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40 protocols using p 2000

1

Spectroscopic Analysis of Chemical Compounds

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Data of optical rotations, UV, and ECD spectra were obtained using Jasco P2000, JASCO V-650, and Jasco J-815 spectrophotometers (Jasco Corporation, Tokyo, Japan), respectively. IR spectra were measured with a Nicolet 5700 spectrometer (Thermo Nicolet Corporation, Madison, SD, USA). GC was performed with an Agilent 7890A instrument (Agilent Technologies, Waldbronn, Germany). The 1D- and 2D-NMR spectra were obtained at 500 or 600 MHz for 1H and at 125 or 150 MHz for 13C, using Bruker 600 and 500 MHz spectrometers (Bruker Corporation, Karlsruhe, Germany). HRESIMS data were acquired with an Agilent 1100 series LC/MSD ion trap mass spectrometer (Agilent Technologies, Waldbronn, Germany). Column chromatography was performed using macroporous resin (Diaion HP-20 and SP-700, from Mitsubishi Chemical Corp., Tokyo, Japan and Sephadex LH-20 columns Pharmacia Fine Chemicals, Uppsala, Sweden. Preparative HPLC was carried out with a Shimadzu LC-6AD instrument with an SPD-20A detector Shimadzu Corp., Tokyo, Japan, using a YMC-Pack ODS-A column (250 mm × 20 mm, 5 μm; YMC Corp., Kyoto, Japan). HPLC-DAD analysis was performed using an Agilent 1200 series system (Agilent Technologies, Waldbronn, Germany) with an Apollo C18 column (250 mm × 4.6 mm, 5 μm; Alltech Corp., Lexington, KY, USA).
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2

Comprehensive Analytical Characterization of Compounds

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The optical rotation was measured by a polarimeter JASCO P-2000 (JASCO, Tokyo, Japan). The infrared spectra were obtained on a FT-IR spectrophotometer, Nicolet™ iS™ 5 FTIR Spectrometer (Thermo Fisher Scientific, Waltham, MA, USA). UV spectra were collected by Spectrophotometer U-3310 UV-Vis (Hitachi, Ltd., Tokyo, Japan). The 1D and 2D NMR spectra were obtained on an Agilent 600 MHz DD2 NMR (Agilent, Santa Clara, CA, USA). The chloroform-d was used as the internal lock. HRESIMS data in positive mode were collected on a Waters LC/Q-TOF SYNAPT G2 (Waters Corporation, Milford, MA, USA) system. All isolations were purified by MPLC and HPLC. The former is Biotage® Isolera™ Systems (Biotage, Uppsala, Sweden), and the powder was filled in the flash column, Biotage® SNAP Cartridge KP-Sil 10 g (Biotage, Uppsala, Sweden), the latter is HPLC system Shimazu LC-2050 (Shimazu, Kyoto, Japan) with a Galaksil column EF-C18-H (5 μm, 120 Å, 10 × 250 mm, C18; Galak Chromatography, Wuxi, Jiangsu, China).
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3

Spectroscopic Analysis of Compounds

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The optical rotations, UV spectra and ECD spectra were recorded with JASCO P-2000, V650 and J-815 spectrometers (JASCO, Easton, MD, USA), respectively. The infrared spectra were measured on Nicolet 5700 spectrometer (Thermo Scientific, FL, USA). The NMR spectra were recorded with Bruker 500 MHz (Bruker-Biospin, Billerica, MA, USA) and 600 MHz NMR spectrometers (Varian, Inc., Palo Alto, CA, USA). HR-ESI-MS spectra were obtained using an Agilent 6520 HPLC-Q-TOF instrument (Agilent Technologies, Waldbronn, Germany). Preparative HPLC separations were performed using a Shimadzu LC-10AT with an ODS-A column (250 mm × 20 mm, 5 μm; YMC Corp., Kyoto, Japan). An Agilent 1200 series system with an Apollo C18 column (250 mm × 4.6 mm, 5 μm; Alltech Corp., KY, USA) was used for HPLC-DAD analysis. An Agilent 7890 A system with a capillary column (HP-5, 60 m × 0.32 mm, with a 1 μm film; Agilent Technologies Inc., CA, USA) was used for GC analysis. Macroporous resin (Diaion HP-20, Mitsubishi Chemical Corp., Tokyo, Japan), RP-C18 (50 μm, YMC Corp., Kyoto, Japan), and Sephadex LH-20 (Pharmacia Fine Chemicals, Uppsala, Sweden) were used for column chromatography.
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4

