長を有するUV光を用いて5分間照射します。 注：代替照射時間sおよび波長は、光開始剤の種類に応じて使用することができます。 </li><li>鋭い刃を用いて石英ディスクからポリマーフィルムを分離します。 DI水浴にフィルムを転送するためにピンセットを使用してください。膜からの溶媒、未反応モノマー/架橋剤、及びゾルを除去するために、最初の24時間中に2回水を変更します。 注：いずれかが存在する場合、ポリマーフィルムは、細孔構造を維持するためにDI水に保管してください。 </li><li> ATR-FTIRおよびDSC分析のための乾燥したフィルムを準備します。 <ol><li>水浴からフィルムを取り出し、それを24時間空気乾燥することができます。 </li><li>真空下で一晩乾燥を80℃の真空オーブン中でフィルムを置き。 </li></ol></li></ol>含浸膜の調製<ol><li>石英ディスク上に多孔質支持体のシートを置きます。 </li><li>支持体の各側には、水/エタノール混合物4に基づいてプレポリマー溶液で2回、フォームブラシをコート使用します。 注：以来トン彼のサポートが疎水性である、エタノールを含有するプレポリマー溶液は、簡単にサポートを濡らしすることができます。 </li><li>サポートの上に別の石英ディスクを置きます。 </li><li> UV架橋剤に試料を置き、254nmの波長を有するUV光を用いて5分間照射します。 </li><li>石英ディスクから含浸膜を除去するために、5分間DI水浴中でアセンブリ全体を浸漬し、慎重に鋭い刃とピンセットを用いて膜を除去します。 </li><li> DI水中で膜を保管してください。溶剤、未反応モノマー/架橋剤、及び膜からゾルを削除するために二回水を変更します。 </li><li> ATR-FTIRおよびDSC分析のために乾燥させ、含浸させた膜を準備します。 <ol><li>水浴から膜を取り外します。膜を24時間周囲条件で乾燥させます。 </li><li>真空下80℃で真空オーブン中で一晩、膜を乾燥させます。 </li></ol></li></ol>自立フィルムおよび含浸ミーの4キャラクタリゼーションmbranes <ol><li> ATR-FTIR分析 <ol><li> FTIR分析のために、ステップ1.1で述べたように、プレポリマー溶液のサンプルを調製。 </li><li>サンプルをスキャンする前に、バックグラウンドスキャンを実行します。 600センチメートル-1から4500センチメートルに波数範囲を設定-1計測の4 -1の解像度で。 </li><li>分析のためのFTIR機でサンプルを置きます。 </li><li>サンプルを削除します。水晶と適切な溶媒で先端を清掃してください。 </li><li>多孔質支持体、プレポリマー溶液、乾燥した自立型のフィルムを、含浸膜を乾燥させ、次のサンプルのために4.1.4 - を繰り返して、4.1.1を繰り返します。 </li></ol></li><li> 差動スキャン熱量測定（DSC） <ol><li>計量バランスのDSCパンと蓋を置き、自分の体重を記録します。 </li><li>パン内の試料の少量（5~10 mg）を置き、蓋を閉じます。 </li><li>サンプルを含むパンを秤量します。 Oの重量差からccupied鍋と蓋と空い鍋と蓋は、試料の重量を計算します。 </li><li>プレスを使用して、気密パン内の試料を密封します。 </li><li>不活性基準が配置されているDSCセル内部密封パンを置きます。 </li><li>空い鍋と蓋の重量とプログラム内の試料の重量を入力します。 </li><li> 10℃/分の加熱速度で160℃まで-80℃からDSCを用いて走査します。 </li><li>製造業者のプロトコルを使用してDSC分析を実行します。 </li><li>前述の手順に従って、異なる試料のDSC実験を繰り返します。 </li></ol></li><li> ペンダントドロップ法を用いて、接触角の測定 <ol><li>膜試料（6ミリメートルによる約30mm）の長方形のストリップを切断します。 </li><li> 10分間、DI水にこのストリップを浸漬した後、5分間、それを乾燥させます。 </li><li>試料ホルダーに乾燥した試料を置きます。 </li><li>透明で試料ホルダーを水没DI水20を含む環境チャンバ。 </li><li>ステンレス鋼針をマイクロシリンジを用いて、膜試料上のn -デカン（約1μL）の滴を分配します。 </li><li>液滴の安定化を確実にするために2分間邪魔されずにセットアップを残します。 </li><li>膜表面上に分配液滴の角度を測定することにより試料の接触角を決定するために、適切な画像解析ソフトウェアを使用。 </li><li>様々な液滴に対して得られた接触角値の平均を取ります。 </li></ol></li><li> デッドエンド濾過システムを用いて、水透過性の特徴付け <ol><li>自立フィルムおよび含浸膜のクーポンを切断するために適切な直径を有するハンマー駆動穴パンチを使用します。 </li><li>デッドエンドろ過セル内部の多孔性支持体上に準備されたクーポンを置きます。 </li><li>サンプルの上にOリングを置きます。二つの半分をねじ込み透過セルのまとめ。 </li><li>透過セルにDI水の約50ミリリットルを加えます。キャップにねじ込み、マグネチックスターラー上で透過セルを配置します。 300と900 rpmの間の撹拌速度を設定します。 </li><li>透過水を収集するために、バランスの上に覆われたビーカーを置きます。風袋引き。 </li><li>ガスボンベのバルブを開きます。所望の圧力は、（自立フィルム45 PSIGおよび含浸膜35 PSIG）に到達するまで圧力調整弁を時計回りに回します。 </li><li>透過セルに圧力を提供するために放出弁を開きます。 </li><li>監視し、時間の経過とともに、ビーカーの重量を記録。 </li><li>水透過性（W）を算出し、透過度（P w）を 4未満に示す溶液-拡散モデルを用いて、21 <img alt="方程式" src="/files/ftp_upload/55426/55426eq1.jpg" /> ここで、wは番目です水濃度（G / L）であり、wは 、Aは、膜の有効面積（mはρE水透過性（L / m 2のHBAR又はLMH /バー）は、P wは 、水透過性（LMHセンチメートル/バー）であります2）において、 量Δmは時間Δt（時間）を超える水透過液（G）の質量の変化であり、Δpが膜（バール）を横切る圧力差であり、Lは膨潤フィルム（CM）の厚さです。 </li><li>膜の防汚性及び排除率を評価するためのpH = 7.4のリン酸緩衝生理食塩水（PBS）溶液中、0.5g / LのBSAを含有するBSA溶液を使用します。 </li><li> BSAの存在下で水フラックスを決定するために、4.4.10 - 繰り返し4.4.5ステップ。次の式22とBSA阻止率を算出 <img alt="方程式" src="/files/ftp_upload/55426/55426eq2.jpg" /> R BSAは、膜（％）のBSA除去率であり、C Pは透過物（G / L）中のBSAの濃度であり、C Fは供給量（g / L）中のBSAの濃度です。 BSAの濃度は、UV分光法により決定することができます。 </li></ol></li></ol>

