Diffusion ordered spectroscopy (DOSY) as a powerful tool for amphiphilic block copolymer characterization and for critical micelle concentration (CMC) determination

Bakkour, Youssef; Darcos, Vincent; Li, Suming; Coudane, Jean

doi:10.1039/c2py20054f

Cited by 81 publications

(73 citation statements)

References 27 publications

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“…SM5). This D value presents the same order of magnitude of those reported by Bakkur et al before and after the PLA–PEO–PLA copolymer reach the critical micellar concentration: D from 6 to 10 10 −11 m 2 s −1 …”

Section: Resultssupporting

confidence: 86%

“…The diffusion coefficient of D = 8.41 × 10 −11 m 2 s −1 in CDCl 3 for PEO (at 3.6 ppm) and PLA (at 5.2 ppm) blocks, and therefore, for the PLA 6 –PEO 8 –PLA 6 copolymer itself, was calculated (Supporting Information, Table SM1 presents D values of the other copolymers). Bakkur et al determined the diffusion coefficient of 5.6 10 −10 m 2 s −1 for a PLA–PEO–PLA copolymer (molar mass of 7700 g mol −1 and a PEO block of 6000 g mol −1 ) by the same technique, using the same solvent and temperature . This value is one order of magnitude higher than the value determined for PLA 6 –PEO 8 –PLA 6 copolymer in CDCl 3 (molar mass of 20,000 g mol −1 , and a PEO block of 8000 g mol −1 ), probably due to the molar mass differences between the copolymers.…”

Section: Resultsmentioning

confidence: 90%

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Amphiphilic polylactide‐poly(ethylene oxide)‐poly(propylene oxide) block copolymers: Self‐assembly behavior and cell affinity

Loiola

Farias

Portugal

et al. 2018

J. Polym. Sci. Part A: Polym. Chem.

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Polylactide (PLA) is a biodegradable polyester recognized for its potential use as a biomedical material. Poly(ethylene oxide) (PEO) and copolymers based on PEO and poly(propylene oxide) (PPO) are biocompatible polyethers widely applied in the biomedical field, particularly as macromolecular nonionic surfactants. In this work, PLA blocks were attached to the PEO and to the PEO and PPO‐based triblock copolymer PEO–PPO–PEO, through ring‐opening polymerization of racemic lactide (rac‐LA) to obtain the amphiphilic triblock PLA–PEO–PLA and pentablock PLA–PEO–PPO–PEO–PLA copolymers containing hydrophilic/hydrophobic blocks with variable block mass ratios. The copolymers were evaluated for chemical composition, molar mass, and thermal properties, and they were used to prepare self‐assemble aggregates in water from tetrahydrofuran polymer solutions. The combination of scattering light experiments and microscopy techniques revealed the spherical morphology of the aggregates with diameters around 180–200 nm, which comprises a hydrophobic PLA core and a hydrophilic polyether shell. The aggregates are nontoxic to human cervical cancer cell line — HeLa cells, as determined by MTS assay, and the aggregates are potential candidates to be applied in the encapsulation of hydrophobic compounds. © 2018 Wiley Periodicals, Inc. J. Polym. Sci., Part A: Polym. Chem. 2018, 56, 2203–2213

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Section: Resultssupporting

confidence: 86%

Section: Resultsmentioning

confidence: 90%

Amphiphilic polylactide‐poly(ethylene oxide)‐poly(propylene oxide) block copolymers: Self‐assembly behavior and cell affinity

Loiola

Farias

Portugal

et al. 2018

J. Polym. Sci. Part A: Polym. Chem.

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“…Despite the competing decomposition, turnover numbers (TON) of 872 (0.1 mol%) and 3500 (0.02 mol%) can be achieved (see SI). At 0.002 mol% (0.01 mg/mL of polymer) the reaction rate is significantly reduced because at this point the polymers do not form self-assembled structures, as confirmed by DOSY NMR spectroscopy (see SI), 32 and hence are unable to sequester the hydrophobic starting materials. At polymer concentrations of 10, 1.0 and 0.5 mg/mL turn over frequencies (TOF) (at 30% conversion) of 7.2, 22.2 and 32.4 min −1 respectively were achieved.…”

Section: Resultsmentioning

confidence: 96%

Catalytic Y-tailed amphiphilic homopolymers – aqueous nanoreactors for high activity, low loading SCS pincer catalysts

et al. 2013

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A new amphiphilic homopolymer bearing an SCS pincer palladium complex has been synthesized by reversible addition fragmentation chain transfer polymerization. The amphiphile has been shown to form spherical and worm-like micelles in water by cryogenic transmission electron microscopy and small angle neutron scattering. Segregation of reactive components within the palladium containing core results in increased catalytic activity of the pincer compound compared to small molecule analogues. This allows carbon-carbon bond forming reactions to be performed in water with reduced catalyst loadings and enhanced activity.

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“…The efficiency of click reaction was also evidenced by DOSY NMR, a powerful tool to characterize block copolymers . Figure shows the DOSY pattern of HPMC 8K ‐ b ‐PLA 2K copolymer in DMSO‐ d 6 .…”

Section: Resultsmentioning

confidence: 99%

Synthesis and Self‐Assembly of Amphiphilic Block Copolymers from Biobased Hydroxypropyl Methyl Cellulose and Poly(l‐lactide)

Wang

Caceres

et al. 2017

Macro Chemistry & Physics

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A series of well‐defined hydroxypropyl methyl cellulose‐block‐poly(l‐lactide) (HPMC‐b‐PLLA) diblock copolymers are synthesized via UV‐initiated thiol‐ene click reaction of thiol‐terminated HPMC with different block lengths and allyl‐terminated PLLA, using 2,2‐dimethoxy‐2‐phenylacetophenone as photocatalyst. The former is obtained by coupling the reducing aldehyde endgroup of short chain HPMC with the amine group of cysteamine, and the latter by ring‐opening polymerization of l‐lactide in the presence of allyl alcohol. Fourier transform infrared (FT‐IR), nuclear magnetic resonance (1H NMR), and diffusion ordered spectroscopy NMR confirm the successful coupling of both blocks. The molar mass of the resulting copolymers ranges from 7000 to 12 800 g mol−1 as determined by size exclusion chromatography. The copolymers are able to self‐assemble in aqueous medium, yielding micelles of 50–100 nm with core–shell structure as evidenced by dynamic light scattering, transmission electron microscopy, and 1H NMR. The critical micelle concentration of copolymers ranges from 0.12 to 0.15 mg mL−1. Last but not the least, the copolymers exhibit thermoresponsive behavior with a lower critical solution temperature around 80 °C.

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Diffusion ordered spectroscopy (DOSY) as a powerful tool for amphiphilic block copolymer characterization and for critical micelle concentration (CMC) determination

Cited by 81 publications

References 27 publications

Amphiphilic polylactide‐poly(ethylene oxide)‐poly(propylene oxide) block copolymers: Self‐assembly behavior and cell affinity

Amphiphilic polylactide‐poly(ethylene oxide)‐poly(propylene oxide) block copolymers: Self‐assembly behavior and cell affinity

Catalytic Y-tailed amphiphilic homopolymers – aqueous nanoreactors for high activity, low loading SCS pincer catalysts

Synthesis and Self‐Assembly of Amphiphilic Block Copolymers from Biobased Hydroxypropyl Methyl Cellulose and Poly(l‐lactide)

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