Comprehensive Spectroscopic Characterization

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NMR spectra were recorded on a Varian 400 (Agilent Technologies, Santa Clara, CA, USA) spectrometer using acetone-d6 as the solvent. Coupling constants are given in Hz. LC-MS analyses were run on an Agilent Infinity 1200 (Agilent Tech.), with autosampler and a diode array detector set at 320 nm, coupled with an Agilent Technologies 6120 Quadrupole (Agilent Tech.) equipped with an electrospray ionization source (ESI) operating in both positive and negative mode. The column was a Kinetex C18 (150 × 2.1 mm, 100 Å, 5 μm) (Phenomenex, Torrance, CA, USA), and the eluent was a mixture of water + 0.1% formic acid (FA) (v/v) (solvent A) and acetonitrile + 0.1% FA (v/v) (solvent B) with the gradient reported in Table 3. The flow was 0.25 mL/min.
Optical rotations were determined on a Jasco P2000 (Jasco, Tokyo, Japan) polarimeter at the wavelength of sodium D (λ = 589 nm) using a quartz cell of 1 dm length. Circular dichroism spectra were recorded on a Jasco J-710 spectropolarimeter using a quartz cell of 0.1 cm optical path.
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5

Analytical Techniques for Chemical Characterization

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1D and 2D NMR spectra were taken on Bruker Avance III 500 MHz. The chemical shift (δ) values are reported in ppm with CDCl3 used as the internal standard, and coupling constants (J) are in Hz. Low- and high-resolution ESIMS and EIMS were measured on a Bruker Daltonics Esquire HCT ultra high capacity trap mass spectrometer, and an Orbitrap mass spectrometer (LTQ Orbitrap XL and Q Exactive Plus, Thermo Fisher Scientific), respectively. Optical rotations, UV, and IR spectra were measured on a JASCO-P-2000 polarimeter (cell length 10 mm), a PerkinElmer#Lambda265, and a Shimadzu model IR Prestige-21 Fourier-transform infrared spectrophotometer, respectively. TLC was performed on Kieselgel 60 F254 (0.25 mm, Merck) and RP-18 F254S (0.25 mm, Merck) coated plates, spots were recognized under ultraviolet light at 254 and 356 nm, and then stained by spraying with 5% H2SO4 in MeOH before heating on a hot plate. Silica gel (Silicycle 70–230 and 230–400 mesh), RP-18 (LiChroprep® 40–63 μm, Merck), and TOYOPEARL® HW-40F (Tosoh, Japan) were used for column chromatography.
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6

Spectroscopic Analysis of Natural Compounds

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The optical rotations, UV spectra, and ECD spectra were recorded with JASCO P-2000, V650 and J-815 spectrometers (JASCO, Easton, MD, USA), respectively. The infrared spectra were measured on a Nicolet 5700 spectrometer (Thermo Scientific, FL, USA). The NMR spectra were recorded with a Bruker 500 MHz nuclear magnetic resonance instrument (Bruker-Biospin, Billerica, MA, USA). HRESIMS reports were obtained from an Agilent 6520 HPLC-Q-TOF (Agilent Technologies, Waldbronn, Germany). Preparative HPLC separations were performed using a Shimadzu LC-10AT with an ODS-A column (250 mm×10 mm, 5 μm; YMC Corp., Kyoto, Japan). An Agilent 1200 series system with an Apollo C 18 column (250 mm×4.6 mm, 5 μm; Alltech Corp., KY, USA) was used for HPLC-DAD analysis. Macroporous resin (Diaion HP-20, Mitsubishi Chemical Corp., Tokyo, Japan), RP-C18 (50 μm, YMC Corp., Kyoto, Japan), and Sephadex LH-20 (Pharmacia Fine Chemicals, Uppsala, Sweden) were used for column chromatography. The Agilent 7890A was used to carry on the GC analysis with a capillary column, HP-5 (60 m×0.32 mm, with a 1 μm film; Agilent Technologies Inc., CA, USA).
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7