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The authors declare that they have no competing financial interests.

我々は、自立フィルムおよび両性イオン性ヒドロゲルに基づいた含浸膜を調製する容易な方法を実証しました。 3（メタ）アクリレートの特徴的なピーク（ すなわち 、810、1,190、及び1410センチメートル-1）得られたポリマーフィルムのIRスペクトルでの消失、膜を含浸させた（ 図2）は 、モノマーおよび架橋剤4の良好な変換を示し<sup class...

増大する需要を満たすためにきれいな水を生成するために、低コストかつエネルギー効率の高い技術を開発する大きな必要性があります。ポリマー膜は、動作1におけるそれらの高いエネルギー効率、低コスト、および単純として、それらの固有の利点に水浄化のための主要な技術として浮上しています。膜は、純水を透過して汚染物質を拒否することができます。しかしながら、膜は、しばしば、それらの有利な相互作用2、3から膜表面に吸着することができる給水中の汚染物質により汚染にさらされます。ファウリングは劇的に必要な膜面積及び水の浄化のコストを増加させる、膜を通して水の流量を減少させることができます。 ファウリングを軽減する効果的なアプローチは、親水性を増加させ、従って良好でを減少させるために、膜表面を改質することです膜表面と汚染物質との間のteractions。一つの方法は、超親水3つのヒドロゲルで薄膜コーティングを使用することです。ヒドロゲルは、多くの場合、高い透水性を持っています。従って、薄膜コーティングは、膜全体を横切るわずかに増加輸送抵抗にもかかわらず、原因緩和ファウリングに膜を通して長期水透過性を増加させることができます。ヒドロゲルはまた、直接浸透アプリケーション4に水浄化用含浸膜に製造することができます。 双性イオン性材料は、正味中性の電荷の両方正と負に帯電した官能基を含有し、静電誘導される水素結合5、6、7、8、9を介して強い表面の水和を有します。強固に結合した水和層は、物理として機能しますエネルギー障壁は、表面に付着する汚染物質を防止する優れた防汚特性10を示します。増加する両性イオン性ポリ（スルホベタインメタクリレート）などのポリマー、（PSBMA）およびポリ（カルボキシベタインメタクリレート）（のpCBMA）11を塗布して膜表面を修飾するために使用されてきた、12、13、14、15、16、17、18表面親水性、したがって防汚性。 ここでは、機械的強度を向上させるために、ポリ（エチレングリコール）ジアクリレート（PEGDA、M N = 700グラム/モル）を使用して架橋される重合を介して、スルホベタインメタクリレート（SBMA）を使用して双性イオン性ヒドロゲルを調製する容易な方法を実証します。我々はまた、提示光重合前に高度に多孔質の疎水性支持体にモノマーと架橋剤を含浸させて堅牢な膜を構築する手順。自立フィルムおよび含浸膜の物理的及び水輸送特性を徹底的に水の浄化のための構造/特性関係を解明することを特徴とします。調製したヒドロゲルは膜の分離特性を向上させるために表面コーティングとして用いることができます。架橋密度を調整することにより、または疎水性多孔質支持体に含浸させることによって、これらの材料はまた、正浸透又は圧力遅延浸透4として浸透プロセスのための十分な機械的強度を有する薄膜を形成することができます。

