Name: synthesis of cyclic polymers and characterization of their diffusive motion in the melt state at the single molecule level
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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. Sintesi di monofunzionale e bifunzionale Poly (THF) <ol><li> Poly monofunzionali (THF) <ol><li> Fiamma asciugare un pallone a 2-collo da 100 ml. Aspirare e riempire il pallone con azoto (3 cicli). </li><li> Aggiungere tetraidrofurano distillato (THF) (50 ml) al pallone. Mettere il pallone in un bagno di acqua a 20 ° C ed equilibrare la temperatura. </li><li> Aggiungere triflato metile (0,5 mmol) al pallone da una siringa. Mescolare la miscela per 5-10 minuti a 20 ° C. </li><li> Aggiungere N</...

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	<li>Honda, S., Yamamoto, T., Tezuka, Y. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Topology-Directed+Control+on+Thermal+Stability:+Micelles+Formed+from+Linear+and+Cyclized+Amphiphilic+Block+Copolymers.">Topology-Directed Control on Thermal Stability: Micelles Formed from Linear and Cyclized Amphiphilic Block Copolymers.</a> J. Am. Chem. Soc. 132 (30), 10251-10253 (2010).</li><li>Honda, S., Yamamoto, T., Tezuka, Y. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Tuneable+enhancement+of+the+salt+and+thermal+stability+of+polymeric+micelles+by+cyclized+amphiphiles.">Tuneable enhancement of the salt and thermal stability of polymeric micelles by cyclized amphiphiles.</a> Nat. Commun. 4, (2013).</li><li>Jun, S., Mulder, B. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Entropy-driven+spatial+organization+of+highly+confined+polymers:+Lessons+for+the+bacterial+chromosome.">Entropy-driven spatial organization of highly confined polymers: Lessons for the bacterial chromosome.</a> Proc. Natl. Acad. Sci. U. S. A. 103 (33), 12388-12393 (2006).</li><li>McLeish, T. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Polymers+without+beginning+or+end.">Polymers without beginning or end.</a> Science. 297 (5589), 2005-2006 (2002).</li><li>McLeish, T. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Polymer+dynamics:+Floored+by+the+rings.">Polymer dynamics: Floored by the rings.</a> Nat. Mater. 7 (12), 933-935 (2008).</li><li>Roovers, J., Tezuka, Y. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Topological Polymer Chemistry: Progress of Cyclic Polymers in Syntheses, Properties and Functions. , 137-156 (2013).</li><li>Klein, J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Evidence+for+reptation+in+an+entangled+polymer+melt.">Evidence for reptation in an entangled polymer melt.</a> Nature. 271 (5641), 143-145 (1978).</li><li>Leger, L., Hervet, H., Rondelez, F. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Reptation+in+entangled+polymer-solutions+by+forced+rayleigh+light-scattering.">Reptation in entangled polymer-solutions by forced rayleigh light-scattering.</a> Macromolecules. 14 (6), 1732-1738 (1981).</li><li>von Meerwall, E. D., Amis, E. J., Ferry, J. D. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Self-diffusion+in+solutions+of+polystyrene+in+tetrahydrofuran+-+comparison+of+concentration+dependences+of+the+diffusion-coefficients+of+polymers,+and+a+ternary+probe+component.">Self-diffusion in solutions of polystyrene in tetrahydrofuran - comparison of concentration dependences of the diffusion-coefficients of polymers, and a ternary probe component.</a> Macromolecules. 18 (2), 260-266 (1985).</li><li>Kapnistos, M., 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=Unexpected+power-law+stress+relaxation+of+entangled+ring+polymers.">Unexpected power-law stress relaxation of entangled ring polymers.</a> Nat. Mater. 7 (12), 997-1002 (2008).</li><li>Adachi, K., Takasugi, H., Tezuka, Y. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Telechelics+having+unstrained+cyclic+ammonium+salt+groups+for+electrostatic+polymer+self-assembly+and+ring-emitting+covalent+fixation.">Telechelics having unstrained cyclic ammonium salt groups for electrostatic polymer self-assembly and ring-emitting covalent fixation.</a> Macromolecules. 39 (17), 5585-5588 (2006).</li><li>Oike, H., Imaizumi, H., Mouri, T., Yoshioka, Y., Uchibori, A., Tezuka, Y. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Designing+unusual+polymer+topologies+by+electrostatic+self-assembly+and+covalent+fixation.">Designing unusual polymer topologies by electrostatic self-assembly and covalent fixation.</a> J. Am. Chem. Soc. 122 (40), 9592-9599 (2000).</li><li>Yamamoto, T., Tezuka, Y. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Topological+polymer+chemistry:+a+cyclic+approach+toward+novel+polymer+properties+and+functions.">Topological polymer chemistry: a cyclic approach toward novel polymer properties and functions.</a> Polym. Chem. 2 (9), 1930-1941 (2011).</li><li>Habuchi, S., Fujiwara, S., Yamamoto, T., Tezuka, Y. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Single-molecule+imaging+reveals+topological+isomer-dependent+diffusion+by+4-armed+star+and+dicyclic+8-shaped+polymers.">Single-molecule imaging reveals topological isomer-dependent diffusion by 4-armed star and dicyclic 8-shaped polymers.</a> Polym. Chem. 6 (22), 4109-4115 (2015).</li><li>Habuchi, S., Fujiwara, S., Yamamoto, T., Vacha, M., Tezuka, Y. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Single-Molecule+Study+on+Polymer+Diffusion+in+a+Melt+State:+Effect+of+Chain+Topology.">Single-Molecule Study on Polymer Diffusion in a Melt State: Effect of Chain Topology.</a> Anal. Chem. 85 (15), 7369-7376 (2013).</li><li>Habuchi, S., Satoh, N., Yamamoto, T., Tezuka, Y., Vacha, M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Multimode+Diffusion+of+Ring+Polymer+Molecules+Revealed+by+a+Single-Molecule+Study.">Multimode Diffusion of Ring Polymer Molecules Revealed by a Single-Molecule Study.</a> Angew. Chem. Int. Ed. 49 (8), 1418-1421 (2010).</li><li>Habuchi, S., Tezuka, Y. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Topological Polymer Chemistry: Progress of Cyclic Polymers in Syntheses, Properties and Functions. , 265-290 (2013).</li><li>Fernandez, P., Bayona, J. M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Use+of+off-line+gel-remeation+chromatography+normal-phase+liquid-chromatography+fro+the+determination+of+polycyclic+aromatic-compounds+in+environmental-samples+and+standard+reference+materials+(air+particulate+matter+and+marine+sediment).">Use of off-line gel-remeation chromatography normal-phase liquid-chromatography fro the determination of polycyclic aromatic-compounds in environmental-samples and standard reference materials (air particulate matter and marine sediment).</a> J. Chromatogr. 625 (2), 141-149 (1992).</li><li>Biesenberger, J. A., Tan, M., Duvdevan, I., Maurer, T. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Recycle+gel+permeation+chromatography.+1.+recycle+principle+and+design.">Recycle gel permeation chromatography. 1. recycle principle and design.</a> J. Polym. Sci. Pol. Lett. 9 (5), 353 (1971).</li><li>Kusumi, A., Sako, Y., Yamamoto, M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Confined+lateral+diffusion+of+membrane-receptors+as+studied+by+single-particle+tracking+(nanovid+microscopy)+-+effects+of+calcium-induced+differentiation+in+cultured+epithelial-cells.">Confined lateral diffusion of membrane-receptors as studied by single-particle tracking (nanovid microscopy) - effects of calcium-induced differentiation in cultured epithelial-cells.</a> Biophys. J. 65 (5), 2021-2040 (1993).</li><li>Schutz, G. J., Schindler, H., Schmidt, T. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Single-molecule+microscopy+on+model+membranes+reveals+anomalous+diffusion.">Single-molecule microscopy on model membranes reveals anomalous diffusion.</a> Biophys. J. 73 (2), 1073-1080 (1997).</li><li>Vrljic, M., Nishimura, S. Y., Brasselet, S., Moerner, W. E., McConnell, H. M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Translational+diffusion+of+individual+class+II+MHC+membrane+proteins+in+cells.">Translational diffusion of individual class II MHC membrane proteins in cells.</a> Biophys. J. 83 (5), 2681-2692 (2002).</li><li>Margineanu, A., 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=Photophysics+of+a+water-soluble+rylene+dye:+Comparison+with+other+fluorescent+molecules+for+biological+applications.">Photophysics of a water-soluble rylene dye: Comparison with other fluorescent molecules for biological applications.</a> J. Phys. Chem. B. 108 (32), 12242-12251 (2004).</li><li>Tezuka, Y., Oike, H. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Self-assembly+and+covalent+fixation+for+topological+polymer+chemistry.">Self-assembly and covalent fixation for topological polymer chemistry.</a> Macromol. Rapid Commun. 22 (13), 1017-1029 (2001).</li><li>Deres, A., 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=The+Origin+of+Heterogeneity+of+Polymer+Dynamics+near+the+Glass+Temperature+As+Probed+by+Defocused+Imaging.">The Origin of Heterogeneity of Polymer Dynamics near the Glass Temperature As Probed by Defocused Imaging.</a> Macromolecules. 44 (24), 9703-9709 (2011).</li><li>Flier, B. M. I., 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=Heterogeneous+Diffusion+in+Thin+Polymer+Films+As+Observed+by+High-Temperature+Single-Molecule+Fluorescence+Microscopy.">Heterogeneous Diffusion in Thin Polymer Films As Observed by High-Temperature Single-Molecule Fluorescence Microscopy.</a> J. Am. Chem. Soc. 134 (1), 480-488 (2012).</li><li>Habuchi, S., Oba, T., Vacha, M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Multi-beam+single-molecule+defocused+fluorescence+imaging+reveals+local+anisotropic+nature+of+polymer+thin+films.">Multi-beam single-molecule defocused fluorescence imaging reveals local anisotropic nature of polymer thin films.</a> Phys. Chem. Chem. Phys. 13 (15), 6970-6976 (2011).</li><li>Zettl, U., 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=Self-Diffusion+and+Cooperative+Diffusion+in+Semidilute+Polymer+Solutions+As+Measured+by+Fluorescence+Correlation+Spectroscopy.">Self-Diffusion and Cooperative Diffusion in Semidilute Polymer Solutions As Measured by Fluorescence Correlation Spectroscopy.</a> Macromolecules. 42 (24), 9537-9547 (2009).</li><li>Kirstein, J., Platschek, B., Jung, C., Brown, R., Bein, T., Brauchle, C. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Exploration+of+nanostructured+channel+systems+with+single-molecule+probes.">Exploration of nanostructured channel systems with single-molecule probes.</a> Nat. Mater. 6 (4), 303-310 (2007).</li></ol>