Solanum melongena L. Root Analysis

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NMR spectra were obtained on Bruker DPX 400 instrument (Bruker, Karlsruhe, Germany) and the optical rotations were determined with a JASCO P-2000 instrument (Jasco, Tokyo, Japan) while, the HR-ESI-MS data was recoreded on Waters Xevo-TOF-MS (Waters, Milford, America). Semipreparative HPLC was conducted with a Waters XBridgeTM Prep C18 column (250×10 mm, 5 μm) (Waters, Milford, America), and the HPLC system was equipped with a Shimadzu CBM-20A, RID detector, and LC-6AD pump (Shimadzu, Tokyo, Japan). Column chromatography was performed using silica gel of 100-120 mesh and 200-300 mesh (Qingdao Marine Chemical Co., Qingdao, China), ODS (YMC Company Ltd., Japan), and Sephadex LH-20 (Merck, Germany). All the solvents were of analytical grade (Tianjinfuyu Co., Tianjin, China).
The roots of Solanum melongena L. were collected in September 2016 from Anguo City, Hebei Province, People's Republic of China. They were identified by Prof. Rui-Feng Fan of the Heilongjiang University of Chinese Medicine. The voucher specimen (No. 20160918) was deposited in Heilongjiang University of Chinese Medicine, Harbin, China.
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8

Characterization of Novel Triterpenoid Saponins

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The HR-ESI-MS data of the new triterpenoid saponins were obtained on a Thermo Orbitrap Fusion Lumos Tribrid Mass Spectrometer. The 1D and 2D NMR spectra were acquired on a Bruker DPX-600 spectrometer in Pyridine-d5 using TMS as internal standard. Preparative high-performance liquid chromatography (HPLC) (LC-20AR, Shimadzu) was performed on Waters Atlantis® Prep T3 (5 μm, 10 × 250 mm column) with a RID-20 A detector, with flow rates of 3 ml/min. Optical rotation measurements were conducted on a JASCO P-2000 instrument. Gas chromatography-mass spectrometry (GC-MS) analysis was performed on an Agilent 7890A system with a DB-5 capillary column. Absorbance (OD) value was detected on a BioTek Epoch™2 Microplate Reader. The FT-IR data of the new triterpenoid saponins was performed on Thermo Scientific Nicolet iS10. Silica gel column chromatography (CC) and octadecyl silica (ODS) chromatography were used in the separation of extracts.
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9

Characterization of Upconversion Nanostructures

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The crystal structures, sizes, morphologies,
and elementary compositions were characterized by SEM (FEI-Sirion
200), TEM (JEM-2010F), and high-resolution TEM (JEM-2100F). The crystalline
compositions and phases of the as-prepared UC materials were characterized
by an X-ray diffractometer (XRD, D8 ADVANCE, Bruker-AXS) using Cu
Kα radiation at 1.5418 nm at a scanning rate of 10°/min.
UC luminescence spectra of samples were obtained on FL4000 fluorophotometer
at room temperature in conjunction with a 980 nm diode laser. The
chirality property was clarified with CD (J-815) and auto polarimeter
(JASCO P-2000).
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10

Optical Rotation of (±)-3-Nitroatenolol Enantiomers

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The optical rotation values were measured for each enantiomer of the synthesized (±)-3-nitroatenolol at 589 nm with a Jasco P-2000 polarimeter using a 10 cm microcell. Each sample was dissolved in MeOH, and the obtained values are reported in Table 1.
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