Preparation of poly(N-isopropylacrylamide) grafted silica bead using hyperbranched polysiloxysilane as polymer brush and application to temperature-responsive HPLC

Seino, Makoto; Yokomachi, Kazutoshi; Hayakawa, Teruaki; Kikuchi, Ryohei; Kakimoto, Masa–aki; Horiuchi, Shin

doi:10.1016/j.polymer.2006.01.027

Cited by 48 publications

(35 citation statements)

References 38 publications

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“…Vinyl-terminated HBPS (P1) was obtained via the self-hydrosilylation of 1,5-divyl-1,1,3,5,5-pentamethyltrisiloxane (AB 2 monomer) in the presence of 0.1 mol% of platinum(0) 1,3-divinyl-1,1,3,3-tetramethyldisiloxane complex as a catalyst. 19 Hydroxyl-terminated HBPS (P2) was obtained from the reaction of the vinyl groups in P1 and 2-mercaptomethanol. The absence of a vinyl peak in the 1 H NMR spectrum of P2 suggested that the conversion from P1 to P2 was successful.…”

Section: Resultsmentioning

confidence: 99%

“…According to a previously reported procedure, 19 vinyl-terminated hyperbranched poly(siloxysilane) (P1) was prepared by hydrosilylation of 1,3,5,5-pentamethyl-1,5-divinyltrisiloxane (AB 2 type monomer) at 0 1C for 3 h in the presence of 0.1 mol% platinum(0) 1,3-divinyl-1,1,3,3-tetramethyldisiloxane complex in the bulk. The obtained P1 was a colorless viscous liquid (23.41 g, 47%).…”

Section: Vinyl-terminated Hbps (Hbps-vinyl) (P1)mentioning

confidence: 99%

“…The prepared silica (5 g), P3 (0.62 g) and 60 ml of hexane were mixed in a 100-ml vial on a roller mixer at room temperature for 48 h. 19 The product was filtered and washed overnight using a Soxhlet extractor. The sample was dried at 80 1C overnight under vacuum to give silica-HBPS-CTA.…”

Section: Trithiocarbonate-terminated Hbps (Hbps-cta) (P3)mentioning

confidence: 99%

“…We have also previously reported that the immobilized PNIPAM strongly adheres to silica beads via the hyperbranched polymer. 19 From these results, P3 was assumed to have been connected to the silica surface by the interaction between the siloxane segment of P3 and the silanol group at the silica surface.…”

Section: Immobilization Of Trithiocarbonate-terminated Hbps (Hbps-ctamentioning

confidence: 99%

“…19 The advantage of hyperbranched polymers in this type of immobilization is not only to maximize the number of the chain-transfer agent (CTA) molecules introduced onto a surface with a limited surface area but also to enable strong adhesion to a silica surface. We report the synthesis of PNIPAM-modified silica beads with a hyperbranched polymer and the results of preliminary cell-adhesion experiments.…”

Section: Introductionmentioning

confidence: 99%

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Poly(N-isopropylacrylamide)-modified silica beads with hyperbranched polysiloxysilane for three-dimensional cell cultivation

Park

Nabae

Surapati

et al. 2012

Polym J

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The immobilization of poly(N-isopropylacrylamide) (PNIPAM) onto the surface of silica beads via hyperbranched polysiloxysilane (HBPS) was studied to develop a new material for cell cultivation. HBPS terminated with a vinyl functional group was synthesized by self-polymerization of an AB 2 monomer. The terminal vinyl group was converted into a chain-transfer agent for reversible addition fragmentation chain transfer (RAFT) polymerization. The obtained HBPS was immobilized on the silica surface by mixing silica beads and HBPS in hexane. The graft polymerization of PNIPAM onto the silica surface was achieved using RAFT polymerization. The molecular weights of the grafted polymers obtained by cleavage from the surface of silica beads using NaOH aqueous solution were in the range of 6000-23 000 and the polydispersity index values were 1.4-1.6. The grafted silica beads have been tested for cell cultivation. Silica-HBPS-g-PNIPAM with a higher molecular weight (M n ) of PNIPAM (cleaved PNIPAM M n ¼ 14 800 and 23 700) showed a thermo-reversible phase transition at approximately 34 1C, and controlled cell adhesion and detachment was demonstrated with these beads.