<table><tbody><tr><td>Poly(ethylene glycol) diacrylate&amp;nbsp;&amp;nbsp;&amp;nbsp;&amp;nbsp;&amp;nbsp;&amp;nbsp;&amp;nbsp;&amp;nbsp;&amp;nbsp;&amp;nbsp;&amp;nbsp;&amp;nbsp;&amp;nbsp;&amp;nbsp;&amp;nbsp;&amp;nbsp;&amp;nbsp; M&lt;sub&gt;n&lt;/sub&gt; = 700 (PEGDA)</td><td>Sigma Aldrich</td><td>455008</td><td></td></tr><tr><td>1-Hydroxycyclohexyl phenyl ketone, 99% (HCPK)</td><td>Sigma Aldrich</td><td>405612</td><td></td></tr><tr><td>[2-(Methacrloyloxy)ethyl dimethyl-(3-sulfopropyl) ammonium hydroxide, 97%</td><td>Sigma Aldrich</td><td>537284</td><td>Acutely Toxic</td></tr><tr><td>Ethanol, 95%</td><td>Koptec, VWR International</td><td>V1101</td><td>Flamable</td></tr><tr><td>Decane, anhydrous, 99%</td><td>Sigma Aldrich</td><td>457116</td><td></td></tr><tr><td>Solupor Membrane</td><td>Lydall</td><td>7PO7D</td><td></td></tr><tr><td>Micrometer&amp;nbsp;</td><td>Starrett</td><td>2900-6</td><td></td></tr><tr><td>ATR-FTIR</td><td>Vertex 70</td><td></td><td></td></tr><tr><td>DSC: TA Q2000</td><td>TA Instruments</td><td></td><td></td></tr><tr><td>Rame&amp;rsquo;-hart Goniometer: Model 190</td><td>Rame&amp;rsquo;-hart Instruments</td><td></td><td></td></tr><tr><td>Ultraviolet Crosslinker: CX-2000</td><td>Ultra-Violet Products</td><td></td><td>UV radiation&amp;nbsp;</td></tr><tr><td>Permeation Cell: Model UHP-43</td><td>Advantec MFS</td><td></td><td></td></tr><tr><td>Deionized Water: Milli-Q Water</td><td>EMD Millipore</td><td></td><td></td></tr></tbody></table>

synthesis of hydrogels with antifouling properties as membranes for water purification

ヒドロゲルは広く防汚性を増加させ、したがって、経時膜を通して安定した水透過性を達成する、浄水のための膜の表面の親水性を高めるために利用されてきました。ここでは、膜用途のための両性イオンに基づくヒドロゲルを製造するための容易な方法を報告しています。自立フィルムは、光重合を介してポリ架橋剤（エチレングリコール）ジアクリレート（PEGDA）とスルホベタインメタクリレート（SBMA）から調製することができます。ヒドロゲルはまた、機械的強度を高めるために、疎水性の多孔性支持体に含浸させることにより調製することができます。これらのフィルムは、ポリマー鎖のダイナミクスのための親水性および示差走査熱量測定（DSC）のためのゴニオメータを用いて、（メタ）アクリレート基の転化の程度を決定するための赤外分光法（ATR-FTIR）を形質転換減衰全反射フーリエ変換によって特徴付けることができます。また、デッドエンドFILTRAに透水性を決定するためのプロトコルを報告しますンシステム及び膜性能に対する汚染物質の影響（ウシ血清アルブミン、BSA）。

ステップ1.1と1.2で指定されたプレポリマー溶液を用いて調製した自立膜は、それぞれ、S50とS30と呼ばれます。詳細情報は、表1に示されています。ステップ1.2で指定されたプレポリマー溶液はまた、IMS30として示される含浸膜を作製しました。多孔性支持体を疎水性ポリエチレンで作られているので、エタノールを含?...

