Name: synthesis of cyclic polymers and characterization of their diffusive motion in the melt state at the single molecule level
Uploaded: 2016-09-26T14:00:00
Description: Watch this Scientific Journal Video about Synthesis of Cyclic Polymers and Characterization of Their Diffusive Motion in the Melt State at the Single Molecule Level at JoVE.com

This work was supported by a Grant-in-Aid for Scientific Research No. 22750122 (S.H.), No. 26288099 (T.Y.), and No. 23350050 (Y.T.) of the Japan Society for the Promotion of Science. S.H. is grateful for The Kurata Memorial Hitachi Science and Technology Foundation. The research reported in this publication was supported by the King Abdullah University of Science and Technology (S.H.).

1. Syntese av Monofunksjonelt og bifunksjonelle Poly (THF) <ol><li> Monofunksjonelle poly (THF) <ol><li> Flamme tørke en 2-halset 100 ml rundbunnet kolbe. Støvsug og fylle flasken med nitrogen (3 sykluser). </li><li> Tilsett destillert tetrahydrofuran (THF) (50 ml) til kolben. Sett kolbe i et vannbad ved 20 ° C og likevekt temperaturen. </li><li> Legg metyltriflat (0,5 mmol) til kolben med en sprøyte. Og blandingen rørt i 5-10 minutter ved 20 ° C. </li><li> Legg N-fenyl pyrrolidin (4-6 ...

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De 4-armert og 8-formede polymerer ble fremstilt via ESA-CF-protokollen (figur 1), som er et kritisk trinn for syntesen. 12,24 Monofunksjonelt og bifunksjonelle lineære poly (THF) s med N -phenylpiperidinium endegrupper var syntetiseres i henhold til den foregående prosedyre. 11 ionebytter ble utført ved gjenutfelling av en acetonoppløsning av en polymer forløper med triflat counteranions i en vandig oppløsning inneholdende en overskuddsmengde av karboksylat. <p ...

Cyclic polymers are unique in that they do not have chain ends. They often exhibit unusual behaviors which is distinct from their linear counterpart, including increased thermal stability of polymer micelles by a linear-to-cyclic conversion,1,2 and spatial organization of DNA in bacterial cells by a loop formation.3 Topological interactions between the cyclic chains are believed to be the critical factor for such unusual behaviors.4,5 Therefore, characterizing the motion and relaxation of cyclic polymers under entangled conditions has been an important research topic in polymer science for decades.6
Cyclic polymer dynamics has been investigated using both synthetic and naturally occurring molecules by means of ensemble averaged experimental methods such as nuclear magnetic resonance (NMR), light scattering, and viscosity measurements.7-9 However, these studies often suffer from impurity molecules in the samples.10 Furthermore, spatiotemporal heterogeneities of the motion of individual molecules caused by inherent structural heterogeneity of entangled polymers are often hidden behind the ensemble averaging in these studies. In order to characterize molecular level dynamics of cyclic polymers, a synthesis method that provides high purity cyclic polymers and an experimental and analysis methods that allow for quantitative characterization of molecular motion at the single molecule level have to be developed. Here, we will show a method to synthesize high-purity cyclic and dicyclic poly(THF)s that incorporate a fluorophore unit using an electrostatic self-assembly and covalent fixation (ESA-CF) process11-13 and a method to analyze the motion of the individual fluorophore-incorporated polymer chains using a combination of mean-squared displacement (MSD) and cumulative distribution function (CDF) analyses.
A proper data processing has been shown to be essential for the accurate characterization of the diffusive motion. With an adequate MSD and CDF analyses, a multiple-mode diffusion of the cyclic and dicyclic polymers in the melt and semi-dilute solution of the linear polymer chains has been revealed,14-16 suggesting the significant effects of the topological states of the polymers on the diffusive motion of the chains under entangled conditions.17 While the experimental and analytical approaches to characterize the motion of the cyclic polymers are described in this protocol, the same method can be used to quantitatively characterize the diffusive motion in many other heterogeneous systems. The approach would be especially suitable when multiple diffusion components existing in the samples are to be analyzed.

