To study the chemical structure of Poly-L-Arg, Poly-L-ArgMA, PβAE homopolymers, copolymers, and their hydrogels, Fourier transforms infrared (FTIR) spectroscopy (Tensor, Bruker, Germany) was used, in the range of 400–4000 cm−1. Furthermore, the chemical modification of Poly L-ArgMA was studied by 1H NMR spectroscopy (Bruker, 500 MHz). 1H NMR spectra of Poly-L-Arg and Poly-L-ArgMA were studied in D2O solvent at 26 °C. Moreover, the molecular weight of the synthesized polymers and their copolymers was verified by gel-permeation chromatography (GPC, Knauer, Germany). While the powder of L-Arg and Poly-L-Arg were dissolved in DDW, PβAE homopolymers and copolymers were dissolved in tetrahydrofuran (THF) for NMR spectroscopy. Also, the zeta potential of the homopolymers and copolymers was determined by Horiba SZ-100 (Japan). The samples were dissolved in DDW and homogenized by an ultrasonic probe (Hielscher, UP400Sfor, Germany) for 30 min and analyzed using a zeta sizer equipped with DLS (Dynamic Light Scattering) device. The wettability the films was also estimated using water contact angle evolution at room temperature (n = 3).
1h nmr spectroscopy
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1H NMR spectroscopy is a powerful analytical technique that utilizes the nuclear magnetic resonance (NMR) phenomenon of hydrogen (1H) nuclei to provide detailed information about the structure and composition of chemical compounds. It is a non-destructive method that allows for the analysis of small quantities of sample without the need for extensive sample preparation.
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22 protocols using 1h nmr spectroscopy
1
Structural Characterization of Polymeric Hydrogels
2
Synthesis of High-Silicone Content Resin
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Example 2
A 3-L flask equipped with a stirrer, thermometer, nitrogen purge line and reflux condenser was charged with 39.75 g (0.15 mol) of compound having formula (S-2), 117.6 g (0.30 mol) of compound having fmmula (S-1), 21.5 g (0.05 mol) of compound having formula (S-6), and 2,000 g of toluene and heated at 70° C. Thereafter, 1.0 g of a toluene solution of chloroplatinic acid (platinum concentration 0.5 wt %) was added, and 48.5 g (0.25 mol) of compound having formula (S-4) and 755.0 g (0.25 mol) of compound having formula (S-5) wherein y=40 (Shin-Etsu Chemical Co., Ltd.) were added dropwise over 1 hour. The molar ratio of the total amount of hydrosilyl groups to the total amount of alkenyl goups was 1/1. At the end of dropwise addition, the reaction solution was heated at 100° C. and aged for 6 hours. Toluene was distilled off in vacuum from the reaction solution, yielding Resin 2. On 1H-NMR spectroscopy (Bruker Corp.), Resin 2 was identified to contain recurring units (a1), (a3) (a4) (b3) and (b4). Resin 2 had a Mw of 83,000 and a silicone content of 76.9 wt %.
3
Synthesis of Resin 1 from Organometallic Precursors
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Example 1
Synthesis of Resin 1
A 3-L flask equipped with a stirrer, thermometer, nitrogen purge line and reflux condenser was charged with 156.8 g (0.40 mol) of the compound having formula (S-1), 53.9 g (0.10 mol) of the compound having formula (S-3a) (UNIOX from NOF Corp.), and 2,000 g of toluene and heated at 70° C. Thereafter, 1.0 g of a toluene solution of chloroplatinic acid (platinum concentration 0.5 wt %) was added, and 97.0 g (0.50 mol) of the compound having formula (S-5) was added dropwise over 1 hour. The ratio of the total moles of hydrosilyl groups to the total moles of alkenyl groups was 1/1. At the end of dropwise addition, the reaction solution was heated at 100° C. and aged for 6 hours. Toluene was distilled off in vacuum from the reaction solution, yielding Resin 1. Resin 1 had a Mw of 43,000. On 1H-NMR spectroscopy (Bruker Corp.), Resin 1 was identified to be a polymer containing repeating units (1) and (2).
4
Synthesis and Characterization of ROS-Sensitive Polymeric Micelles
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The synthesis of TK linker, TK linker-conjugated polyethylene glycol (PEG-TK), and (PEG)-stearamine (C18) conjugate (PTC) was performed according to our previous publication [15 (link)]. As a control, we also prepared ROS-non-sensitive polymer (PC) by conjugating stearic acid to PEG-AM. Briefly, 200 mg of m-PEG amine was reacted with 160 mg of stearic acid with 160 µl of TEA, 480 mg of EDC, and 290 mg of NHS in 20 ml of DMF at 37 ℃ overnight with stirring under N2 purging. The sample was then purified by dialysis (MWCO = 12–14 KDa) against DW for one day, followed by freeze-drying. The chemical structures of the synthesized PTC and PC were confirmed using proton nuclear magnetic resonance (1H NMR) spectroscopy (400 Hz, Bruker: Billerica, MA, USA) in chloroform (CHCl3). ROS-sensitive PTC and ROS-non-sensitive PC empty micelles were prepared by the self-assembly of PTC and PC under sonication and dialysis.