Watch this Scientific Journal Video about Synthesis of Hydrogels with Antifouling Properties As Membranes for Water Purification at JoVE.com

Synthesis of Hydrogels with Antifouling Properties As Membranes for Water Purification

This paper reports practical methods to prepare hydrogels in freestanding films and impregnated membranes and to characterize their physical properties, including water transport properties.

水質浄化のための膜のような防汚特性を持つハイドロゲルの合成

Hydrogels have been widely utilized to enhance the surface hydrophilicity of membranes for water purification, increasing the antifouling properties and ...

synthesis-hydrogels-with-antifouling-properties-as-membranes-for

Universidad de Cartagena UDEC

Research

JoVE Journal

Bioengineering

9.3K ビュー.  The State University of New York at Buffalo. This paper reports practical methods to prepare hydrogels in freestanding films and impregnated membranes and to characterize their physical properties, including water transport properties. 

ビデオ: Synthesis of Hydrogels with Antifouling Properties As Membranes for Water Purification

Electrophoretic Crystallization of Ultrathin High-performance Metal-organic Framework Membranes

We report the synthesis of thin, highly intergrown, polycrystalline metal-organic framework (MOF) membranes on a wide range of unmodified porous and non-porous supports (polymer, ceramic, metal, carbon, and graphene). We developed a novel crystallization technique, which is termed the ENACT approach: the electrophoretic nuclei assembly for the crystallization of highly intergrown thin films (ENACT). This approach allows for a high density of heterogeneous nucleation of MOFs on a chosen substrate via the electrophoretic deposition (EPD) directly from the precursor sol. The growth of well-packed MOF nuclei leads to a highly intergrown polycrystalline MOF film. We show that this simple approach can be used for the synthesis of thin, intergrown zeolite imidazole framework (ZIF)-7 and ZIF-8 films. The resulting 500 nm-thick ZIF-8 membranes show a considerably high H2 permeance (8.3 x 10-6 mol m-2 s-1 Pa-1) and ideal gas selectivities (7.3 for H2/CO2, 15.5 for H2/N2, 16.2 for H2/CH4, and 2655 for H2/C3H8). An attractive performance for C3H6/C3H8 separation is also achieved (a C3H6 permeance of 9.9 x 10-8 mol m-2 s-1 Pa-1 and a C3H6/C3H8 ideal selectivity of 31.6 at 25 &#176;C). Overall, the ENACT process, owing to its simplicity, can be extended to synthesize intergrown thin films of a wide range of nanoporous crystalline materials.

A simple, reproducible, and versatile approach for the synthesis of intergrown, polycrystalline metal-organic framework membranes on a wide range of unmodified porous and non-porous supports is presented.

極薄高性能金属有機性フレームワーク膜の電気泳動の結晶化

We report the synthesis of thin, highly intergrown, polycrystalline metal-organic framework (MOF) membranes on a wide range of unmodified porous and ...

化学

Fabricating Superhydrophobic Polymeric Materials for Biomedical Applications

Superhydrophobic materials, with surfaces possessing permanent or metastable non-wetted states, are of interest for a number of biomedical and industrial applications. Here we describe how electrospinning or electrospraying a polymer mixture containing a biodegradable, biocompatible aliphatic polyester (e.g., polycaprolactone and poly(lactide-co-glycolide)), as the major component, doped with a hydrophobic copolymer composed of the polyester and a stearate-modified poly(glycerol carbonate) affords a superhydrophobic biomaterial. The fabrication techniques of electrospinning or electrospraying provide the enhanced surface roughness and porosity on and within the fibers or the particles, respectively. The use of a low surface energy copolymer dopant that blends with the polyester and can be stably electrospun or electrosprayed affords these superhydrophobic materials. Important parameters such as fiber size, copolymer dopant composition and/or concentration, and their effects on wettability are discussed. This combination of polymer chemistry and process engineering affords a versatile approach to develop application-specific materials using scalable techniques, which are likely generalizable to a wider class of polymers for a variety of applications.

Two- and three-dimensional superhydrophobic polymeric materials are prepared by electrospinning or electrospraying biodegradable polymers blended with a lower surface energy polymer of similar composition.

バイオメディカル応用のための超疎水性高分子材料を製造します

Superhydrophobic materials, with surfaces possessing permanent or metastable non-wetted states, are of interest for a number of biomedical and industrial ...

