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11 protocols using uv 2600 pc spectrometer

1

Analytical Characterization of Natural Products

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Semipreparative HPLC (Agilent Technologies, 1260 Infinity II series) was performed using an ODS column (YMC-pack ODS-A, 10 mm × 250 mm, 5 μm). Column chromatography (CC) was performed over silica gel (200–300 mesh; Qingdao Marine Chemical Group Co., Qingdao, China) and Sephadex LH-20 (Amersham Biosciences Inc., Piscataway, NJ, USA) and octadecylsilyl silica gel (YMC Co., Ltd., Kyoto, Japan; 50 μm), respectively. Spots were detected on TLC (Qingdao Marine Chemical Factory, Qingdao, China) under 254 nm UV light. The NMR spectra were obtained on a Bruker Avance-600 MHz spectrometer (Bruker, Billerica, MA, USA) with tetramethylsilane as an internal standard. HR-ESI-MS spectra were recorded on a Bruker miXis TOF-QII mass spectrometer (Bruker, Billerica, MA, USA). Optical rotations were determined with a Perkin Elmer MPC 500 (Waltham, MA, USA) polarimeter. The UV, IR, and ECD spectra were recorded on a Shimadzu UV-2600 PC spectrometer (Shimadzu, Kyoto, Japan), an IR Affinity-1 spectrometer (Shimadzu, Kyoto, Japan), and a Chirascan circular dichroism spectrometer (Applied Photophysics, Leatherhead Surrey, UK), respectively. The artificial sea salt was a commercial product (Guangzhou Haili Aquarium Technology Company, Guangzhou, China). Cells were disrupted using a high pressure homogenizer NanoGenizer (Genizer LLC, Irvine, CA, USA).
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2

Spectroscopic Analysis of Natural Compounds

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Optical rotations were measured on a PerkinElmer MPC 500 (Waltham) polarimeter. The UV, IR, and CD spectra were recorded on a Shimadzu UV-2600 PC spectrometer (Shimadzu), an IR Affinity-1 spectrometer (Shimadzu), and a Chirascan circular dichroism spectrometer (Applied Photophysics), respectively. NMR spectra were recorded on a Bruker Avance spectrometer (Bruker) operating at 500 and 700 MHz for 1H NMR and 125 and 175 MHz for 13C NMR that used tetramethylsilane as an internal standard. High resolution electrospray ionization mass spectroscopy (HRESIMS) spectra were acquired on a Bruker miXis TOF-QII mass spectrometer (Bruker). Column chromatography was performed over silica gel (200–300 mesh) (Qingdao Marine Chemical Factory). Spots were detected on TLC (Qingdao Marine Chemical Factory) under 254-nm UV light. All solvents employed were analytical grade (Tianjin Fuyu Chemical and Industry Factory). Semipreparative HPLC was performed using an octadecylsilyl (ODS) column (YMC-pack ODS-A, YMC Co., Ltd., 10 mm × 250 mm, 5 μm). Artificial sea salt was a commercial product (Guangzhou Haili Aquarium Technology Company).
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3

Analytical Techniques for Compound Characterization

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NMR spectra were obtained
on a Bruker Avance spectrometer (Bruker) operating at 500 and 700
MHz for 1H NMR 125 and 175 MHz and for 13C NMR
with TMS as the internal reference. HRESIMS spectra data were measured
with a Bruker maXis quadrupole-time-of-flight mass spectrometer (Bruker).
Optical rotations were recorded on a PerkinElmer MPC 500 (Waltham)
polarimeter. UV spectra were acquired using a Shimadzu UV-2600 PC
spectrometer (Shimadzu). ECD spectra were measured with a Chirascan
circular dichroism spectrometer (Applied Photophysics). X-ray diffraction
intensity data were collected on a CrysAlis PRO CCD area detector
diffractometer with graphite-monochromated Cu Kα radiation (λ
= 1.54184). TLC and column chromatography (CC) were performed on plates
precoated with silica gel GF254 (10–40 μm) and over silica
gel (200–300 mesh) (Qingdao Marine Chemical Factory) and Sephadex
LH-20 (Amersham Biosciences), respectively. Spots were detected on
TLC (Qingdao Marine Chemical Factory) under a 254 nm UV light. All
solvents employed were of analytical grade (Tianjin Fuyu Chemical
and Industry Factory). Semipreparative HPLC was carried out using
an octadecyl-silica (ODS) column (YMC-pack ODS-A, YMC Co. Ltd., 10
× 250 mm, 5 μm, 2 mL/min). The artificial sea salt was
a commercial product (Guangzhou Haili Aquarium Technology Company).
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4

