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19 protocols using unity inova 500 ft nmr

1

Nuclear Magnetic Resonance Analysis Protocol

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All reagents and solvents were purchased as reagent grade and were used without further purification. Nuclear magnetic resonance (NMR) spectra were recorded on a Varian Unity INOVA 500 FT-NMR. Chemical shifts for samples were measured in DMSO-d6 and calibrated against sodium salt of 3-(trimethylsilyl) propionic-2,2,3,3-d4 acid (TSP) as an external reference in a sealed capillary tube. NMR data were processed and analyzed with MestReNova Version 6.1.1-6384. The melting point was determined on a Mel-Temp (Electrothermal 120 VAC 50/60 Hz) melting point apparatus and was uncorrected. Elemental analysis was carried out by ECS 4010 Analytical Platform (Costech Instrument) elemental analyzer at Jackson State University.
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2

Spectroscopic Characterization of Compounds

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Measurements of optical rotations and IR spectra were carried out on a JASCO P-1020 polarimeter and FT/IR-4100 infrared spectrophotometer (JASCO Corporation, Tokyo, Japan), respectively. ESIMS and HRESIMS were performed on a Bruker APEX II (Bruker, Bremen, Germany) mass spectrometer. The NMR spectra were recorded on a Varian 400MR FT-NMR at 400 and 100 MHz for 1H and 13C, respectively or a Varian Unity INOVA500 FT-NMR at 500 and 125 MHz for 1H and 13C, respectively (Varian Inc., Palo Alto, CA, USA). Silica gel or reversed-phase (RP-18, 230–400 mesh) silica gel was used for column chromatography and analytical thin-layer chromatography (TLC) analysis (Kieselgel 60 F-254, 0.2 mm, Merck, Darmstadt, Germany), respectively. Isolation and purification of compounds by high-performance liquid chromatography (HPLC) were achieved using an Hitachi L-2455 HPLC apparatus (Hitachi, Tokyo, Japan) equipped with a Supelco C18 column (250 × 21.2 mm, 5 μm, Supelco, Bellefonte, PA, USA).
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3

Analytical Techniques for Chemical Characterization

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Optical rotations and IR spectra were recorded on a JASCO P-1020 polarimeter and FR/IR-4100 infrared spectrophotometer (Jasco Corporation, Tokyo, Japan), respectively. NMR spectra were acquired on a Varian Unity Inova 500 FT-NMR (Varian Inc., Palo Alto, CA, USA) at 500 and 125 MHz for 1H and 13C, respectively; or on Varian 400 MR FT-NMR instrument at 400 MHz and 100 MHz for 1H and 13C, respectively. The data of low-resolution electron spray ionization mass spectroscopy (LRESIMS) were measured by Bruker APEX II mass spectrometer. The data of HRESIMS were obtained by Bruker Apex-Qe 9.4T mass spectrometer. Silica gel 60 and reverse-phased silica gel (RP-18; 230–400 mesh) were used for normal-phase and reverse-phased column chromatography. Precoated silica gel plates (Kieselgel 60 F254, 0.2 mm) (Merck, Darmstadt, Germany) were used for analytical TLC. High-performance liquid chromatography was performed on a Hitachi L-2455 HPLC apparatus with a Supelco C18 column (ODS-3, 5 μm, 250 × 20 mm; Sciences Inc., Tokyo, Japan).
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4

Spectroscopic Analysis of Organic Compounds

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Measurements of optical rotations, IR, and circular dichroisms spectra were performed on the JASCO P-1020 polarimeter, FT/IR-4100 infrared spectrophotometer (JASCO Corporation, Tokyo, Japan), and Jasco J-715 CD spectrometer, respectively. LRESIMS were measured on a Bruker APEX II (Bruker, Bremen, Germany) mass spectrometer, and HRESIMS were measured on the Bruker APEX II and the Impact HD Q-TOF mass spectrometers (both Bruker, Bremen, Germany). The NMR experiments were recorded on a Varian Unity INOVA 500 FT-NMR (Varian Inc., Palo Alto, CA, USA). The silica gel (40−63 μm, Merck, Billerica, MA, USA) and reversed-phase silica gel (RP-18, 40−63 μm, Merck, Darmstadt, Germany) were used for column chromatography. The thin-layer chromatography (TLC) analysis was carried out on aluminum plates coated with silica gel (Silica gel 60 F254, 100 μm, Merck, Darmstadt, Germany) or C18 gel (Silica gel 60 RP-18 F254s, 100 μm, Merck, Darmstadt, Germany). High-performance liquid chromatography (HPLC) was performed on a Hitachi L-2455 HPLC apparatus (Hitachi, Tokyo, Japan) with a Supelco C18 column (250 × 21.2 mm, 5 μm, Supelco, Bellefonte, PA, USA).
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5

