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5 protocols using uv 2201 spectrometer

1

Spectroscopic Characterization of Natural Products

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Optical rotations were measured with a Perkin-Elmer 241 polarimeter. The UV spectra were conducted on a Shimadzu UV-2201 spectrometer. ECD spectra were recorded on a JASCO J-815 spectrometer. HRESIMS were recorded on Agilent Accurate-Mass-Q-TOF MS 6520 system equipped with electrospray ionization (ESI) source. NMR spectra were recorded on a Bruker AV-600 NMR spectrometer using TMS as an internal standard. The chromatographic silica gel (200–300 mesh) and polyamide (100–200 mesh) were purchased from Qingdao Marine Chemical Factory (Qingdao, China) and ODS (50 μm) was produced by YMC Co. LTD., Kyoto, Japan. Sephadex LH-20 was purchased from GE Healthcare. RP-HPLC separations were conducted using a Shimadzu LC-20AT liquid chromatograph with a YMC-PACK ODS-A column (250 × 10 mm, 5 μm) and Knauer K-2600 UV detector. Chiral separation was conducted in a Daicel AS-H column (250 × 4.6 mm, 5 μm) from Daicel Chemical Industries, Ltd. (Japan). TLC spots were visualized under UV light and by dipping into 10% H2SO4 in EtOH followed by heating. RAW 264.7 cells, human chronic myelogenous leukemia (K562) and human lung carcinoma (A549) cell lines were obtained from National infrastructure of cell line resource.
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2

Spectroscopic and Chromatographic Characterization

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The UV spectra were conducted on a UV-2201 spectrometer (Shimadzu, Kyoto, Japan). The FT-IR spectra were obtained on a Bruker IFS-55 spectrometer (Bruker, Ettlingen, Germany) by a KBr disk method. ESI-MS spectra were conducted on an Agilent 1100 ion trap spectrometer (Agilent Technologies, Palo Alto, CA, USA). HRESI-MS was recorded on a QFT-ESI mass spectrometer (Varian, Palo Alto, CA, USA). 1H-NMR and 13C-NMR spectra were recorded on Bruker ARX-300 and AV-600 NMR spectrometers (Bruker, Ettlingen, Germany) using pyridine-d5 as an internal standard [δH/C 7.20, 7.57, 8.72/123.44, 135.43, 149.84 (C5D5N)]. Optical rotations were measured with a Perkin-Elmer 241 polarimeter (Perkin-Elmer, Boston, MA, USA). The chromatographic silica gel (200−300 mesh) was purchased from Qingdao Ocean Chemical Factory (Qingdao, China) and ODS (50 μm) was purchased from YMC Co. Ltd, Kyoto, Japan. Sephadex LH-20 was purchased from GE Healthcare, Uppsala, Sweden. RP-HPLC analysis and semi-preparation were conducted using HITACHI L2130 series pumping system equipped with a HITACHI L2400 UV detector (Tokyo, Japan) and performed with a C-18 column (10 × 250 mm, 10 μm; YMC Co. Ltd, Kyoto, Japan).
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3

Chromatographic Characterization of Natural Compounds

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The optical rotations were measured with a Perkin-Elmer 241 polarimeter. The UV spectra were conducted on a Shimadzu UV-2201 spectrometer. ECD spectra were recorded on a JASCO J-815 spectrometer. NMR spectra were recorded on a Bruker ARX-600 spectrometer (600 MHz, Bruker Co., Ltd, Karlsruhe, Germany). LC-MS data were obtained using LTQ Orbitrap velospro (Thermo Fisher Scientific Co., Ltd., Bremen, Germany). High performance liquid chromatography (HPLC) was performed on Agilent 1260 pump (Agilent Technologies Co., Ltd., Palo Alto, CA, USA), coupled with Agilent analytical, semi-preparative or preparative Kromasil Eternity XT-5-C18 columns (250 mm × 4.6 mm and 250 mm × 10 mm, respectively), Kromasil Eternity XT-5-PhenylHexyl columns (250 mm × 4.6 mm and 250 mm × 10 mm, respectively) and Cosmosil 5C18-MSII (250 mm × 4.6 mm and 250 mm × 20 mm, respectively). TLC and preparative TLC were monitored on precoated Silica gel plates (GF254, Qingdao Haiyang Chemical Co., Ltd., Qingdao, China). Column chromatography was performed on Silica gel (200−300 mesh, Qingdao Marine Chemical Ltd., Qingdao, China) and Sephadex LH-20 (Pharmacia Fine Chemical Co., Ltd., Uppsala, Sweden).
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4

Comprehensive Analytical Techniques for Natural Product Characterization

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Optical rotations were recorded on an Anton Paar MCP 200 polarimeter. UV spectra were measured on a Shimadzu UV-2201 spectrometer. ECD spectra were obtained on a Bio-Logic MOS 450 spectrometer. IR spectra were measured on a Bruker IFS-55 spectrometer. 1D and 2D NMR spectra were acquired on Bruker AV-400 or AV-600 NMR spectrometers. Mass spectra were measured on Bruker micrOTOFQ-Q mass spectrometer. Single-crystal X-ray diffraction data was collected on a Rigaku Saturn 724 CCD diffractometer. Column chromatography (CC) were performed with D101 macroporous adsorption resin (D101 MAR), silica gel, ODS, and Sephadex LH-20. Semipreparative HPLC was performed with YMC ODS column, and the HPLC system was equipped with a Shimadzu SPD-20A UV–vis detector and LC-6AD pump.
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5

Comprehensive Spectroscopic Analysis of Natural Products

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1H NMR, 13C NMR, HSQC, and HMBC were recorded on the Bruker-ARX-400 and Bruker-AV-600 NMR with tetramethylsilane (TMS) as internal standard. HRESIMS spectra were measured on a Bruker micrOTOF-Q mass spectrometer. Optical rotations were measured by the JASCO P-2000 polarimeter. UV spectra were recorded on a Shimadzu UV-2201 spectrometer. ECD spectra were measured on the BioLogic MOS 450 AF/CD at room temperature. Multimode Reader were used by a Varioskan Flash. The semi-preparative HPLC was a Shimadzu SPD-20A series equipped with an YMC C18 column (250 × 20 mm, 5 μm, 2 mL/min). Chiral HPLC was a CHIRALPAK IB (250 × 4.6 mm) from Daicel Chiral Technologies Co., Ltd., China. Column chromatography (CC) was conducted on silica gel (100–200 and 200–300 mesh) and preparative and analytical TLC was performed on precoated GF254 plates (Qingdao Haiyang Chemical Co., Ltd., China), octadecyl silane (ODS) (50 µm, YMC Co., Ltd., Kyoto, Japan) and Sephadex LH-20 (GE Healthcare, Uppsala, Sweden). All the organic solvents were purchased from Yuwang and Laibo Chemicals Industries, Ltd., China.
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