5
Synthesis and Characterization of Resin 3
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Example 3
Synthesis of Resin 3
A 3-L flask equipped with a stirrer, thermometer, nitrogen purge line and reflux condenser was charged with 106.0 g (0.40 mol) of the compound having formula (S-2), 53.9 g (0.10 mol) of the compound having formula (S-3a), and 2,000 g of toluene and heated at 70° C. Thereafter, 1.0 g of a toluene solution of chloroplatinic acid (platinum concentration 0.5 wt %) was added, and 97.0 g (0.50 mol) of the compound having formula (S-5) was added dropwise over 1 hour. The ratio of the total moles of hydrosilyl groups to the total moles of alkenyl groups was 1/1. At the end of dropwise addition, the reaction solution was heated at 100° C. and aged for 6 hours. Toluene was distilled off in vacuum from the reaction solution, yielding Resin 3. Resin 3 had a Mw of 34,000. On 1H-NMR spectroscopy (Bruker Corp.), Resin 3 was identified to be a polymer containing repeating units (1) and (4).
6
Synthesis of Resin 4 via Hydrosilylation
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Example 4
Synthesis of Resin 4
A 3-L flask equipped with a stirrer, thermometer, nitrogen purge line and reflux condenser was charged with 9.8 g (0.025 mol) of the compound having formula (S-1), 10.8 g (0.025 mol) of the compound having formula (S-7), 13.3 g (0.05 mol) of the compound having formula (S-2), 215.6 g (0.40 mol) of the compound having formula (S-3a), and 2,000 g of toluene and heated at 70° C. Thereafter, 1.0 g of a toluene solution of chloroplatinic acid (platinum concentration 0.5 wt %) was added, and 97.0 g (0.50 mol) of the compound having formula (S-5) was added dropwise over 1 hour. The ratio of the total moles of hydrosilyl groups to the total moles of alkenyl groups was 1/1. At the end of dropwise addition, the reaction solution was heated at 100° C. and aged for 6 hours. Toluene was distilled off in vacuum from the reaction solution, yielding Resin 4. Resin 4 had a Mw of 50,000. On 1H-NMR spectroscopy (Bruker Corp.), Resin 4 was identified to be a polymer containing repeating units (1), (2), (3), and (4).
7
Synthesis of Resin 2 from Multifunctional Compounds
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Example 2
Synthesis of Resin 2
A 3-L flask equipped with a stirrer, thermometer, nitrogen purge line and reflux condenser was charged with 172.0 g (0.40 mol) of the compound having formula (S-7), 53.9 g (0.10 mol) of the compound having formula (S-3a), and 2,000 g of toluene and heated at 70° C. Thereafter, 1.0 g of a toluene solution of chloroplatinic acid (platinum concentration 0.5 wt %) was added, and 97.0 g (0.50 mol) of the compound having formula (S-5) was added dropwise over 1 hour. The ratio of the total moles of hydrosilyl groups to the total moles of alkenyl groups was 1/1. At the end of dropwise addition, the reaction solution was heated at 100° C. and aged for 6 hours. Toluene was distilled off in vacuum from the reaction solution, yielding Resin 2. Resin 2 had a Mw of 25,000. On 1H-NMR spectroscopy (Bruker Corp.), Resin 2 was identified to be a polymer containing repeating units (1) and (3).
8
Physico-chemical Characterization of PBAEs
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The hydrodynamic size (Dynamic Light Scattering (DLS)) and zeta potential of un-capped (acrylated terminated) PBAEs dissolved in 100 mM phosphate buffer (pH = 6.0) at about 20 mg mL–1 were measured using a Malvern Zetasizer Nano ZS (Malvern Instruments, Malvern, UK); zeta potentials were calculated using the Smoluchowsky model.
Molecular weight of each PBAE in the library was determined by gel permeation chromatography (GPC) using a Shimadzu-LC-20Ai system equipped with a SuperdexTM 75 10/300 GL column; the mobile phase was 100% sodium acetate buffer pH = 5 eluted at 1 mL min–1. Number-averaged (Mn) and weight-averaged molecular weight (Mw) were calculated using PEG standards. Because the molar masses were measured by GPC, they are not the real values but only apparent values due to the use of PEG standards and due to possible different hydrodynamic volumes of PEG standards and poly(beta-amino esters) of identical molar mass.
1H-NMR spectroscopy was performed (Bruker BioSpin GmbH) to identify the structures and estimate drug load of the conjugated PBAE–DEX. Samples were prepared at 10–12 mg mL in DMSO-d6.
Molecular weight of each PBAE in the library was determined by gel permeation chromatography (GPC) using a Shimadzu-LC-20Ai system equipped with a SuperdexTM 75 10/300 GL column; the mobile phase was 100% sodium acetate buffer pH = 5 eluted at 1 mL min–1. Number-averaged (Mn) and weight-averaged molecular weight (Mw) were calculated using PEG standards. Because the molar masses were measured by GPC, they are not the real values but only apparent values due to the use of PEG standards and due to possible different hydrodynamic volumes of PEG standards and poly(beta-amino esters) of identical molar mass.
1H-NMR spectroscopy was performed (Bruker BioSpin GmbH) to identify the structures and estimate drug load of the conjugated PBAE–DEX. Samples were prepared at 10–12 mg mL in DMSO-d6.
9
Structural Characterization of F68-VES Polymer
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The structure of F68–VES polymer was confirmed by 1H nuclear magnetic resonance (1H NMR) spectroscopy and fourier transform infrared (FTIR) spectroscopy. F68–VES polymer was detected by 1H NMR spectroscopy (Bruker Optik GmbH, Ettlingen, Germany) at 400 MHz using DMSO-d6 as solvent. FTIR spectrophotometer (Nicolet, Hudson, NH, USA) was used to additionally demonstrate the structure of F68–VES in the absorbance range of 400–4,000 cm−1.
10
Synthesis of Photodegradable PEG Polymer
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