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Avance spectrometers 300 mhz

Manufactured by Bruker

The Avance spectrometers 300 MHz are high-performance nuclear magnetic resonance (NMR) instruments designed for analytical applications. These spectrometers operate at a frequency of 300 MHz and are capable of performing a variety of NMR experiments to analyze the structure and composition of chemical compounds.

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4 protocols using avance spectrometers 300 mhz

1

Polymer Molecular Weight Characterization

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Polymer molecular weight distributions were determined using a Tosoh size exclusion chromatography (SEC) TSK-GEL α-3000 and α-e4000 columns (Tosoh Bioscience, Montgomeryville, PA) connected in series to an Agilent 1200 Series Liquid Chromatography System (Santa Clara, CA), Wyatt Technology miniDAWN TREOS, three-angle multiangle light scattering instrument, and Optilab TrEX, refractive index detector (Santa Barbara, CA). HPLC-grade N,N′-dimethylformamide containing 0.1 wt % LiBr at 60°C was used as the mobile phase at a flow rate of 1 ml/min in a nonaqueous SEC system. Absolute molecular weight averages (Mn and Mw), polydispersity indices, and dn/dc were calculated using ASTRA software (Wyatt). Monomer conversion was determined by 1H NMR spectroscopy from the crude (T0 and Tfinal) polymer solution. Molecular weight was determined on the basis of monomer conversion. The final polymer compositions and drug wt % of the purified and lyophilized polymers were determined using 1H NMR spectroscopy (Bruker Avance spectrometers 300 MHz).
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2

Synthesis of Enzyme-Labile Prodrug Monomer

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The synthetic scheme illustrated in fig. S1 was followed to obtain the prodrug monomer SVCTQ-MA carrying enzyme labile linker valine-citrulline. All synthesized monomers and intermediates were purified by precipitation and/or silica gel column chromatography techniques. The successful synthesis and purity of the monomers were confirmed and characterized by NMR spectroscopy (Bruker Avance spectrometers 300 MHz) and electrospray ionization MS (ESI-MS; Bruker Esquire ion trap mass spectrometer). Detailed experimental procedures, NMR spectra, and ESI-MS spectral characterization of SVCTQ-MA are provided in the Supplementary Materials (figs. S2 to S5). The synthetic procedures for GalNAc-MA and VCTQ-MA have been previously published (46 (link)).
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3

Synthesis and Characterization of PI-103 Prodrug and Fluorescein Monomers

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Synthetic schemes in Figures S1A and S2A were followed to obtain PI-103 prodrug monomer and fluorescein monomer, respectively. PI-103 monomer was synthesized by conjugating the phenolic hydroxyl group of PI-103 to the carboxylic end of mono-2-(methacryloyloxy)ethyl succinate (SMA) using N-(3-dimethylaminopropyl)-N′-ethylcarbodimide hydrochloride (EDCI.HCl) as the coupling agent and N,N-dimethylpyridin-4-amine (DMAP) as the base. Fluorescein monomer was synthesized by a four-step synthetic pathway starting from 4-aminobutanoic acid using carbodiimide/DMAP coupling chemistry. The amine group was first protected with Boc group, and then coupled with 2-hydroxyethyl methacrylate (HEMA). Deprotection of the Boc group yielded amine terminated methacrylate derivative which upon conjugation with NHS activated 5-carboxyfluorescein afforded the fluorescein monomer. All the synthesized monomers and intermediates were purified by precipitation and/or silica gel column chromatography techniques. The successful synthesis and purity of the monomers were confirmed and characterized by 1H NMR spectroscopy (Bruker Avance spectrometers 300 MHz) and Electrospray Ionization-Mass spectrometry (Bruker Esquire ion trap mass spectrometer) (Figure S1B, S1C, S2B, S2C).
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4

Synthesis and Characterization of TAF Monomers

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Synthetic Scheme S1A and Scheme S2 in the supporting information were followed to obtain p-hydroxybenzyloxycarbonyl TAF methacrylate (Benzyl-TAFMA, monomer 6) and ethyloxycarbonyl TAF methacrylate (Alkyl-TAFMA, monomer 10) monomers, respectively. All the synthesized compounds were purified by precipitation and/or silica gel column chromatography. The successful synthesis and purity of the monomers were confirmed and characterized by 1 H NMR spectroscopy (Bruker Avance spectrometers 300 MHz) and Electrospray Ionization-Mass spectrometry (Bruker Esquire ion trap mass spectrometer). The full synthetic procedures and associated characterization data are detailed in the supporting information.
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