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			<td height="21" style="height:21px;width:320px;">Materials</td>
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			<td height="21" style="height:21px;width:320px;">THF</td>
			<td style="width:240px;">Godo</td>
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			<td height="21" style="height:21px;width:320px;">Wakosil C-300</td>
			<td style="width:240px;">Wako Pure Chemical Industries</td>
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			<td height="21" style="height:21px;width:320px;">Acetone</td>
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			<td height="21" style="height:21px;width:320px;">Toluene</td>
			<td style="width:240px;">Godo</td>
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			<td height="21" style="height:21px;width:320px;">n-Hexane</td>
			<td style="width:240px;">Godo</td>
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			<td height="21" style="height:21px;width:320px;">CHCl3</td>
			<td style="width:240px;">Kanto Chemical</td>
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			<td height="21" style="height:21px;width:320px;">Bio-Beads S-X1</td>
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			<td height="21" style="height:21px;width:320px;">Methyl triflate</td>
			<td style="width:240px;">Nacalai Tesque</td>
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			<td height="21" style="height:21px;width:320px;">Triflic anhydride</td>
			<td style="width:240px;">Nacalai Tesque</td>
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			<td height="21" style="height:21px;width:320px;">Potassium Hydroxide</td>
			<td style="width:240px;">Wako Pure Chemical Industries</td>
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			<td height="21" style="height:21px;width:320px;">Ethanol</td>
			<td style="width:240px;">Wako Pure Chemical Industries</td>
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			<td height="21" style="height:21px;width:320px;">Poly(tetrahydrofuran)</td>
			<td style="width:240px;">Aldrich</td>
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			<td height="21" style="height:21px;width:320px;">Chloroform</td>
			<td style="width:240px;">Wako Pure Chemical Industries</td>
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			<td height="21" style="height:21px;width:320px;">Immersion oil</td>
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			<td height="21" style="height:21px;width:320px;">Equipment</td>
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			<td height="21" style="height:21px;width:320px;">2-Neck 100-mL round-bottom flask</td>
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			<td height="21" style="height:21px;width:320px;">Filter paper</td>
			<td style="width:240px;">Whatman</td>
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			<td height="21" style="height:21px;width:320px;">Reflux condenser</td>
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			<td height="21" style="height:21px;width:320px;">Water bath</td>
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			<td height="21" style="height:21px;width:320px;">Magnetic stirrer</td>
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			<td height="21" style="height:21px;width:320px;">Rotary evaporator</td>
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			<td height="21" style="height:21px;width:320px;">Microscope cover slips (24 x 24 mm, No. 1)</td>
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			<td height="21" style="height:21px;width:320px;">Staining jar</td>
			<td style="width:240px;">AS ONE Corporation</td>
			<td style="width:119px;">1-7934-01</td>
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			<td height="21" style="height:21px;width:320px;">Ultrasonic cleaner</td>
			<td style="width:240px;">VWR International&#160;</td>
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		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:320px;">Inverted microscope</td>
			<td style="width:240px;">Olympus</td>
			<td style="width:119px;">IX71</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:320px;">Ar-Kr ion laser</td>
			<td style="width:240px;">Coherent</td>
			<td style="width:119px;">Innova 70C</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:320px;">Berek compensator</td>
			<td style="width:240px;">Newport</td>
			<td align="right" style="width:119px;">5540</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:320px;">Excitation filter</td>
			<td style="width:240px;">Semrock</td>
			<td style="width:119px;">LL01-488-12.5</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:320px;">Dichloric mirror</td>
			<td style="width:240px;">Omega optical</td>
			<td style="width:119px;">500DRLP</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:320px;">Emission filter</td>
			<td style="width:240px;">Semrock</td>
			<td style="width:119px;">BLP01-488R-25</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:320px;">Lens and mirror</td>
			<td style="width:240px;">Thorlabs</td>
			<td style="width:119px;"></td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:320px;">EM-CCD camera</td>
			<td style="width:240px;">Andor Technology</td>
			<td style="width:119px;">iXon</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:320px;">Objective lens (x100, N.A. = 1.3)</td>
			<td style="width:240px;">Olympus</td>
			<td style="width:119px;">UPLFLN 100XOP</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:320px;">Objective heater</td>
			<td style="width:240px;">Bioptechs</td>
			<td style="width:119px;"></td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:320px;">Preparative GPC</td>
			<td style="width:240px;">Japan Analytical Industry</td>
			<td style="width:119px;">LC-908</td>
			<td></td>
		</tr>
	</tbody>
</table>

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.

