Name: synthesis of poly(n-isopropylacrylamide) janus microhydrogels for anisotropic thermo-responsiveness and organophilic/hydrophilic loading capability
Uploaded: 2016-02-27T13:00:00
Description: Watch this Scientific Journal Video about Synthesis of PolyN-isopropylacrylamide Janus Microhydrogels for Anisotropic Thermo-responsiveness and Organophilic/Hydrophilic Loading Capability at JoVE.com

This work was supported by the National Research Foundation of Korea (NRF) grant funded by the Korea Government (MSIP (Nos. 2014R1A2A1A01006527 and 2011-0030075).

1. Fremstilling af en Master Mold for Hydrodynamisk Fokusering mikrofluidapparatet (HFMD) gennem Fotolitografi <ol><li> Design en fotomaske for HFMD (figur 1a) ved hjælp af computer-assisteret design (CAD) software i overensstemmelse med producentens protokol. </li><li> Skyl en 4 &#39;siliciumskive med acetone, isopropylalkohol (IPA), og deioniseret (DI) vand til fjernelse af organisk og uorganisk støv fra waferen. </li><li> Rengør siliciumskiven med O 2 plasma ved 100 W strøm i 5 minut...

<ol>
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W. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Poly(N-isopropylacrylamide)+soluble+polymer+supports+in+catalysis+and+synthesis.">Poly(N-isopropylacrylamide) soluble polymer supports in catalysis and synthesis.</a> Macromolecules. 31 (18), 6053-6062 (1998).</li><li>Lapeyre, V., Gosse, I., Chevreux, S., Ravaine, V. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Monodispersed+glucose-responsive+microgels+operating+at+physiological+salinity.">Monodispersed glucose-responsive microgels operating at physiological salinity.</a> Biomacromolecules. 7 (12), 3356-3363 (2006).</li><li>Hoare, T., Pelton, R. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Engineering+glucose+swelling+responses+in+poly(N-isopropylacrylamide)-based+microgels.">Engineering glucose swelling responses in poly(N-isopropylacrylamide)-based microgels.</a> Macromolecules. 40 (3), 670-678 (2007).</li><li>Xu, S., Zhang, J., Paquet, C., Lin, Y., Kumacheva, E. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=From+hybrid+microgels+to+photonic+crystals.">From hybrid microgels to photonic crystals.</a> Adv. 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S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=One-step+microfluidic+synthesis+of+Janus+microhydrogels+with+anisotropic+thermo-responsive+behavior+and+organophilic/hydrophilic+loading+capability.">One-step microfluidic synthesis of Janus microhydrogels with anisotropic thermo-responsive behavior and organophilic/hydrophilic loading capability.</a> Langmuir. 29 (49), 15137-15141 (2013).</li><li>Seo, K. D., Kim, D. S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Microfluidic+synthesis+of+thermo-responsive+poly(N-isopropylacrylamide)-poly(ethylene+glycol)+diacrylate+microhydrogels+as+chemo-embolic+microspheres.">Microfluidic synthesis of thermo-responsive poly(N-isopropylacrylamide)-poly(ethylene glycol) diacrylate microhydrogels as chemo-embolic microspheres.</a> J. Micromech. 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To ikke-blandbare basismaterialer anvendes generelt til at syntetisere Janus microhydrogels. Indtil for nylig var Janus microhydrogels bestående af det samme grundmateriale sjældent rapporteret og de ​​rapporterede Janus microhydrogels ikke havde en klar intern morfologi på grund af forstyrrelser forårsaget af blandbarhed af dets materialer. 35, 36 I denne protokol, demonstrerer vi en metode at syntetisere Janus microhydrogels består udelukkende af den enkelte basismateriale, PNIPAAm, med en klart op...

