pNIPAm containing 5 mol% 2-acrylamido-2-methyl-1-propanesulfonic acid (AMPS) and 1 mol% Acrylic Acid (AAc) were synthesized in a precipitation polymerization reaction as described previously [44 , 51 (link)]. Briefly, 794.1 mg of NIPAm (Thermo Fisher Scientific), 28.5 mg of N,N’-methylenebisacrylamide (MBA, Sigma-Aldrich), and 76.5 mg of AMPS (Sigma-Aldrich) were added to 70 °C MilliQ water (18.2 MΩ·cm resistivity, Millipore) that had been refluxed under nitrogen for 30 minutes. 5 μL of AAc (99.5%, Thermo Fisher Scientific) and 164 μL of sodium dodecyl sulfate (SDS, 10% w/v, Sigma-Aldrich) were added to the solution, and polymerization was initiated by the addition of 33.7 mg of potassium persulfate (Sigma-Aldrich). For fluorescent nanoparticle synthesis, 1 mol% fluorescein o-acrylate was pre-dissolved in 3% DMSO and then added to the shell polymer mixture and allowed to equilibrate for 30 minutes before the initiation of polymerization. After 5 hours, the reaction was cooled to room temperature and then dialyzed against MilliQ water for 7 days using a 15,000 MWCO dialysis membrane (Spectra-Por). Following dialysis, the purified poly(NIPAm-MBA-AMPS-AAc) nanoparticles were lyophilized and stored at room temperature.
Nipam
Manufactured by Thermo Fisher Scientific
NIPAM is a laboratory reagent used in various analytical and experimental procedures. It functions as a monomer for the synthesis of polymers, which can serve as model systems or have other applications in scientific research. The core purpose of NIPAM is to provide a chemical building block for researchers to utilize in their investigations, without making claims about its intended use or performance.
Automatically generated - may contain errors
Lab products found in correlation
Penicillin, by Thermo Fisher Scientific (2 mentions)
Streptomycin, by Thermo Fisher Scientific (2 mentions)
Rpmi 1640 medium, by Thermo Fisher Scientific (2 mentions)
Potassium persulfate, by Merck Group (1 mentions)
Sodium dodecyl sulfate (sds), by Merck Group (1 mentions)
N n methylenebis acrylamide mba, by Merck Group (1 mentions)
Milli q water, by Merck Group (1 mentions)
Chloroauric acid, by Merck Group (1 mentions)
Fetal bovine serum (fbs), by Sartorius (1 mentions)
Deionized water 18.2 mω, by Merck Group (1 mentions)
Molecular sieves, by Merck Group (1 mentions)
Nh4oh, by Thermo Fisher Scientific (1 mentions)
N n dimethylformamide (dmf), by Thermo Fisher Scientific (1 mentions)
Ddmat, by Merck Group (1 mentions)
1 3 propanesultone, by Merck Group (1 mentions)
Ethanol, by Avantor (1 mentions)
Sodium hydroxide (naoh), by Avantor (1 mentions)
Ammonia solution 28 30, by Merck Group (1 mentions)
3 methacryloxypropyltrimethoxysilane, by Merck Group (1 mentions)
N n methylenebisacrylamide, by Merck Group (1 mentions)
9 protocols using nipam
1
Synthesis of Fluorescent pNIPAm Nanoparticles
2
Synthesis and Characterization of PNIPAM-Based Nanoparticles
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Tetrahydrofuran (THF) and 1,4-dioxane were obtained from Innovative Technology Inc. Ethylene glycol (99%) was purchased from Aladdin (Shanghai, People’s Republic of China). 2-(Dodecylthiocarbonothioylthio)-2-methylpropionic acid N-hydroxysuccinimide ester (DIMA),2,2′-azobis (isobutyronitrile) (AIBN; 95%) and Am (99%) were obtained from Aladdin and recrystallized from methanol before use. NIPAM (99%) was provided by Thermo Fisher Scientific (Shanghai, People’s Republic of China) and recrystallized from hexane twice before use. 3-(4,5-Dime-thylthiazol-2-yl)-2,5-diphenyltetrazolium bromide (MTT), poly(vinyl pyrrolidone) (PVP, molecular weight =55,000), chloroauric acid (HAuCl4·3H2O, 99.99%) and 4,6-diamidimo-2-phenylindole were all bought from Sigma-Aldrich (Boston, MA, USA). Sodium hyaluronate (HA, molecular weight =100 kDa) and HAase were provided by Sangon Biological Engineering Technology Co., Ltd (Shanghai, People’s Republic of China). RPMI 1640 medium, streptomycin and penicillin were obtained from Thermo Fisher Scientific (Waltham, MA, USA). Fetal bovine serum was purchased from Biological Industries (Kibbutz Beit Haemek, Israel).
Deionized water (18.2 MΩ; EMD Millipore, Billerica, MA, USA) was utilized in all experiments.