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Section: Resultsmentioning

confidence: 99%

Section: Vinyl-terminated Hbps (Hbps-vinyl) (P1)mentioning

confidence: 99%

Section: Trithiocarbonate-terminated Hbps (Hbps-cta) (P3)mentioning

confidence: 99%

Section: Immobilization Of Trithiocarbonate-terminated Hbps (Hbps-ctamentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

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Poly(N-isopropylacrylamide)-modified silica beads with hyperbranched polysiloxysilane for three-dimensional cell cultivation

Park

Nabae

Surapati

et al. 2012

Polym J

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Preparation and characterization of temperature‐responsive chromatographic column containing poly(N‐isopropylacrylamide) and poly([2‐(methacryloyloxy)‐ ethyl]trimetylammonium chloride)

Dai

Chen

Liu

et al. 2011

J of Applied Polymer Sci

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This article described the preparation of temperature-responsive chromatographic column containing poly(N-isopropylacrylamide) and poly quaternary ammonium salt. Poly (N-isopropylacrylamide) and poly ([2-(methacryloyloxy)ethyl]trimetylammonium chloride) were synthesized and grafted to amino modified silica gel. The temperature responsive polymer grafted silica gel was characterized using Fourier transform infrared spectroscopy, thermoweight loss, and elemental analysis. The temperature responsive chromatographic column was used to analyze lactic acid and creatine phosphate disodium salt by controlling of the column temperature from 10 to 50 C. The mixture of lactic acid and creatine phosphate disodium salt was baseline separated at pH 6

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Separation of peptides with an aqueous mobile phase by temperature‐responsive chromatographic column

Liu¹,

Liang²,

Geng³

et al. 2012

J of Separation Science

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Peptide separation technology is significant and is still an analytical challenge in proteomic studies. We report a simple preparation method for poly(N-isopropylacrylamide) grafted silica through the copolymerization of N-isopropylacrylamide with acetyl moieties immobilized on the silica surfaces. Differential scanning calorimetry results indicated that the prepared silica exhibited a sharp phase transition at 35.03°C. Silica grafted with poly(N-isopropylacrylamide) was evaluated as a temperature-responsive chromatography medium for the separation of peptides using 0.2 M NaCl solution as a mobile phase. Results indicated that at 10°C, the peptides were not resolved, but baseline separation with prolonged retention time at 50°C was attained. Particularly, a mixture of four peptides was efficiently separated within 8 min. The theoretical plate number of every peptide was more than 2500, and the resolutions were more than 3.40. The increased selectivity of the temperature-responsive column resulted from the temperature-modulated hydrophobic interaction with peptides. The retention times of these peptides were related to their hydrophobicities. This protocol provided a reliable set of chromatographic tool usable across all research and development applications that required isolation and analysis of peptides. It may represent a step forward in the complex analysis of hydrophobic and other proteins.

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Preparation of poly(N-isopropylacrylamide) grafted silica bead using hyperbranched polysiloxysilane as polymer brush and application to temperature-responsive HPLC

Cited by 48 publications

References 38 publications

Poly(N-isopropylacrylamide)-modified silica beads with hyperbranched polysiloxysilane for three-dimensional cell cultivation

Poly(N-isopropylacrylamide)-modified silica beads with hyperbranched polysiloxysilane for three-dimensional cell cultivation

Preparation and characterization of temperature‐responsive chromatographic column containing poly(N‐isopropylacrylamide) and poly([2‐(methacryloyloxy)‐ ethyl]trimetylammonium chloride)

Separation of peptides with an aqueous mobile phase by temperature‐responsive chromatographic column

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