生物工学

Three-Dimensionally Printed Microfluidic Cross-flow System for Ultrafiltration/Nanofiltration Membrane Performance Testing

Minimization and management of membrane fouling is a formidable challenge in diverse industrial processes and other practices that utilize membrane technology. Understanding the fouling process could lead to optimization and higher efficiency of membrane based filtration. Here we show the design and fabrication of an automated three-dimensionally (3-D) printed microfluidic cross-flow filtration system that can test up to 4 membranes in parallel. The microfluidic cells were printed using multi-material photopolymer 3-D printing technology, which used a transparent hard polymer for the microfluidic cell body and incorporated a thin rubber-like polymer layer, which prevents leakages during operation. The performance of ultrafiltration (UF), and nanofiltration (NF) membranes were tested and membrane fouling could be observed with a model foulant bovine serum albumin (BSA). Feed solutions containing BSA showed flux decline of the membrane. This protocol may be extended to measure fouling or biofouling with many other organic, inorganic or microbial containing solutions. The microfluidic design is especially advantageous for testing materials that are costly or only available in small quantities, for example polysaccharides, proteins, or lipids due to the small surface area of the membrane being tested. This modular system may also be easily expanded for high throughput testing of membranes.&#160;

Design and fabrication of a three-dimensionally (3-D) printed microfluidic cross-flow filtration system is demonstrated. The system is used to test performance and observe fouling of ultrafiltration and nanofiltration (thin film composite) membranes.

限外濾過/ナノ濾過膜性能試験のための三次元プリントマイクロ流体クロスフローシステム

Minimization and management of membrane fouling is a formidable challenge in diverse industrial processes and other practices that utilize membrane ...

Proof-of-Concept for Gas-Entrapping Membranes Derived from Water-Loving SiO2/Si/SiO2 Wafers for Green Desalination

Desalination through direct contact membrane distillation (DCMD) exploits water-repellent membranes to robustly separate counterflowing streams of hot and salty seawater from cold and pure water, thus allowing only pure water vapor to pass through. To achieve this feat, commercial DCMD membranes are derived from or coated with water-repellent perfluorocarbons such as polytetrafluoroethylene (PTFE) and polyvinylidene difluoride (PVDF). However, the use of perfluorocarbons is limiting due to their high cost, non-biodegradability, and vulnerability to harsh operational conditions. Unveiled here is a new class of membranes referred to as gas-entrapping membranes (GEMs) that can robustly entrap air upon immersion in water. GEMs achieve this function by their microstructure rather than their chemical make-up. This work demonstrates a proof-of-concept for GEMs using intrinsically wetting SiO2/Si/SiO2 wafers as the model system; the contact angle of water on SiO2 is &#952;o &#8776; 40&#176;. Silica-GEMs had 300 &#956;m-long cylindrical pores whose diameters at the (2 &#956;m-long) inlet and outlet regions were significantly smaller; this geometrically discontinuous structure, with 90&#176; turns at the inlets and outlets, is known as the &#34;reentrant microtexture&#34;. The microfabrication protocol for silica-GEMs entails designing, photolithography, chrome sputtering, and isotropic and anisotropic etching. Despite the water loving nature of silica, water does not intrude silica-GEMs on submersion. In fact, they robustly entrap air underwater and keep it intact even after six weeks (&#62;106 seconds). On the other hand, silica membranes with simple cylindrical pores spontaneously imbibe water (&#60; 1 s). These findings highlight the potential of the GEMs architecture for separation processes. While the choice of SiO2/Si/SiO2 wafers for GEMs is limited to demonstrating the proof-of-concept, it is expected that the protocols and concepts presented here will advance the rational design of scalable GEMs using inexpensive common materials for desalination and beyond.

Proof-of-Concept for Gas-Entrapping Membranes Derived from Water-Loving SiO2/Si/SiO2 Wafers for Green Desalination

Presented here is a stepwise protocol for realizing gas-entrapping membranes (GEMs) from SiO2/Si wafers using integrated circuit microfabrication technology. When silica-GEMs are immersed in water, the intrusion of water is prevented, despite the water-loving composition of silica.

水を愛するSiO2 /Si/SiO2ウェハーから得られるガス包み込み膜の概念実証

Desalination through direct contact membrane distillation (DCMD) exploits water-repellent membranes to robustly separate counterflowing streams of hot and ...

