400 mhz nmr spectrometer

¹H NMR spectra and ¹³C NMR spectra were recorded on an Agilent AM400 spectrometer. ¹⁹F NMR was recorded on an Agilent 400 MHz NMR spectrometer (CFCl₃ as outside standard and low field is positive). Chemical shifts (δ) are reported in ppm, and coupling constants (J) are in Hertz (Hz). The following abbreviations were used to explain the multiplicities: s = singlet, d = doublet, t = triplet, q = quartet, m = multiplet, br = broad. NMR yield was determined by ¹⁹F NMR using fluorobenzene as an internal standard before working up the reaction.
All reagents were used as received from commercial sources, unless specified otherwise, or prepared as described in the literature. All reagents were weighed and handled in air at room temperature. Blue LEDs (430–490 nm, peak wavelength: 455.0 nm) and purple LEDs (380–425 nm, peak wavelength: 395.0 nm) were bought online.

¹H NMR spectra were recorded on an Agilent 400 MHz NMR spectrometer at room temperature. Fourier transform infrared (FT-IR) spectra were measured with a Perkin-Elmer Spectrum Two FT-IR spectrophotometer. Number and weight average molecular weights (M_n and M_w) and molecular weight distributions (M_w/M_n) were determined by gel permeation chromatography (GPC) using an Agilent GPC Instrument (Model 1100) consisting of a pump, a refractive index detector and two Waters Styragel columns (HR 5E, HR 4E), using THF as the eluent at a flow rate of 0.5 mL/min at 23 °C and toluene as an internal standard. Molecular weights were calculated by using monodisperse polystyrene standards. UV–vis spectra were registered on a Schimadzu 1601 spectrophotometer. Fluorescence spectra were recorded on a Shimadzu RF-1501 spectrofluorophotometer. Thermal stabilities and the glass transition temperatures of the polymers were investigated on a Perkin-Elmer TGA/DTA 7300 thermal analysis systems, under N₂ flow with a heating rate of 20 °C/min. Molecular weights of PCL-CH, PCL-(Br)₂, PCL-(N₃)₂ and PCL-(PI)₂ were calculated with the aid of polystyrene standards by using the following conversion formula [35 (link)]: M_PCL = 0.259 M_PSt^1.073.

General Remarks. All reagents were purchased from commercial sources and used as received without purification. Reactions were monitored by thin-layer chromatography on 0.25 mm silica plate (F-254) visualizing with UV light (254 nm) and KMnO₄ solution. Flash chromatography was performed using silica gel (230–400 mesh) with hexanes and EtOAc as eluent. ¹H and ¹³C NMR spectra were recorded on Agilent 400 MHz NMR spectrometer. Chemical shifts (δ) are reported in parts per million (ppm), and coupling constants (J) are expressed in hertz (Hz). IR spectra were recorded on FT-IR using diamond attenuated total reflection (ATR) technique and were described as wavenumbers (cm⁻¹). High resolution mass spectrometry (HRMS) were measured with electrospray ionization (ESI) and quadrupole time of flight (Q-TOF) mass analyzer. Physicochemical properties were generated by CS ChemProp. Cellular fluorescence was measured with multi-plate reader (Tecan, Männedorf, Switzerland) at 490 nm/520 nm. NMR spectra of compound 1a-1q is provided as supplementary materials.

This study was carried out in strict accordance with the recommendations in the Guide for the Care and Use of Laboratory Animals of the National Institutes of Health. The protocol was approved by the International Animal Care and Use Committee of the University of North Carolina at Greensboro (Protocol Number: 11–02). All techniques were performed under isoflurane anesthesia, and all efforts were made to minimize suffering.
A panel of fullerene derivatives was synthesized at Luna Innovations and characterized for particle size using dynamic light scattering (Malvern Instruments, Zetasizer Nano ZS, Westborough, Massachusetts, USA), qNano (Izon Science, qNano, Cambridge, Massachusetts, USA) and nano particle tracking analysis, (Malvern Instruments, Nanosight LM10, Westborough, Massachusetts, USA), zeta potential (Malvern Instruments, Zetasizer Nano ZSP, Westborough, Massachusetts, USA), NMR (Agilent Technologies, 400 Mhz NMR Spectrometer, Santa Clara, California, USA), and FT-IR (Agilent Technologies, Varian 670 FT-IR, Santa Clara, California, USA). A representative physiochemical characterization schematic for the two fullerene derivatives used for the in vivo studies (ALM, a liposome encapsulated C₇₀ fullerene and TGA, a water-soluble C₇₀ fullerene conjugated with four glycolic acids) is shown in [27 (link),31 (link)].