The instruments and experimental conditions were the same as those described in a previous paper [28 (link)]. Optical rotations were measured on a JASCO P-1030 automatic digital polarimeter (Jasco). IR spectra were obtained using a JASCO FT-IR 620 spectrophotometer (Jasco). NMR spectra were recorded on a Bruker DRX-500 or AV-600 spectrometer (Bruker) using standard Bruker pulse programs. Chemical shifts (δ) were given with reference to tetramethylsilane (TMS) as an internal standard. HR-ESI-TOF-MS data were obtained using a Water-Micromass LCT mass spectrometer (Waters-Micromass). CC was conducted by Diaion HP-20 (Mitsubishi-chemical), silica gel Chromatorex BW-300 (Fuji-Silysia Chemical), and ODS silica gel COSMOSIL 75C18-OPN (Nacalai Tesque). Analytical TLC was performed on precoated silica gel 60 F254 or RP18 F254S plates (0.25 mm thick) (Merck). The spots were detected by spraying the plates with 10% H2SO4 aqueous solution and then heating. HPLC was conducted using a system consisting of a CCPM pump (Shimadzu), an RI-8021 (Tosoh) or a Shodex OR-2 (Showa-Denko) detector, and a Rheodyne injection port (Rohnert Park). A TSK gel ODS-100Z column (10 mm i.d. × 250 mm, 5 µm) (Tosoh) was used for the preparative HPLC. Enzymatic hydrolysis was carried out using naringinase (EC 232-962-4, Sigma), acetic acid (AcOH) and potassium acetate (AcOK) (Wako).
P 1030
Manufactured by Jasco
Sourced in Japan
The P-1030 is a laboratory equipment designed for general laboratory use. It serves as a general-purpose tool for various experimental and analytical tasks. The core function of the P-1030 is to provide a reliable and consistent platform for conducting various laboratory procedures.
Automatically generated - may contain errors
Lab products found in correlation
Cosmosil 75c18 opn, by Nacalai Tesque (4 mentions)
Microtof mass spectrometer, by Bruker (3 mentions)
Diaion hp 20, by Mitsubishi (2 mentions)
Aviii 500 spectrometer, by Bruker (2 mentions)
Spekol 1200 spectrophotometer, by Analytik Jena (2 mentions)
Alpha spectrometer, by Bruker (2 mentions)
Ft ir 620 spectrophotometer, by Jasco (1 mentions)
Shodex or 2, by Resonac (1 mentions)
Av 600, by Bruker (1 mentions)
Rp 18 f254s plates, by Merck Group (1 mentions)
Drx 500, by Bruker (1 mentions)
6224a accurate mass tof lc ms system, by Agilent Technologies (1 mentions)
Al 400, by JEOL (1 mentions)
Eca 600, by JEOL (1 mentions)
Jms t100gc, by JEOL (1 mentions)
Jms dx303, by JEOL (1 mentions)
Rp 18 f254, by Merck Group (1 mentions)
Jms 700, by JEOL (1 mentions)
Ft ir 480 plus ft ir spectrometer, by Jasco (1 mentions)
6210 esi tof mass spectrometer, by Agilent Technologies (1 mentions)
12 protocols using p 1030
1
Analytical Techniques for Structural Characterization
2
Characterization of Natural Products
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A JASCO P-1030 digital polarimeter was used for optical rotation measurements. Preparative high-performance liquid chromatography (HPLC) with a system equipped with ELITE P-230 pumps and a UV detector was used. High-resolution mass spectra (HR-ESI-TOF-MS) were obtained with an Agilent Technologies 6224A accurate mass TOF LC/MS system. NMR spectra were observed with Bruker AV III-500 spectrometer and NMR chemical shifts in δ (ppm) were referenced to solvent peaks of δC 77.0 and δH 7.26 for CDCl3. Column chromatography was performed by using silica gel (200–300 mesh, Yantai Chemical Industry Research Institute, Yantai, China) or reversed phase C18 (Octadecylsilyl, ODS) silica gel (Cosmosil 75C18-OPN, Nacalai Tesque, Kyoto, Japan).