Deionized water (18.2 MΩ; EMD Millipore, Billerica, MA, USA) was utilized in all experiments.
3
Synthesis of PNIPAM-Coated Nanoparticles
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All
chemicals were purchased from Sigma-Aldrich
and used as received unless stated otherwise. H2O2 (30%) was from ACROS, N-isopropyl acrylamide (NIPAM)
and NH4OH (28–30%) from Fischer, H2SO4 (98%) and EtOH (99.5%) from SOLVECO, and ω-mercaptoundecyl
bromoisobutyrate from ProChimia. Water was of ASTM research grade
type 1 ultrafiltered water (Milli-Q water). Buffers were based on
phosphate-buffered saline (PBS) tablets (0.01 M phosphate, 0.13 M
NaCl, pH 7.4).
Monomer NIPAM (99%) was recrystallized from hexane
at 85 °C and stored under N2. The polymerization solvent
MeOH was dried over 3 Å molecular sieves (Merck) and then stored
under N2.
chemicals were purchased from Sigma-Aldrich
and used as received unless stated otherwise. H2O2 (30%) was from ACROS, N-isopropyl acrylamide (NIPAM)
and NH4OH (28–30%) from Fischer, H2SO4 (98%) and EtOH (99.5%) from SOLVECO, and ω-mercaptoundecyl
bromoisobutyrate from ProChimia. Water was of ASTM research grade
type 1 ultrafiltered water (Milli-Q water). Buffers were based on
phosphate-buffered saline (PBS) tablets (0.01 M phosphate, 0.13 M
NaCl, pH 7.4).
Monomer NIPAM (99%) was recrystallized from hexane
at 85 °C and stored under N2. The polymerization solvent
MeOH was dried over 3 Å molecular sieves (Merck) and then stored
under N2.
4
Synthesis of Thermoresponsive Ionic Liquid Polymers
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The chemical reagents including chloromethylstyrene (CMS, >97%, Alfa), N-methylimidazole (98%, Tianjin Yichuangcheng Chemical Company), sodium tetrafluoroborate (NaBF4, >99%, Tianjin Chemical Company) and hydroquinone (>98%, Tianjin Chemical Company) were used as received. The monomer of N-isopropylacrylamide (NIPAM, >99%, Acros Organics) was purified by recrystallization in an acetone/n-hexane mixture (50/50 by volume). The ionic liquid monomer of 1-(4-vinylbenzyl)-3-methylimidazolium tetrafluoroborate ([VBMI][BF4], seeing 1H NMR spectrum in Fig. S1† ) was synthesized initially by nucleophilic substitution reaction of CMS with N-methylimidazole and then anion exchange reaction with sodium tetrafluoroborate.8 (link) The initiator of 2,2′-azobis(isobutyronitrile) (AIBN, >98%, Tianjin Ruijinte Chemical Reagent) was recrystallized from ethanol prior to use. S-1-Dodecyl-S′-(α,α′-dimethyl-α′′-acetic acid)trithiocarbonate (DDMAT) was synthesized as discussed elsewhere.55 (link) All the other reagents were analytic grade and used as received. Deionized water was used in the present study.
5
Synthesis of Functional Polymers
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2-Cyano-2-propyl dodecyl trithiocarbonate
(2-CPDT, Strem, >97%), HPLC grade N,N-dimethylformamide (DMF, Alfa Aeser, >99.7%), CDCl3 (Acros,
>99.8%), and N,N′-methylenebis(acrylamide)
(MBAM, Sigma-Aldrich, 99%) were used as received. Vinyl monomers N,N-dimethylacrylamide (DMA, Sigma-Aldrich,
99%), N-(3-methoxypropyl)acrylamide (MPAM, Sigma-Aldrich,
95%), and 4-acryloylmorpholine (MORPH, TCI, >98%) were filtered
with
basic alumina before use. Vinyl monomer N-isopropylacrylamide
(NIPAM, Acros, stabilized >99%) was recrystallized from hexanes
(Fisher,
certified ACS >99.9%) and dried under vacuum. MVM 1,4-diacrylylpiperazine
(PIPBAM, CarboSynth, >98.5%) was dissolved in DMF and filtered
with
diatomaceous earth before use. 2,2′-Azobis(2-methylpropionitrile)
(AIBN, Sigma, >98%) was recrystallized from methanol (MeOH, Fisher,
HPLC grade > 99.9%) and dried under vacuum before use.