工学

Fabricating Degradable Thermoresponsive Hydrogels on Multiple Length Scales via Reactive Extrusion, Microfluidics, Self-assembly, and Electrospinning

While various smart materials have been explored for a variety of biomedical applications (e.g., drug delivery, tissue engineering, bioimaging, etc.), their ultimate clinical use has been hampered by the lack of biologically-relevant degradation observed for most smart materials. This is particularly true for temperature-responsive hydrogels, which are almost uniformly based on polymers that are functionally non-degradable (e.g., poly(N-isopropylacrylamide) (PNIPAM) or poly(oligoethylene glycol methacrylate) (POEGMA)). As such, to effectively translate the potential of thermoresponsive hydrogels to the challenges of remote-controlled or metabolism-regulated drug delivery, cell scaffolds with tunable cell-material interactions, theranostic materials with the potential for both imaging and drug delivery, and other such applications, a method is required to render the hydrogels (if not fully degradable) at least capable of renal clearance following the required lifetime of the material. To that end, this protocol describes the preparation of hydrolytically-degradable hydrazone-crosslinked hydrogels on multiple length scales based on the reaction between hydrazide and aldehyde-functionalized PNIPAM or POEGMA oligomers with molecular weights below the renal filtration limit. Specifically, methods to fabricate degradable thermoresponsive bulk hydrogels (using a double barrel syringe technique), hydrogel particles (on both the microscale through the use of a microfluidics platform facilitating simultaneous mixing and emulsification of the precursor polymers and the nanoscale through the use of a thermally-driven self-assembly and cross-linking method), and hydrogel nanofibers (using a reactive electrospinning strategy) are described. In each case, hydrogels with temperature-responsive properties similar to those achieved via conventional free radical cross-linking processes can be achieved, but the hydrazone cross-linked network can be degraded over time to re-form the oligomeric precursor polymers and enable clearance. As such, we anticipate these methods (which may be generically applied to any synthetic water-soluble polymer, not just smart materials) will enable easier translation of synthetic smart materials to clinical applications.

Protocols are described for the fabrication of degradable thermoresponsive hydrogels based on hydrazone cross-linking of polymeric oligomers on the bulk scale, microscale, and nanoscale, the latter for preparation of both gel nanoparticles and nanofibers.

自己組織化反応押出、マイクロフルイディクス, 経由で複数の長さスケールでの分解性感温ハイドロゲルを加工・ エレクトロスピニング

While various smart materials have been explored for a variety of biomedical applications (e.g., drug delivery, tissue engineering, bioimaging, etc.), ...

Ultrathin Porated Elastic Hydrogels As a Biomimetic Basement Membrane for Dual Cell Culture

The basement membrane is a critical component of cellular bilayers that can vary in stiffness, composition, architecture, and porosity. In vitro studies of endothelial-epithelial bilayers have traditionally relied on permeable support models that enable bilayer culture, but permeable supports are limited in their ability to replicate the diversity of human basement membranes. In contrast, hydrogel models that require chemical synthesis are highly tunable and allow for modifications of both the material stiffness and the biochemical composition via incorporation of biomimetic peptides or proteins. However, traditional hydrogel models are limited in functionality because they lack pores for cell-cell contacts and functional in vitro migration studies. Additionally, due to the thickness of traditional hydrogels, incorporation of pores that span the entire thickness of hydrogels has been challenging. In the present study, we use poly-(ethylene-glycol) (PEG) hydrogels and a novel zinc oxide templating method to address the previous shortcomings of biomimetic hydrogels. As a result, we present an ultrathin, basement membrane-like hydrogel that permits the culture of confluent cellular bilayers on a customizable scaffold with variable pore architectures, mechanical properties, and biochemical composition.

Current bilayer culture models do not allow for functional in vitro studies that mimic in vivo microenvironments. Using polyethylene glycol and a zinc oxide templating method, this protocol describes the development of an ultrathin biomimetic basement membrane with tunable stiffness, porosity, and biochemical composition that closely mimics in vivo extracellular matrices.

デュアルのバイオミメティック基底膜として極薄 Porated 弾性ゲルの細胞培養

The basement membrane is a critical component of cellular bilayers that can vary in stiffness, composition, architecture, and porosity. In vitro studies ...

An Additive Manufacturing Technique for the Facile and Rapid Fabrication of Hydrogel-based Micromachines with Magnetically Responsive Components

Polyethylene glycol (PEG)-based hydrogels are biocompatible hydrogels that have been approved for use in humans by the FDA. Typical PEG-based hydrogels have simple monolithic architectures and often function as scaffolding materials for tissue engineering applications. More sophisticated structures typically take a long time to fabricate and do not contain moving components. This protocol describes a photolithography method that allows for facile and rapid microfabrication of PEG structures and devices. This strategy involves an in-house developed fabrication stage that allows for the rapid fabrication of 3D structures by building upwards in a layer-by-layer fashion. Independent moving components can also be aligned and assembled onto support structures to form integrated devices. These independent components are doped with superparamagnetic iron oxide nanoparticles that are sensitive to magnetic actuation. In this manner, the fabricated devices can be actuated using external magnets to yield movement of the components within. Hence, this technique allows for the fabrication of sophisticated MEMS-like devices (micromachines) that are composed entirely out of a biocompatible hydrogel, able to function without an onboard power source, and respond to a contact-less method of actuation. This manuscript describes the fabrication of both the fabrication set-up as well as the step-by-step method for the microfabrication of these hydrogels-based MEMS-like devices.