3
Phytochemical Analysis and Isolation
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The chemical reagents used were of HPLC grade and purchased from TEDIA (Rhode Island, USA). The others were of analytical grade and obtained from Sinopharm Chemical Reagent Co. Ltd. (Shanghai, China). The preparative HPLC system was equipped with two ELITE P-230 pumps and an UV detector. Optical rotations were determined on a JASCO P-1030 digital polarimeter. High-resolution ESI-TOF-MS analyses were performed on an Agilent Technologies 6224A Accurate-Mass TOF LC/MS system (Santa Clara, CA, USA). Nuclear magnetic resonance (NMR) spectra were recorded on a Bruker AV III-500 spectrometer (Bruker, Billerica, MA, USA). Column chromatography was performed over the silica gel (200–300 mesh, Yantai Chemical Industry Research Institute, Yantai, China) or reversed phase C18 (Octadecylsilyl, ODS) silica gel (Cosmosil 75C18-OPN, Nacalai Tesque, Japan).
4
Analytical Techniques for Natural Products
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Analytical TLC was performed on silica gel 60F254 and RP-18F254S (Merck). Column chromatography was carried out on silica gel 60 (70–230 mesh, Merck) and COSMOSIL 75C18-OPN (Nacalai Tesque, Inc.). NMR spectra were recorded on JEOL ECA-600 and AL-400. Chemical shifts for 1H and 13C NMR are given in parts per million (δ) relative to tetramethylsilane (δH 0.00) and residual solvent signals (δC 77.0) as internal standards. Mass spectra were measured on JEOL JMS-700, JMS-DX303, and JMS-T 100 GC. Optical rotations were measured on JASCO P-1030.
5
Spectroscopic Analysis of Novel Compounds
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Optical rotations were recorded on a JASCO P-1030 automatic digital polarimeter, and UV spectra were recorded with a JASCO V-550 UV/VIS spectrophotometer. IR spectra were determined using a JASCO FT/IR-480 plus FT-IR spectrometer. HRESIMS data were determined by an Agilent 6210 ESI/TOF mass spectrometer. NMR spectra were obtained by a Bruker AV-400 spectrometer with TMS as an internal standard. Preparative HPLC was performed using a Varian chromatograph equipped with a C18 reversed-phase column (Cosmosil, 5 µm, 10 mm × 250 mm). Analytical HPLC was performed using a Waters chromatograph equipped with a C18 reversed phase column (Cosmosil, 5 µm, 4.6 mm × 250 mm). Silica gel (200–300 mesh; Qingdao Marine Chemical, Inc.), ODS silica gel (50 µm; YMC), and Sephadex LH-20 (Pharmacia) were used for column chromatography experiments. Silica gel GF254 plates (Yantai Chemical Industry Research Institute, Yantai, China) were used for thin-layer chromatography (TLC).
6
Spectroscopic characterization of organic compounds
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All chemicals were purchased from Wako Pure Chemical Industries (Osaka, Japan), Kanto Chemicals (Tokyo, Japan) and Nacalai Tesque (Kyoto, Japan).
Optical rotations were measured on a JASCO P-1030 polarimeter. NMR spectra were recorded on a JEOL ECA 500 (500 MHz) spectrometer. Chemical shifts are denoted in δ (ppm) relative to residual solvent peaks as internal standards (CD3OD: δH 3.31, δC 49.0). LC–MS experiments and ESI–TOF MS/MS analyses were performed with an amaZon SL-NPC (Bruker Daltonics) or LCMS-2020 (Shimadzu) spectrometer coupled with a Shimadzu HPLC system equipped with an LC-20AD intelligent pump. GC–MS experiments were performed with a Shimadzu-QP2010 Ultra system. HRESIMS analyses were performed with a Thermo Scientific LTQ Orbitrap XL (LTQ XL coupled with LTQ QR) spectrometer.
Optical rotations were measured on a JASCO P-1030 polarimeter. NMR spectra were recorded on a JEOL ECA 500 (500 MHz) spectrometer. Chemical shifts are denoted in δ (ppm) relative to residual solvent peaks as internal standards (CD3OD: δH 3.31, δC 49.0). LC–MS experiments and ESI–TOF MS/MS analyses were performed with an amaZon SL-NPC (Bruker Daltonics) or LCMS-2020 (Shimadzu) spectrometer coupled with a Shimadzu HPLC system equipped with an LC-20AD intelligent pump. GC–MS experiments were performed with a Shimadzu-QP2010 Ultra system. HRESIMS analyses were performed with a Thermo Scientific LTQ Orbitrap XL (LTQ XL coupled with LTQ QR) spectrometer.