Analytical Techniques for Natural Product Characterization

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Optical rotations were measured using an (Anton) MCP500 polarimeter. HRESIMS were used for a Bruker maXis TOF-Q mass spectrometer, while infrared spectra were acquired on a Shimadzu IR spectrometer. NMR spectra were measured on Bruker spectrometer. The UV spectra were carried out on a Shimadzu UV-2600 PC spectrometer. Open chromatography column was performed on silica gel (100-300 mesh, Qingdao, China), YMC ODS-A (S-50 μm, 12 nm) (YMC Co., Ltd., Kyoto, Japan). HPLC was accomplished using ODS column (YMC-5μm, ODS-A) Sephadex LH-20 (GE, Sweden). The RAW 264.7 cells were obtained from the Chinese Academy of Sciences (Shanghai, China)
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5

Analytical Techniques for Natural Product Characterization

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The UV spectrum was recorded on a Shimadzu UV-2600 PC spectrometer (Shimadzu, Beijing, China). The IR spectrum was obtained using an IR Affinity-1 spectrometer (Shimadzu). Optical rotations were determined with an Anton Paar MPC 500 polarimeter. HRESIMS spectra were recorded with a Bruker maXis Q-TOF mass spectrometer. The NMR spectra were recorded on a Bruker Avance-500 spectrometer (Bruker BioSpin International AG, Fällanden, Switzerland), and chemical shifts were recorded as δ-values. Semipreparative high-performance liquid chromatography (HPLC) was performed on the Hitachi Primaide with a DAD detector, using an ODS column (YMC-pack ODS-A, 10 × 250 mm, 5 μm). Thin-layer chromatography analysis (TLC) and column chromatography (CC) were carried out on plates precoated with silica gel GF254 (10–40 μm) and over silica gel (200–300 mesh) (Qingdao Marine Chemical Factory, Qingdao, China) and Sephadex LH-20 (Amersham Biosciences, Uppsala, Sweden), respectively. Spots were detected on TLC (Qingdao Marine Chemical Factory) under 254 nm UV light. All solvents employed were of analytical grade (Tianjin Fuyu Chemical and Industry Factory, Tianjin, China).
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6

Comprehensive Analytical Characterization Protocol

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Optical rotations were determined using an AntonPaar MCP500 polarimeter. UV spectra were measured with a Shimadzu UV-2600 PC spectrometer. IR spectra were recorded on a Shimadzu IR Affinity-1 spectrometer with KBr pellets. 1D and 2D NMR spectra were collected on a Bruker DRX-500 spectrometer, δ in ppm rel. to TMS, J in Hz. HRESIMS were performed using a Bruker maXis TOF-Q mass spectrometer (Bruker, Daltonics, Billerica, MA, USA). Silica gel (100–200 mesh, 200–300 mesh, Qingdao Marine Chemical Ltd., Qingdao, China), Sephadex LH-20 (GE Healthcare Bio-sciences AB, Uppsala, Sweden), YMC*GEL ODS-A (S-50 μm, 12 nm) (YMC Co., Ltd., Kyoto, Japan) were used for column chromatography. Semipreparative HPLC was performed using an ODS column (YMC-ODS-A, 250 × 10 mm, 5 μm). CD spectra were measured on a Biologic MOS-450 spectra polarimeter (Biologic Science, Claix, France). ECD spectra were measured with a Chirascan circular dichroism spectrometer (Applied Photophysics). MTT and antimicrobial assays were analyzed using a microplate reader (BioTek Synergy H1, BioTek Instruments, Inc., Winooski, VT, USA).
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7