Hydrogels are a network of hydrophilic polymer chains.1 An increasing amount of research in the field of hydrogels has promoted significant advances and revealed their similarity to biological tissues; the properties of hydrogels allow the uptake of large amounts of water while maintaining their structure. Environmentally responsive hydrogels have also been studied extensively because of their ability to swell or shrink reversibly in response to external stimuli.2 Several triggers, including temperature,3-5 pH,6,7 light,8,9 electric fields,10,11 and specific molecules, such as glucose,12,13 have been suggested to control the geometric shape of hydrogels. Among the many environmentally responsive hydrogels currently available, poly(N-isopropylacrylamide) (PNIPAAm), a well-known thermo-responsive hydrogel, exhibits volume shrinkage above a low critical solution temperature (LCST) of 32 &#176;C.14 A recent study by Sasaki et al.15 reported the intriguing liquid-liquid phase separation of supersaturated NIPAAm, which is the monomer of PNIPAAm. According to this report, supersaturated NIPAAm was dissolved with a 10-fold molar excess of H2O, and soon after, the solution separated into two liquid phases when allows to stand at a temperature above 25 &#176;C; by contrast, dilute NIPAAm was dissolved homogeneously under the same conditions.
Microparticles made of environmentally responsive hydrogels are fascinating candidates for application in drug delivery,16,17 catalysis,18 sensing,19,20 and photonics.21 Traditional synthetic methods including emulsion polymerization, are used to produce hydrogel microparticles with polydispersity.22,23 However, certain applications require microparticles with a narrow size distribution, for example, to stabilize the pharmacokinetics of drug delivery.24 Irregularly shaped or polydisperse embolic microparticles aggregate proximally into clusters, leading to chronic inflammatory responses in embolic particles for cancer therapeutic treatment.25,26
The microfluidic approach is at the forefront of research as a means of fabricating micro-sized particles with narrow size distributions and complex shapes.27-31 The advantages of fabricating microparticles in the microfluidic device are predicated by the small characteristic length of the microfluidic device, which results in a low Reynolds number. In contrast to traditional bulk emulsification where drops are formed in parallel, microdroplets produced in microfluidic devices are generated in series and subsequently polymerized into microparticles upon exposure to UV irradiation. The fundamental principle of droplet formation using a microfluidic device is balance between the interfacial tension and the shear force of the sheath fluid acting on the core fluid. 
Despite the obvious advantages of microfluidic fabrication of droplets/particles, Janus droplets/particles consisting of the same base material are rarely reported because the internal morphology of these droplets/particles is generally disturbed by the diffusion and perturbation of the core fluids. To circumvent this intrinsic limitation, two groups recently reported the preparation of the Janus microparticles by employing heat-induced phase separation of colloidal nanoparticles and UV-directed phase separation.32,33
To this end, we report a microfluidic approach to synthesize Janus microhydrogels entirely composed of a single base material and obtain a product with clearly compartmentalized morphology. Our approach is based on the primary concept of liquid-liquid phase separation of supersaturated NIPAAm monomer. The resulting Janus microhydrogels were found to possess unique properties including anisotropic thermo-responsiveness and organophilic/hydrophilic loading capability.