7
Spectroscopic Characterization of Compounds
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One and two-dimensional nuclear magnetic resonance spectroscopy were recorded on Bruker AVANCE 600 (600 MHz) spectrometer. Chemical shifts of 1H NMR were reported in parts per million (ppm, d) relative to HDO (d = 4.70) in D2O. Low resolution mass and high-resolution mass spectrum were obtained on a JEOL JMS-700T for fast atom bombardment ionization (FAB) [positive mode, matrix: glycerol]. Optical rotations were taken on a JASCO P-1030 polarimeter with a sodium lamp (D line). Amino acid analysis was performed by an enantiomer labeling method of amino acid analysis (110°C, 24 h) at HiPep Laboratories. The analytical data are informed in Supplemental Results.
8
Comprehensive Characterization of Compound
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UV spectrum was performed in MeOH on a Spekol 1200 spectrophotometer from Analytik Jena. Optical rotation was measured with a JASCO P-1030 digital polarimeter. FT-IR spectrum was measured on a Bruker ALPHA spectrometer. NMR spectra were acquired in acetone-d6 or CD3OD or DMSO-d6 on either a Bruker Avance 400 MHz or Bruker Avance 500 MHz NMR spectrometer. HRESIMS data was determined on a Bruker MicrOTOF mass spectrometer.
9
Structural Characterization of Compounds
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Optical rotation was measured on a JASCO P-1030 digital polarimeter. UV spectra were recorded on a Hitachi U-2900 spectrophotometer. IR spectra were measured on a Nicolet Avatar-360 spectrometer with KBr pellets. NMR spectra were obtained on Varian Mercucy Plus 400 instruments. Chemical shifts were reported with TMS as internal standard or with respect to acetone-d6 (δH 2.04, δC 206.0 ppm). EIMS (70 eV) and HREIMS were recorded on an Agilent 5973N and a Waters Micromass GCT mass spectrometer, respectively. ESIMS and HRESIMS were performed on an Agilent 1100 LC/MSD and a Bruker Daltonics ApexIII mass spectrometer, respectively. Semi-preparative HPLC was performed on an Agilent 1200 (Agilent Technologies, Palo Alto, CA, USA) and a Sepax Amethyst C18 column (150 × 10 mm, 5 μm, Sepax Techologies, Inc., Newark, DE, USA), using a UV detector set at 210 nm. Column chromatography (CC) was performed on silica gel (200-300 mesh, Yantai Institute of Chemical Technology, Yantai, People’s Republic of China), Diaion HP-20 (Mitsubishi Chemical Co., Tokyo, Japan), and Sephadex LH-20 gel (GE Healthcare Amersham Biosciences, Uppsala, Sweden). Fractions were monitored by TLC analysis run on precoated silica gel GF254 plates (10–40 μm, Yantai Institute of Chemical Technology, Yantai, People’s Republic of China).
10
Spectroscopic Analysis of Organic Compounds
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1H and 13C-NMR spectra were taken on a Bruker Ultrashield Avance 600 spectrometer at 600 MHz and 150 MHz, respectively, with TMS as an internal standard. IR and UV spectra were measured on a HORIBA FT-720 FT-IR spectrophotometer and JASCO V-520 UV–vis spectrophotometer, respectively. Optical rotation was measured on a JASCO P-1030 digital polarimeter. Positive ion HR-ESI-MS was recorded using an LTQ Orbitrap XL mass spectrometer (Thermo Fisher Scientific, Waltham, MA, USA). Silica gel open column chromatography (CC) and reversed-phase (ODS) CC were performed on silica gel 60 (E. Merck, Darmstadt, Germany), and Cosmosil 75C18-OPN (Nacalai Tesque, Kyoto, Japan; Φ = 35 mm, L = 350 mm), respectively. HPLC was performed on an ODS column (Inertsil ODS-3, GL Science, Tokyo, Japan; Φ = 6 mm, L = 250 mm, 1.5 mL/min), and the eluate was monitored with a JASCO RI-930 intelligent detector and a JASCO PU-1580 intelligent pump unless otherwise specified.
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