(2-CPDT, Strem, >97%), HPLC grade N,N-dimethylformamide (DMF, Alfa Aeser, >99.7%), CDCl3 (Acros,
>99.8%), and N,N′-methylenebis(acrylamide)
(MBAM, Sigma-Aldrich, 99%) were used as received. Vinyl monomers N,N-dimethylacrylamide (DMA, Sigma-Aldrich,
99%), N-(3-methoxypropyl)acrylamide (MPAM, Sigma-Aldrich,
95%), and 4-acryloylmorpholine (MORPH, TCI, >98%) were filtered
with
basic alumina before use. Vinyl monomer N-isopropylacrylamide
(NIPAM, Acros, stabilized >99%) was recrystallized from hexanes
(Fisher,
certified ACS >99.9%) and dried under vacuum. MVM 1,4-diacrylylpiperazine
(PIPBAM, CarboSynth, >98.5%) was dissolved in DMF and filtered
with
diatomaceous earth before use. 2,2′-Azobis(2-methylpropionitrile)
(AIBN, Sigma, >98%) was recrystallized from methanol (MeOH, Fisher,
HPLC grade > 99.9%) and dried under vacuum before use.
6
Synthesis of NIPAM-based Polymers
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Azobisisobutyronitrile (AIBN, Merck, 98%) and N-isopropylacrylamide (NIPAM, Acros, 99%) purification was performed via re-crystallization from methanol and n-hexane respectively. 4-Vinylpyridine (4-VP, Sigma-Aldrich, 95%) was refined through vacuum distillation. 2-(Dodecylthiocarbonothioylthio)-2-methylpropionic acid (DDMAT, Sigma-Aldrich, 98% HPLC) make dried under vacuum, preliminary to use. 1,4-Dioxane (Fluka, 99.5%) dried initially using CaCl2 and then by refluxing in the presence of sodium wire. 1,3-Propanesultone (Sigma-Aldrich, 98%) was used as obtained.
7
Synthesis of PNIPAm-based Hydrogels
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N-Isopropylacrylamide (NIPAm, Acros Organics 99%) was
recrystallized from hexane before use.
N,N’-Methylenebis(acrylamide) (BIS,
Sigma-Aldrich, 99%) and 2,2′-Azobis(2-methylpropionamidine)-dihydro-chloride
(AMPA, Sigma-Aldrich, 97%) and hexadecyl(trimethyl)ammonium bromide (CTAB,
Sigma-Aldrich 98%) were used as received.
recrystallized from hexane before use.
N,N’-Methylenebis(acrylamide) (BIS,
Sigma-Aldrich, 99%) and 2,2′-Azobis(2-methylpropionamidine)-dihydro-chloride
(AMPA, Sigma-Aldrich, 97%) and hexadecyl(trimethyl)ammonium bromide (CTAB,
Sigma-Aldrich 98%) were used as received.
8
Versatile Polymer Nanoparticle Synthesis
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Ethanol and sodium hydroxide were purchased from VWR. NIPAM was obtained from Acros Organics. NtBAM, DAAM, N,N'-methylenebisacrylamide (BIS) and 3-Methacryloxypropyltrimethoxysilane (MPS) were obtained from Sigma-Aldrich. Potassium persulfate (KPS), sodium dodecyl sulfate (SDS), tetraethyl orthosilicate (TEOS), and ammonia solution (28-30%) were purchased from Merck.
9
Synthesis and Characterization of PNIPAm
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Three different PNIPAm samples were used for our experiments. These include a commercial PNIPAm from Sigma-Aldrich [cat # 535311-10G]. Using light scattering and size exclusion chromatography, we estimate absolute molecular weight M w and poly dispersity (PDI) to be M w (SLS) = 293 kDa, M w (GPC) = 309 kDa, and PDI = 2.69. N l value is estimated using the equation N l = (M w /PDI)/M 0 , where M 0 is the NIPAm formula weight. This corresponds to N l = 962 (sample PNIPAm-963). Furthermore, we have prepared two PNIPAm samples by RAFT polymerization giving chain lengths bracketing that corresponding to N l B 100l p to better correlate all-atom simulations and experimental observations (details will be described in the next section).
Before starting the polymerization procedure, N-isopropyl acrylamide (NIPAm, Acros, 99%) was recrystallized three times in series by adding a benzene solution (B30% NIPAm by weight) to an approximate 12-fold excess of pentane at room temperature. 4,4 0 -Azobis(4-cyanovaleric acid) (ACVA, Aldrich, Z98%,), 4-((((2-carboxyethyl)thio)carbonothioyl)thio)-4-cyanopentanoic acid (BM1433, 495%, boron molecular) and all other materials were purchased from commercial sources and utilized as received.
Before starting the polymerization procedure, N-isopropyl acrylamide (NIPAm, Acros, 99%) was recrystallized three times in series by adding a benzene solution (B30% NIPAm by weight) to an approximate 12-fold excess of pentane at room temperature. 4,4 0 -Azobis(4-cyanovaleric acid) (ACVA, Aldrich, Z98%,), 4-((((2-carboxyethyl)thio)carbonothioyl)thio)-4-cyanopentanoic acid (BM1433, 495%, boron molecular) and all other materials were purchased from commercial sources and utilized as received.
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