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4 protocols using unity 500 mhz spectrometer

1

Characterization of Hybrid Nanoparticles

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The chemical structure of the HACA and the degree of substitution of the CA were assessed by using 1H-NMR (Varian Unity 500MHz spectrometer, Palo Alto, CA, USA), in which CD3OD and D2O were used as the solvent. The hydrodynamic size and zeta potential of the HANPs and MPN-HANPs were observed by dynamic light scattering (DLS) using a Zetasizer Nano ZS90 (Malvern Ins. Worcestershire, UK) with a He-Ne 633nm laser at a 90° detection angle. The morphologies of the HANPs and MPN-HANPs were characterized by using HR-TEM (JEOL-2100F, Tokyo, Japan) operated at an accelerating voltage of 200 kV. For TEM images, the samples were dispersed in deionized water (DIW) and dropped onto a 300-mesh copper grid. The nanoparticles were then treated with 1% uranyl acetate for negative staining. The UV-visible (UV-Vis) absorption spectra were measured on a UV-vis spectrophotometer (Optizen 3220UV, Mecasys Co., Ltd., Daejeon, Korea). To investigate the stability of the nanoparticles, the changes in the scattering intensity of the HANPs and MPN-HANPs were assessed in the presence of sodium dodecyl sulfate (SDS) as a typical micelle-destabilizing agent. Briefly, the HANP and MPN-HANPs (1 mg/mL in DIW) were incubated with or without SDS (2.5 mg/mL). The resulting solutions were kept at room temperature and the scattering intensity of each solution was recorded using DLS as a function of time.
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2

NMR and MS Characterization of Phormidolide

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General Procedures: All 13C NMR spectra were recorded in CDCl3 on a Bruker AM 400 NMR spectrometer operating at a 13C resonance frequency of 100.61 MHz and processed with 1.0 Hz line broadening (zgig Bruker pulse program). 1H NMR spectrum of phormidolide was recorded with residual CHCl3 as the internal standard (δC 77.0, δH 7.26) on a Varian Unity 500 MHz spectrometer. 1H NMR spectrum and 2D NMR spectra of phormidolide acetonide derivatives were obtained on a Bruker 600 MHz spectrometer equipped with a 1.7 mm MicroCryoProbe. Semi-preparative HPLC was carried out using a Waters 515 pump system equipped with a Waters 996 PDA. High resolution electrospray ionization mass spectra (HRESIMS) were obtained using an Agilent 1290 Infinity system with an Agilent 6530 Accurate Mass Q-TOF LC/MS.
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3

Spectroscopic Characterization of Compounds

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1D (1H and 13C) and 2D (COSY, ROESY, HSQC, and HMBC) NMR spectra were acquired on a Varian Unity 500 MHz spectrometer (Varian Inc., Palo Alto, CA, USA). UV spectra were obtained on a Shimadzu UV-1650PC spectrophotometer (Shimadzu Corporation, Kyoto, Japan). IR spectra were recorded on a JASCO FT/IR-4100 spectrophotometer (JASCO Corporation, Tokyo, Japan). Optical rotations were measured on a Autopol III polarimeter (Rudolph Research Analytical, Hackettstown, NJ, USA). High-resolution ESIMS was recorded on a hybrid ion-trap time-of-flight mass spectrometer (SYNAPT G2, Wasters Corporation, Milford, CT, USA). HPLC was performed on a PrimeLine pump (Analytical Scientific Instrument, Inc., El Sobrante, CA, USA) with RI-101 (Shodex, Munich, Germany). Semi-preparative HPLC was performed using an ODS column (YMC-Pack-ODS-A, 250 × 10 mm i.d, 5 µm) (YMC Corporation, Kyoto, Japan). Analytical HPLC was conducted on an ODS column (YMC-Pack-ODS-A, 250 × 4.6 mm i.d, 5 µm) (YMC Corporation, Kyoto, Japan).
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4

Instrumental Characterization of Compounds

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Optical rotations were measured on a JASCO P-2000 polarimeter. LC-MS/MS analysis was carried out using a ThermoFinnigan LCQ AdvantageMax mass detector equipped with an electrospray ionization (ESI) source. HRESIMS spectra were obtained using an Agilent 1290 Infinity system with an Agilent 6530 Accurate Mass Q-TOF LC/MS, and 1H NMR spectra were obtained using a Varian Unity 500 MHz spectrometer. Semipreparative HPLC was carried out using a Waters 515 pump system equipped with a Waters 996 PDA.
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