Analytical Techniques for Compound Characterization

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Measurements of circular dichroisms, optical rotations, and IR spectra were carried out on a Jasco J-715 CD spectrometer, JASCO P-1020 polarimeter, and FT/IR-4100 infrared spectrophotometer (JASCO Corporation, Tokyo, Japan), respectively. ESIMS was performed on a Bruker APEX II (Bruker, Bremen, Germany) mass spectrometer, and HRESIMS was performed on a Bruker APEX II and Impact HD Q-TOF mass spectrometers (Bruker, Bremen, Germany). The NMR spectra were recorded on a Varian 400MR FT-NMR at 400 and 100 MHz for 1H and 13C, respectively; a Varian Unity INOVA500 FT-NMR (both Varian Inc., Palo Alto, CA, USA) at 500 and 125 MHz for 1H and 13C, respectively; or a JEOL ECZ600R FT-NMR (Japan) at 600 and 150 MHz for 1H and 13C, respectively. Silica gel and reversed-phase (RP-18, 230–400 mesh) silica gel were used for column chromatography and analytical thin-layer chromatography (TLC) analysis (Kieselgel 60 F-254, 0.2 mm, Merck, Darmstadt, Germany), respectively. The isolation and purification of compounds by high-performance liquid chromatography (HPLC) were achieved using a Hitachi L-2455 HPLC apparatus (Hitachi, Tokyo, Japan) equipped with a Supelco C18 column (250 × 21.2 mm, 5 μm, Supelco, Bellefonte, PA, USA).
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6

Isolation and Characterization of Bioactive Compounds

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Values of the specific optical rotation of the isolates were measured with a JASCO P-1020 polarimeter (JASCO Corporation, Tokyo, Japan). Infrared spectra were recorded using a JASCO FT/IR-4100 infrared spectrophotometer (JASCO Corporation, Tokyo, Japan). The CD spectrum was recorded on a Jasco J-815 circular dichroism (CD) spectropolarimeter (JASCO, Tokyo, Japan) in MeOH. 1H- and 13C-NMR spectra were acquired on a Varian 400MR FT-NMR (or Varian Unity INOVA500 FT-NMR) instrument (Varian Inc., Palo Alto, CA, USA) at 400 MHz (or 500 MHz) and 100 MHz (or 125 MHz), respectively, in CDCl3 or C6D6. LR-ESI-MS and HR-ESI-MS experiments were carried out using a Bruker APEX II (Bruker, Bremen, Germany) mass spectrometer. Silica gel (230–400 mesh) was used as the adsorbent for normal-phase column chromatography. Thin-layer chromatography (TLC) analyses were performed with precoated silica gel plates (Kieselgel 60 F-254, 0.2 mm, Merck, Darmstadt, Germany). Further purification of impure fractions or compounds was further achieved by high-performance liquid chromatography on a Hitachi L-7100 HPLC instrument (Hitachi Ltd., Tokyo, Japan) with a Merck Hibar Si-60 column (250 mm × 21 mm, 7 μm; Merck, Darmstadt, Germany) and on a Hitachi L-2455 HPLC apparatus (Hitachi, Tokyo, Japan) with a Supelco C18 column (250 mm × 21.2 mm, 5 μm; Supelco, Bellefonte, PA, USA).
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7