Spectroscopic Analysis of Natural Compounds

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The UV and IR spectra were recorded on a Shimadzu UV-2600 PC spectrometer (Shimadzu, Beijing, China) and an IR Affinity-1 spectrometer (Shimadzu), respectively. Optical rotations were determined with an Anton Paar MPC 500 (Anton, Graz, Austria) polarimeter. High resolution electrospray ionization mass spectroscopy (HRESIMS) spectra were acquired on a Bruker maXis Q-TOF mass spectrometer (Bruker BioSpin International AG, Fällanden, Swizerland). The NMR spectra were recorded on a Bruker Avance spectrometer (Bruker) operating at 500 and 700 MHz for 1H NMR and 125 and 175 MHz for 13C NMR that used tetramethylsilane as an internal standard. Semipreparative high-performance liquid chromatography (HPLC) was performed on the Hitachi Primaide with a DAD detector, using an ODS column (YMC-pack ODS-A, 10 × 250 mm, 5 μm). Column chromatography was performed over silica gel (200–300 mesh) (Qingdao Marine Chemical Factory, Qingdao, China). Spots were detected on TLC (Qingdao Marine Chemical Factory) under 254 nm UV light. All solvents employed were of analytical grade (Tianjin Fuyu Chemical and Industry Factory, Tianjin, China).
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8

Spectroscopic Analysis of Natural Compounds

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The optical rotations were achieved using a PerkinElmer MPC 500 (Waltham) polarimeter. The UV spectra were recorded on a Shimadzu UV-2600 PC spectrometer (Shimadzu). The ECD spectra were measured using a Chirascan circular dichroism spectrometer (Applied Photophysics). The IR spectra were measured on an IR Affinity-1 spectrometer (Shimadzu, Beijing, China). The NMR spectra were obtained on a Bruker Avance spectrometer (Bruker) operating at 700 MHz for 1H NMR and 175 MHz for 13C NMR, using tetramethylsilane as an internal standard. The HRESIMS spectra were collected on a Bruker mix TOF-QII mass spectrometer (Bruker). The TLC and column chromatography (CC) were performed on plates pre-coated with GF254 silica gel (10−40 μm) and over silica gel (200−300 mesh) (Qingdao Marine Chemical Factory) and a Sephadex LH-20 (Amersham Biosciences), respectively. All of the solvents employed were of analytical grade (Tianjin Fuyu Chemical and Industry Factory). The semipreparative HPLC was performed on an HPLC (Hitachi-L2130, diode array detector, Hitachi L-2455, Tokyo, Japan) using a Phenomenex ODS column (250 mm × 10.0 mm i.d., 5 μm; Phenomenex, Torrance, CA, USA). The artificial sea salt was a commercial product (Guangzhou Haili Aquarium Technology Company, Guangzhou, China).
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9

Characterization of Organic Compounds

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All solvents used in isolation were of analytical grade and obtained from Sinopharm group. Optical rotations: MPC 500 (Waltham) polarimeter (PerkinElmer Ltd., Waltham, MA, USA). Electronic circular dichroism (ECD) spectra: (Applied Photophysics Ltd., Leatherhead, UK). UV spectra: Shimadzu UV-2600 PC spectrometer (Shimadzu, J.P.). NMR spectra: Bruker 600 MHz spectrometer using TMS as standard (Bruker BioSpin Group, Rheinstetten, Germany). HR-ESI-MS spectra: Thermo Q-T of Micromass spectrometer (Thermo Electron Corporation, Waltham, MA, USA). Preparative HPLC: Waters 2525 pump, Waters 2998 DAD detector, and Waters 2767 Autopurifcation System (Waters Corporation, Milford, MA, USA).
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10

Instrumental Analysis of Molecular Compounds

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Optical rotations were measured on an AntonPaar MCP500 polarimeter. IR spectra were performed on a Shimadzu IR spectrometer with KBr disk. HRESIMS were used for a Bruker maXis TOF-Q mass spectrometer. Bruker DRX-500 spectrometer was used to measure the NMR spectra. The UV spectra were recorded on a Shimadzu UV-2600 PC spectrometer. Silica gel (100–200 mesh, 200–300 mesh, Qingdao, China), YMC*GEL ODS-A (S-50 μm, 12 nm) (YMC Co., Ltd., Kyoto, Japan), Sephadex LH-20 (GE, Sweden) were used for column chromatography. Semipreparative HPLC was used for ODS column (YMC-ODS-A). CD spectra were performed on a Biologic MOS-450 spectra polarimeter.
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