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	<tbody>
		<tr height="20">
			<td height="20" style="height:20px;width:216px;">Silicon wafer</td>
			<td style="width:88px;">LG Siltron</td>
			<td style="width:119px;">4&#34;, Test grade</td>
			<td style="width:167px;">Wafer for master mold fabrication</td>
		</tr>
		<tr height="60">
			<td height="60" style="height:60px;width:216px;">Acetone</td>
			<td style="width:88px;">Samchun Pure Chemical</td>
			<td style="width:119px;">A0097</td>
			<td>Cleaning silicon wafer</td>
		</tr>
		<tr height="60">
			<td height="60" style="height:60px;width:216px;">Isopropyl alcohol (IPA)</td>
			<td style="width:88px;">Daejung Chemicals &#38; Metals</td>
			<td style="width:119px;">5035-4404</td>
			<td>Cleaning silicon wafer</td>
		</tr>
		<tr height="60">
			<td height="60" style="height:60px;width:216px;">Water purification system</td>
			<td style="width:88px;">Merck Millipore</td>
			<td style="width:119px;">EMD Millipore RIOs Essential 5</td>
			<td>Prepering&#160; deionized water</td>
		</tr>
		<tr height="40">
			<td height="40" style="height:40px;width:216px;">O2 plasma machine</td>
			<td style="width:88px;">Femto Science</td>
			<td style="width:119px;">VITA-A</td>
			<td>Cleaning silicon wafer</td>
		</tr>
		<tr height="40">
			<td height="40" style="height:40px;width:216px;">SU-8 2150 negative photoresist</td>
			<td style="width:88px;">MicroChem</td>
			<td style="width:119px;">Y111077 0500L1GL</td>
			<td>Photoresist for master mold fabrication</td>
		</tr>
		<tr height="40">
			<td height="40" style="height:40px;width:216px;">Hot plate</td>
			<td style="width:88px;">Misung Scientific</td>
			<td style="width:119px;">HP330D, HP150D</td>
			<td>Baking SU-8</td>
		</tr>
		<tr height="40">
			<td height="40" style="height:40px;width:216px;">SU-8 developer</td>
			<td style="width:88px;">Microchem</td>
			<td style="width:119px;">Y020100 4000L1PE</td>
			<td>Developing SU-8</td>
		</tr>
		<tr height="40">
			<td height="40" style="height:40px;width:216px;">Mask aligner system for photolithograpy</td>
			<td style="width:88px;">Shinu Mst Co.</td>
			<td style="width:119px;">CA-6M</td>
			<td>Photolithography</td>
		</tr>
		<tr height="40">
			<td height="40" style="height:40px;width:216px;">Sylgard 184 silicone elastomer kit</td>
			<td style="width:88px;">Dow Corning</td>
			<td style="width:119px;">1064891</td>
			<td>PDMS casting</td>
		</tr>
		<tr height="80">
			<td height="80" style="height:80px;width:216px;">Laboratory Corona Treater</td>
			<td style="width:88px;">Electro-technic Products Inc.</td>
			<td style="width:119px;">Model BD-20AC</td>
			<td>PDMS air plasma treatment&#160;</td>
		</tr>
		<tr height="40">
			<td height="40" style="height:40px;width:216px;">N-isopropylacrylamide (NIPAAm)</td>
			<td style="width:88px;">Sigma-Aldrich</td>
			<td style="width:119px;">415324-50G</td>
			<td>Monomer</td>
		</tr>
		<tr height="60">
			<td height="60" style="height:60px;width:216px;">N,N&#39;-methylenebisacrylamide (MBAAm)</td>
			<td style="width:88px;">Sigma-Aldrich</td>
			<td style="width:119px;">146072-100G</td>
			<td>Crosslinker of NIPAAm</td>
		</tr>
		<tr height="60">
			<td height="60" style="height:60px;width:216px;">4-(2-hydroxyethoxy)phenyl-(2-hydroxy-2-propyl)ketone, Irgacure 2959</td>
			<td style="width:88px;">BASF</td>
			<td style="width:119px;">55047962</td>
			<td>Photoinitiator of NIPAAm</td>
		</tr>
		<tr height="40">
			<td height="40" style="height:40px;">ABIL EM 90</td>
			<td style="width:88px;">Evonik Industries</td>