An additive manufacturing strategy for processing UV-crosslinkable hydrogels has been developed. This strategy allows for the layer-by-layer assembly of microfabricated hydrogel structures as well as the assembly of independent components, yielding integrated devices containing moving components that are responsive to magnetic actuation.

ハイドロゲルを用いたマイクロ磁気応答性の高いコンポーネントとの容易な迅速な製造のための製造技術の添加剤

Polyethylene glycol (PEG)-based hydrogels are biocompatible hydrogels that have been approved for use in humans by the FDA. Typical PEG-based hydrogels ...

Photodegradable Hydrogel Interfaces for Bacteria Screening, Selection, and Isolation

Biologists have long attempted to understand the relationship between phenotype and genotype. To better understand this connection, it is crucial to develop practical technologies that couple microscopic cell screening with cell isolation at high purity for downstream genetic analysis. Here, the use of photodegradable poly(ethylene glycol) hydrogels for screening and isolation of bacteria with unique growth phenotypes from heterogeneous cell populations is described. The method relies on encapsulating or entrapping cells with the hydrogel, followed by culture, microscopic screening, then use of a high-resolution light patterning tool for spatiotemporal control of hydrogel degradation and release of selected cells into a solution for retrieval. Applying different light patterns allows for control over the morphology of the extracted cell, and patterns such as rings or crosses can be used to retrieve cells with minimal direct UV light exposure to mitigate DNA damage to the isolates. Moreover, the light patterning tool delivers an adjustable light dose to achieve various degradation and cell release rates. It allows for degradation at high resolution, enabling cell retrieval with micron-scale spatial precision. Here, the use of this material to screen and retrieve bacteria from both bulk hydrogels and microfabricated lab-on-a-chip devices is demonstrated. The method is inexpensive, simple, and can be used for common and emerging applications in microbiology, including isolation of bacterial strains with rare growth profiles from mutant libraries and isolation of bacterial consortia with emergent phenotypes for genomic characterizations.

The use of photodegradable hydrogels to isolate bacterial cells by utilizing a high-resolution light pattering tool is reported. Essential experimental procedures, results, and advantages of the process are reviewed. The method enables rapid and inexpensive isolation of targeted bacteria showing rare or unique functions from heterogeneous communities or populations.

細菌スクリーニング、選択、および分離のための光分解性ヒドロゲルインターフェース

Biologists have long attempted to understand the relationship between phenotype and genotype. To better understand this connection, it is crucial to ...

Synthesis of Strong Adhesive Hydrogel, Gelatin O-Nitrosobenzaldehyde

Adhesive materials have become popular biomaterials in the field of biomedical and tissue engineering. In our previous work, we presented a new material - gelatin o-nitrosobenzaldehyde (gelatin-NB) - which is mainly used for tissue regeneration and has been validated in animal models of corneal injury and inflammatory bowel disease. This is a novel hydrogel formed by modifying biological gelatin with o-nitrosobenzaldehyde (NB). Gelatin-NB was synthesized by activating the carboxyl group of NB-COOH and reacting with gelatin through 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (EDC) and N-hydroxysuccinimide (NHS). The obtained compound was purified to generate the final product, which can be stably stored for at least 18 months. NB has a strong adhesion to -NH2 on the tissue, which can form many C = N bonds, thus increasing the adhesion of gelatin-NB to the tissue interface. The preparation process comprises steps for the synthesis of the NB-COOH group, modification of the group, synthesis of gelatin-NB, and purification of the compound. The goal is to describe the specific synthesis process of gelatin-NB in detail and to demonstrate the application of gelatin-NB to damage repair. Moreover, the protocol is presented to further strengthen and expand the nature of the material produced by the scientific community for more applicable scenarios.

The protocol presented here shows the synthesis of a strong adhesive hydrogel gelatin o-nitrosobenzaldehyde (gelatin-NB). Gelatin-NB has rapid and efficient tissue adhesion ability, which can form a strong physical barrier to protect wound surfaces, so it is expected to be applied to the field of injury repair biotechnology.

強接着性ハイドロゲルゼラチンO-ニトロソベンズアルデヒドの合成

Adhesive materials have become popular biomaterials in the field of biomedical and tissue engineering. In our previous work, we presented a new material - ...