Characterization of Novel Compounds

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All of the reagents and solvents were purchased
as reagent grade and used without further purification. Nuclear magnetic
resonance (NMR) spectra were recorded on a Varian Unity INOVA 500
FT-NMR. Chemical shifts for the samples were measured in DMSO-d6 and calibrated against the sodium salt of
3-(trimethylsilyl)propionic-2,2,3,3-d4 acid (TSP) as an external reference in a sealed capillary tube.
NMR data were processed and analyzed with MestReNova version 6.1.1-6384.
The IR spectra were recorded on a Perkin Elmer-Spectrum One Fourier
transform infrared spectrometer with KBr disks in the range of 4000–400
cm–1. The melting point was determined on a Mel-Temp
(Electrothermal 120 VAC 50/60 Hz) melting point apparatus and was
uncorrected. Mass spectral data were obtained at electrospray ionization
mass spectrometry (ESI-MS) positive mode on a TSQ Quantum GC (Thermo
Scientific). Elemental analysis was carried out using an ECS 4010
Analytical Platform (Costech Instrument) at Jackson State University.
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8

Characterization of Chemical Compounds

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Optical rotations were measured on a JASCO P-1020 polarimeter (Jasco Corporation, Tokyo, Japan). IR spectra were recorded on a JASCO FT/IR-4100 spectrophotometer (Jasco). ESIMS and HRESIMS data were performed on a BRUKER APEX II mass (Bruker, Bremen, Germany) spectrometers. The NMR spectra were recorded on a Varian Unity INOVA 500 FT-NMR (Varian Inc., Palo Alto, CA, USA) at 500 MHz for 1H and 125 MHz for 13C or on a Varian 400 FT-NMR (Varian Inc.) at 400 MHz for 1H and 100 MHz for 13C in CDCl3 or C6D6 using TMS as internal standard (δ in ppm, J in Hz). Silica gel 60 (230–400 mesh, Merck, Darmstadt, Germany) pre-coated silica gel plates (Merck, Kieselgel 60 F254, 0.2 mm) were used for open CC and analytical TLC analysis, respectively. Isolation by HPLC was performed by a Hitachi L-2455 instrument (Hitachi Ltd., Tokyo, Japan) equipped with a reversed-phase (RP-18) column (ODS-3, 5 µm, 250 × 20 mm, Sciences Inc., Tokyo, Japan).
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9

Analytical Characterization of Compounds

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Optical rotations and IR spectra were measured on a JASCO P-1020 polarimeter and a JASCO FT/IR-4100 (JASCO Corporation, Tokyo, Japan) spectrophotometer, respectively. HRESIMS spectra were measured on a Bruker APEX II mass spectrometer (Bruker, Bremen, Germany). 1H and 13C NMR spectra were obtained on a Varian Unity INOVA 600 FT-NMR (or Varian Unity INOVA500 FT-NMR) instruments (Varian Inc., Palo Alto, CA, USA) at 600 MHz (or 500 MHz) for 1H, and 150 MHz (or 125 MHz) for 13C in CDCl3. Thin-layer chromatography (TLC) analyses were performed on precoated silica (Si) gel plates (Kieselgel 60 F-254, 0.2 mm), and Si gel (230–400 mesh) (Merck, Darmstadt, Germany) and C18-reversed phase Si gel (RP-18; 40–63 µM) (Parc-Technologique BLVD, Quebec, Canada) were used for column chromatography. Further purification and the isolation of compounds were performed by reversed-phase high-performance liquid chromatography (RP-HPLC) on a Hitachi L-2455 HPLC apparatus with a Supelco C18 column (250 × 21.2 mm, 5 μm).
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10

Spectroscopic Characterization of Compounds

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All reagents and solvents were purchased as reagent grade and used without further purification. Nuclear magnetic resonance (NMR) spectra were recorded on a Varian Unity INOVA 500 FT-NMR. Chemical shifts for samples were measured in CDCl3 or DMSO-d6 and calibrated with tetramethylsilane (TMS) as an internal reference. Elemental analysis was carried out using an ECS 4010 Analytical Platform (Costech Instrument) at Jackson State University. The absorbance was measured on a UV-2600 UV-VIS spectrophotometer (SHIMADZU). Mass spectral data were obtained in the ESI-MS positive mode on a TSQ Quantum GC (Thermo Scientific).
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