			<td style="width:119px;">201109</td>
			<td>Sufactant for oil</td>
		</tr>
		<tr height="60">
			<td height="60" style="height:60px;width:216px;">Vortex mixer</td>
			<td style="width:88px;">Scientific Industries Inc.</td>
			<td style="width:119px;">Vortex-Genie 2</td>
			<td>Mixing</td>
		</tr>
		<tr height="60">
			<td height="60" style="height:60px;width:216px;">Tygon tubing</td>
			<td style="width:88px;">Saint-Gobain</td>
			<td style="width:119px;">I.D. 1/32&#34;, O.D. 3/32&#34;, Wall 1/32&#34;</td>
			<td>Connecting tube between syringes and HFMD</td>
		</tr>
		<tr height="40">
			<td height="40" style="height:40px;width:216px;">UV light source</td>
			<td style="width:88px;">Hamamatsu</td>
			<td style="width:119px;">Spot light source LC8</td>
			<td>Polymerization from NIPAAm to PNIPAAm</td>
		</tr>
		<tr height="60">
			<td height="60" style="height:60px;width:216px;">Syringes, NORM-JECT (3ml)</td>
			<td style="width:88px;">Henke-Sass Wolf GmbH</td>
			<td style="width:119px;">22767</td>
			<td>Loading of materials</td>
		</tr>
		<tr height="40">
			<td height="40" style="height:40px;width:216px;">Syringe pump</td>
			<td style="width:88px;">KD Scientific</td>
			<td style="width:119px;">KDS model 200</td>
			<td>Perfusion of materials</td>
		</tr>
		<tr height="40">
			<td height="40" style="height:40px;width:216px;">Tegitol Type NP-10</td>
			<td style="width:88px;">Sigma-Aldrich</td>
			<td style="width:119px;">NP10-500ML</td>
			<td>Surfactant for water</td>
		</tr>
		<tr height="40">
			<td height="40" style="height:40px;width:216px;">Oil red O</td>
			<td style="width:88px;">Sigma-Aldrich</td>
			<td style="width:119px;">O0625-25G</td>
			<td>Dye for N-rich phase</td>
		</tr>
		<tr height="40">
			<td height="40" style="height:40px;width:216px;">Oil Blue N</td>
			<td style="width:88px;">Sigma-Aldrich</td>
			<td style="width:119px;">391557-5G</td>
			<td>Dye for N-rich phase</td>
		</tr>
		<tr height="40">
			<td height="40" style="height:40px;width:216px;">Yellow food dye</td>
			<td style="width:88px;">Edentown F&#38;B</td>
			<td style="width:119px;">NA</td>
			<td>Dye for N-poor phase</td>
		</tr>
		<tr height="40">
			<td height="40" style="height:40px;width:216px;">Green food dye</td>
			<td style="width:88px;">Edentown F&#38;B</td>
			<td style="width:119px;">NA</td>
			<td>Dye for N-poor phase</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">Power supply</td>
			<td style="width:88px;">Agilent</td>
			<td style="width:119px;">E3649A</td>
			<td>Power soruce for thermoelectric moduel</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">Thermoelectric module</td>
			<td style="width:88px;">Peltier</td>
			<td style="width:119px;">FALC1-12710T125</td>
			<td>Temparature control</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">Centrifuge machine</td>
			<td style="width:88px;">Labogene</td>
			<td style="width:119px;">1248R</td>
			<td>Settling down microhydrogels</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">24-well plate</td>
			<td style="width:88px;">SPL Life Sciences</td>
			<td style="width:119px;">32024</td>
			<td>Reservoir for observation</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">Optical microscope</td>
			<td style="width:88px;">Nikon</td>
			<td style="width:119px;">ECLIPSE 80i</td>
			<td>Optical observation</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">Image analysis software</td>
			<td style="width:88px;">IMT i-Solution Inc.</td>
			<td style="width:119px;">iSolutions DT</td>
			<td>Measurement of radius</td>
		</tr>
	</tbody>
</table>