CFPS反応の各種ハイドロゲルマトリックスへの埋め込み

Methods for Embedding Cell-Free Protein Synthesis Reactions in Macro-Scale Hydrogels

Synthetic gene networks provide a platform for scientists and engineers to design and build novel systems with functionality encoded at a genetic level. While the dominant paradigm for the deployment of gene networks is within a cellular chassis, synthetic gene networks may also be deployed in cell-free environments. Promising applications of cell-free gene networks include biosensors, as these devices have been demonstrated against biotic (Ebola, Zika, and SARS-CoV-2 viruses) and abiotic (heavy metals, sulfides, pesticides, and other organic contaminants) targets. Cell-free systems are typically deployed in liquid form within a reaction vessel. Being able to embed such reactions in a physical matrix, however, may facilitate their broader application in a wider set of environments. To this end, methods for embedding cell-free protein synthesis (CFPS) reactions in a variety of hydrogel matrices have been developed. One of the key properties of hydrogels conducive to this work is the high-water reconstitution capacity of hydrogel materials. Additionally, hydrogels possess physical and chemical characteristics that are functionally beneficial. Hydrogels can be freeze-dried for storage and rehydrated for use later. Two step-by-step protocols for the inclusion and assay of CFPS reactions in hydrogels are presented. First, a CFPS system can be incorporated into a hydrogel via rehydration with a cell lysate. The system within the hydrogel can then be induced or expressed constitutively for complete protein expression through the hydrogel. Second, cell lysate can be introduced to a hydrogel at the point of polymerization, and the entire system can be freeze-dried and rehydrated at a later point with an aqueous solution containing the inducer for the expression system encoded within the hydrogel. These methods have the potential to allow for cell-free gene networks that confer sensory capabilities to hydrogel materials, with the potential for deployment beyond the laboratory.

著者スポットライト:ハイドロゲルに無細胞タンパク質合成反応を埋め込むための新しいアプローチ 

Here, we present two protocols for embedding cell-free protein synthesis reactions in macro-scale hydrogel matrices without the need for an external liquid phase.

マクロスケールハイドロゲルへの無細胞タンパク質合成反応の埋め込み法

Synthetic gene networks provide a platform for scientists and engineers to design and build novel systems with functionality encoded at a genetic level. ...

水質浄化のための膜のような防汚特性を持つハイドロゲルの合成

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極薄高性能金属有機性フレームワーク膜の電気泳動の結晶化

バイオメディカル応用のための超疎水性高分子材料を製造します

限外濾過/ナノ濾過膜性能試験のための三次元プリントマイクロ流体クロスフローシステム

水を愛するSiO2 /Si/SiO₂ウェハーから得られるガス包み込み膜の概念実証

自己組織化反応押出、マイクロフルイディクス, 経由で複数の長さスケールでの分解性感温ハイドロゲルを加工・エレクトロスピニング

デュアルのバイオミメティック基底膜として極薄 Porated 弾性ゲルの細胞培養

ハイドロゲルを用いたマイクロ磁気応答性の高いコンポーネントとの容易な迅速な製造のための製造技術の添加剤

細菌スクリーニング、選択、および分離のための光分解性ヒドロゲルインターフェース

強接着性ハイドロゲルゼラチンO-ニトロソベンズアルデヒドの合成

マクロスケールハイドロゲルへの無細胞タンパク質合成反応の埋め込み法

水質浄化のための膜のような防汚特性を持つハイドロゲルの合成

要約

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この動画の章

極薄高性能金属有機性フレームワーク膜の電気泳動の結晶化

バイオメディカル応用のための超疎水性高分子材料を製造します

限外濾過/ナノ濾過膜性能試験のための三次元プリントマイクロ流体クロスフローシステム

水を愛するSiO2 /Si/SiO2ウェハーから得られるガス包み込み膜の概念実証

自己組織化反応押出、マイクロフルイディクス, 経由で複数の長さスケールでの分解性感温ハイドロゲルを加工・ エレクトロスピニング

デュアルのバイオミメティック基底膜として極薄 Porated 弾性ゲルの細胞培養

ハイドロゲルを用いたマイクロ磁気応答性の高いコンポーネントとの容易な迅速な製造のための製造技術の添加剤

細菌スクリーニング、選択、および分離のための光分解性ヒドロゲルインターフェース

強接着性ハイドロゲルゼラチンO-ニトロソベンズアルデヒドの合成

マクロスケールハイドロゲルへの無細胞タンパク質合成反応の埋め込み法

水を愛するSiO2 /Si/SiO₂ウェハーから得られるガス包み込み膜の概念実証

自己組織化反応押出、マイクロフルイディクス, 経由で複数の長さスケールでの分解性感温ハイドロゲルを加工・エレクトロスピニング