I polimeri 4-armati e sagomati-8 sono state preparate tramite il protocollo ESA-CF (figura 1), che è un passaggio fondamentale per la sintesi. 12,24 monofunzionale e bifunzionale poli lineare (THF) s con N terminali -phenylpiperidinium erano sintetizzato secondo la procedura precedente. 11 lo scambio ionico è stata effettuata da riprecipitazione di una soluzione in acetone di un precursore polimero con counteranions triflato in una soluzione acquosa contenente un eccesso...

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>
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			<td height="21" style="height:21px;width:320px;">n-Hexane</td>
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			<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>
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			<td height="21" style="height:21px;width:320px;">Triflic anhydride</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;">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.

Il perylene diimide-incorporato stella 4 armata e forma-8 poli dicyclic (THF) s sono stati sintetizzati utilizzando il elettrostatica auto-assemblaggio e covalente fissaggio (ESA-CF) di processo (Figura 1, Figura 2). Immagini di fluorescenza singola molecola time-lapse sono stati misurati per il 4-armata (Figura 3a) e 8 a forma di polimeri (figura 3b). Le immagini time-lapse di fluorescenza (Figura 3) mo...

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

Un protocollo per la sintesi e la caratterizzazione di moto diffusivo di polimeri ciclici a livello di singola molecola è presentato.

Sintesi di ciclici polimeri e caratterizzazione di loro moto diffusivo allo stato fuso alla molecola Piano unico

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

Isolamento e Caratterizzazione chimica del lipide A da batteri Gram-negativi

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

Ricerca

Chimica

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

Sintesi di hypervalent iodonio Alchinile triflati per l&#39;applicazione di Generazione 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-e-pool Sintesi e caratterizzazione di peptidi Terziario Ammide Biblioteca

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

Ammide Accoppiamento di reazione per la sintesi di leganti a base di Bispyridine e il loro Complessazione di platino come diciclici agenti antitumorali

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

La sintesi, caratterizzazione e reattività di una serie di rutenio<em&gt; N</em&gt; -triphos<sup&gt; Ph</sup&gt; Complessi

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

Sintesi, Caratterizzazione, e funzionalizzazione di ibrida UA / CdS e Au / ZnS core / shell nanoparticelle

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

Protocollo per la sintesi di<em&gt; Ortho</em&gt; Derivati ​​all&#39;anilina -trifluoromethoxylated

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

Sintesi di proteine ​​bioconiugati<em&gt; via</em&gt; Chimica cisteina-maleimmide

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

Intuizioni le interazioni di aminoacidi e peptidi con materiali inorganici Uso singola molecola Forza Spettroscopia

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

Mediante voltammetria ciclica, UV-Vis-NIR ed EPR Spectroelectrochemistry per analizzare composti organici

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