synthesis of poly(n-isopropylacrylamide) janus microhydrogels for anisotropic thermo-responsiveness and organophilic/hydrophilic loading capability

Janus microparticles are compartmentalized particles with differing molecular structures and/or functionality on each of their two sides. Because of this unique property, Janus microparticles have been recognized as a new class of materials, thereby attracting a great deal of attention from various research fields. The versatility of these microparticles has been exemplified through their uses as building blocks for self-assembly, electrically responsive actuators, emulsifiers for painting and cosmetics, and carriers for drug delivery. This study introduces a detailed protocol that explicitly describes a synthetic method for designing novel Janus microhydrogels composed of a single base material, poly(N-isopropylacrylamide) (PNIPAAm). Janus microdroplets are firstly generated via a hydrodynamic focusing microfluidic device (HFMD) based on the separation of a supersaturated aqueous NIPAAm monomer solution and subsequently polymerized through exposure to UV irradiation. The resulting Janus microhydrogels were found to be entirely composed of the same base material, featured an easily identifiable compartmentalized morphology, and exhibited anisotropic thermo-responsiveness and organophilic/hydrophilic loading capability. We believe that the proposed method introduces a novel hydrogel platform with the potential for advanced synthesis of multi-functional Janus microhydrogels.

Figur 3a viser en skematisk afbildning af forsøgsopstillingen anvendes til at syntetisere Janus microhydrogels via HFMD. De N-rige og N-fattige faser blev præcist injiceret i HFMD som centrale væsker 1 og 2 og derefter fusioneret og opdelt i Janus mikrodråber ved åbningen af ​​sheathvæsken af ​​mineralolie på grund af Rayleigh kapillær ustabilitet. Derfor blev Janus mikrodråber sammensat af N-rige og N-fattige faser genereret med succes som vist...

Watch this Scientific Journal Video about Synthesis of PolyN-isopropylacrylamide Janus Microhydrogels for Anisotropic Thermo-responsiveness and Organophilic/Hydrophilic Loading Capability at JoVE.com

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

We present a protocol to synthesize Janus microhydrogels composed entirely of the same base material, poly(N-isopropylacrylamide) (PNIPAAm), with a clearly compartmentalized structure base on the phase separation of a supersaturated NIPAAm monomer solution. The synthesized Janus microhydrogels show unique properties such as anisotropic thermo-responsiveness and organophilic/hydrophilic loading capability.

Syntese af poly (<em&gt; N</em&gt; -isopropylacrylamide) Janus Microhydrogels for Anisotropisk Thermo-lydhørhed og organofile / Hydrofil Loading Capability

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

Research

JoVE Journal

Chemistry

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

Synthesis, Cellular Delivery and In vivo Application of Dendrimer-based pH Sensors

Synthesis, Cellular Delivery and In vivo Application of Dendrimer-based pH Sensors

Synthesis, Cellular Levering og<em&gt; In vivo</em&gt; Anvendelse af Dendrimer-baserede pH-sensorer

The development of  fluorescent indicators represented a revolution for life sciences. Genetically  encoded and synthetic fluorophores with sensing ...

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We demonstrate a method for the synthesis of multicomponent nanostructures consisting of CdS and CdSe with rod and tetrapod morphologies. A seeded ...

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Syntese af hypervalente iodonium Alkynyl Triflater om anvendelse af Generering Cyanocarbenes

The procedures described in this article involve the synthesis and isolation of hypervalent iodonium alkynyl triflates (HIATs) and their subsequent ...

Protocol for the Synthesis of Ortho-trifluoromethoxylated Aniline Derivatives

Protocol for the Synthesis of Ortho-trifluoromethoxylated Aniline Derivatives

Protokol til syntese af<em&gt; Ortho</em&gt; -trifluoromethoxylated anilinderivater

Molecules bearing trifluoromethoxy (OCF3) group often show desired pharmacological and biological properties. However, facile synthesis of ...

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Syntese og karakterisering af supramolekylære Colloids

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

Synthesis of Protein Bioconjugates via Cysteine-maleimide Chemistry

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Syntese af Protein biokonjugater<em&gt; via</em&gt; Cystein-maleimid Kemi

The chemical linking or bioconjugation of proteins to fluorescent dyes, drugs, polymers and other proteins has a broad range of applications, such as the ...

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Hydroquinon Based Syntese af guld nanorods

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

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

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

Kontrolleret Syntese og fluorescens Tracking af stærkt Uniform Poly (<em&gt; N</em&gt; -isopropylacrylamide) Mikrogeler

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

Facet-to-facet Linking of Shape-anisotropic Colloidal Cadmium Chalcogenide Nanostructures

Facet til facet sammenkædning af form-anisotrope kolloid Cadmium Chalcogenide nanostrukturer

Here, we describe a protocol that allows for shape-anisotropic cadmium chalcogenide nanocrystals (NCs), such as nanorods (NRs) and tetrapods (TPs), to be ...

Grafting Multiwalled Carbon Nanotubes with Polystyrene to Enable Self-Assembly and Anisotropic Patchiness

Podning Multiwalled kulstof-nanorør med polystyren aktivere samlesæt og anisotrope Patchiness

We demonstrate a straightforward protocol to graft pristine multiwalled carbon nanotubes (MWCNTs) with polystyrene (PS) chains at the sidewalls through a ...