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5 protocols using jms ax505wa

1

Characterization of Organometallic Complexes

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1H NMR and 13C NMR spectra were characterized by Bruker 400 MHz NMR spectrometer (Bruker-DRX400), and the chemical shifts (δ) and coupling constant (J) were expressed in ppm and hertz, respectively. Mass spectra were obtained by mass spectrometer JEOL (JMS-AX505WA), and elemental analysis was performed using CE Instrument (EA1110) instrument. Thermal analyses of DGA/TGA were performed by SDT Q600 V20.9 Build 20 instrument. Cyclic voltametric experiments were executed with a model 273A (Princeton Applied Research) using a one-compartment electrolysis cell consisting of a platinum working electrode, a platinum wire counter electrode, and a quasi Ag+/Ag electrode as a reference. The measurements were carried out in 0.5 mM CH2Cl2 solution with tetrabutylammonium tetrafluoroborate as supporting electrolyte at a scan rate of 50 mV s−1. Each oxidation potential was calibrated with ferrocene as a reference.
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2

Spectroscopic Characterization of Organic Compounds

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All reagents
and solvents from commercial sources
were used without further purification. Reactions were monitored by
thin-layer chromatography (TLC) using pre-coated silica gel plates
60F254 (Merck) in a UV light detector (254 nm). Flash column chromatography
was performed over a silica gel (70–230 mesh) purchased from
Merck. Melting points (mp) were measured in opened capillary tubes
using a Büchi B-540 without correction. 1H NMR and 13C{1H} NMR spectra were recorded on a Varian VNMRS500
(500 MHz) spectrometer using residual solvent peaks as an internal
standard (CHCl3: δ 7.26 ppm for proton, δ 77.16
ppm for carbon; DMSO: δ 2.50 ppm for proton, δ 39.97 ppm
for carbon). High-resolution mass spectra (HRMS) were obtained on
a JEOL JMS-AX 505wA, JEOL JMS-HX/HX 110A spectrometer.
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3

Isolation and Structural Elucidation of Compounds from Three Plant Species

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Compounds L1-7, O1-14, and U1-9 were isolated from J. sinensis Dode (Juglandaceae) (L1, O1-4, O10-14, and U1-9),[12 (link)13 (link)] P. koreana Nakai (Ranunculaceae) (L2-7, O6, and O9),[14 (link)] and H. helix L. (O5, O7, and O8) using repeated column chromatography and high-performance liquid chromatography. The structures of these compounds were unequivocally determined by diverse spectroscopic analyses, such as 1D, 2D nuclear magnetic resonance (NMR) experiments, mass spectrometry analyses, as well as by comparison with the literature for the known compounds. The 1H and 13C NMR 1H-1H correlation spectroscopy, Heteronuclear single quantum coherence spectroscopy (HSQC), and heteronuclear multiple bond correlation spectra were recorded on a Bruker AMX 400 (Bruker BioSpin GmbH, Karlsruhe, Germany) or 500 (Bruker BioSpin GmbH, Karlsruhe, Germany) spectrometer in pyridine-d5. High- and low-resolution FABMS (Fast Atom Bombardment Mass Spectrometry) were obtained on a JEOL JMS-AX505WA. Detection of DNA cycle and apoptosis on hepatic stellate cells-T6 cells was conducted by flow cytometry (BD Biosciences, FACSCalibur, Franklin Lakes, NJ, USA).
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4

Characterization of NI Derivatives

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TEOS was purchased from TCI (Tokyo, Japan), and the other chemicals were purchased from Sigma-Aldrich Co. (St Louis, MO, USA). All chemicals were used without further purification. The NI derivatives were characterized by 1H and 13C NMR (500 MHz; Varian, Palo Alto, CA, USA) and mass spectrometer (JMS-AX505WA; JEOL, Tokyo, Japan). Photophysical properties were obtained by UV–visible spectrometer (S-3100; Scinco, Seoul, South Korea), fluorescence spectrophotometer (FP-6500; Jasco, Oklahoma City, OK, USA), and absolute QY system (C9920-02; Hamamatsu Photonics, Hamamatsu, Japan). Size and surface charge in different environments were measured by NanoComposix (San Diego, CA, USA).
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5

Analytical Methods for Compound Characterization

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n-Hexane, n-butanol (n-BuOH), ethyl acetate (EtOAc), chloroform (CHCl3), ethanol (EtOH), and pyridine-d5 (MA, USA) were obtained from SamChun Pure Chemical Co., Korea. Fast atom bombardment mass was conducted using a JEOL JMS-AX505WA (Jeol, Japan), mass spectrometer. A high-resolution LC/MS/MS analysis was done in a Xevo G2 Q-TOF LC/MS/MS system (Waters, USA) using an ACQUITY UPLC I Class system (Dionex). The 1H- and 13C-NMR spectra were checked with a Bruker Avance 500 NMR spectrophotometer (Bremen, Germany) with trimethylsilane (TMS), the internal standard. Thin-layer chromatography (TLC) was conducted on Kiesel gel 60 F254 (250-μm) silica gel plate (Art. 5715, Merck Co., Darmstadt, Germany), and visualized by a 10% H2SO4 spraying in a methanol (MeOH) solution. Accordingly, CC was performed with a LiChroprep RP-18 (40-63 μm, Merck Co.). An MPLC system (Biotage, Uppsala, Sweden), which was equipped with cartridges (KP-SIL, 39 mm × 225 mm), was used. The sugar determinations were conducted with an HP 5890 series II GC (Hewlett-Packard, Avondale, PA, USA) using an HP-5 capillary column (30 m × 0.32 mm i.d., 0.25-μm film thickness; Agilent, J&W Scientific, Folsom, CA, USA; injector temperature: 200°C; detector temperature: 200°C; column temperature: 230°C; and flow rate of He gas: 1 mL/min).
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