Den perylen diimid-innlemmet fire-armet stjerne og 8 formet dicyklisk poly (THF) s ble syntetisert ved anvendelse av den elektrostatiske selv-sammenstillingen og kovalent fiksering (ESA-CF) Fremgangsmåte (figur 1, figur 2). Time-lapse single-molekyl fluorescens bildene ble målt for fire-armet (figur 3a) og 8-formet (figur 3b) polymerer. De time-lapse fluorescens bilder (figur 3) viser romlig isolerte l...

Watch this Scientific Journal Video about Synthesis of Cyclic Polymers and Characterization of Their Diffusive Motion in the Melt State at the Single Molecule Level at JoVE.com

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

En protokoll for syntese og karakterisering av diffusive bevegelse av cykliske polymerer på enkelt molekyl nivå er presentert.

Syntese av Sykliske Polymers og karakterisering av deres diffusiv Motion i smeltet tilstand ved enkelt molekyl nivå

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 ...

Research

JoVE Journal

Chemistry

Isolation and Chemical Characterization of Lipid A from Gram-negative Bacteria

Isolation and Chemical Characterization of Lipid A fra Gram-negative bakterier

Lipopolysaccharide (LPS) is the major cell surface molecule of gram-negative bacteria, deposited on the outer leaflet of the outer membrane bilayer. LPS ...

Synthesis of Hypervalent Iodonium Alkynyl Triflates for the Application of Generating Cyanocarbenes

Syntese av Hypervalent jod Alkynyl Triflates for anvendelse av Generering Cyanocarbenes

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

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

Split-and-pool Syntese og karakterisering av Peptide Tertiær Amide Library

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

Amide Coupling Reaction for the Synthesis of Bispyridine-based Ligands and Their Complexation to Platinum as Dinuclear Anticancer Agents

Amid koplingsreaksjon for syntese av Bispyridine-baserte Ligander og deres kompleks til Platinum som bisykliske legemidler mot kreft

Amide coupling reactions can be used to synthesize bispyridine-based ligands for use as bridging linkers in multinuclear platinum anticancer drugs. ...

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

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

The Synthesis, Characterization og reaktivitet av en serie av Ruthenium<em&gt; N</em&gt; -triphos<sup&gt; Ph</sup&gt; Komplekser

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

Syntese, karakterisering og funksjon av Hybrid Au / CDer og Au / ZnS Kjerne / Shell Nanopartikler

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

Protocol for the Synthesis of Ortho-trifluoromethoxylated Aniline Derivatives

Protocol for the Synthesis of Ortho-trifluoromethoxylated Aniline Derivatives

Protokoll for syntese av<em&gt; Ortho</em&gt; -trifluoromethoxylated anilinderivater

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

Synthesis of Protein Bioconjugates via Cysteine-maleimide Chemistry

Synthesis of Protein Bioconjugates via Cysteine-maleimide Chemistry

Syntese av Protein Bioconjugates<em&gt; via</em&gt; Cystein-maleimide kjemi

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

Insights into the Interactions of Amino Acids and Peptides with Inorganic Materials Using Single-Molecule Force Spectroscopy

Innsikt i de Samhandling av aminosyrer og peptider med uorganiske materialer Bruke Single-Molecule Force spektroskopi

The interactions between proteins or peptides and inorganic materials lead to several interesting processes. For example, combining proteins with minerals ...

Using Cyclic Voltammetry, UV-Vis-NIR, and EPR Spectroelectrochemistry to Analyze Organic Compounds

Bruke sykliske Voltammetry, UV-Vis-NIR og EPR Spectroelectrochemistry å analysere organiske forbindelser

Cyclic voltammetry (CV) is a technique used in the analysis of organic compounds. When this technique is combined with electron paramagnetic resonance ...