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7 protocols using mixis tof qii mass 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

Comprehensive Analytical Techniques for Natural Products

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Optical rotations were measured with an AntonPaar MCP 200 automatic polarimeter. Ultraviolet (UV) spectra were obtained on a UV-2550 spectrophotometer (Shimadzu Corporation, Tokyo, Japan). IR spectra were recorded on a Bruker Tensor 27 FT-IR spectrometer (film). 1D and 2D-NMR spectra were carried out on a Bruker AM-400 and an Avance-500 spectrometer, δ in ppm rel. to TMS, J in Hz. ESIMS and HRESIMS were measured with a Bruker miXis TOF-QII mass spectrometer (Bruker, Fällanden, Switzerland), respectively. Silica gel (100–200 mesh, 300–400 mesh, Qingdao Marine Chemical Ltd., Qingdao, China), Sephadex LH-20 (GE Healthcare Bio-sciences AB, Uppsala, Sweden), and YMC GEL ODS-A (S-50 μm, 12 nm) (YMC Co., Ltd., Kyoto, Japan) were used for column chromatography. Semipreparative HPLC analyses were performed using an ODS column (YMC-ODS-A, 250 × 20 mm, 5 μm). Circular dichroism (CD) spectra were measured on a Chirascan circular dichroism spectrometer (Applied Photophysics Ltd., Leatherhead, UK). MTT assays were analyzed using a microplate reader (BioTek Synergy H1, BioTek Instruments, Inc., Vermont, USA).
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4

Structural Elucidation of Organic Compounds

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UV spectra were measured on a Shimadzu UV-2600 PC spectrophotometer (Shimadzu, Kyoto, Japan). Optical rotations were recorded on a PerkinElmer MPC 500 (Waltham, MA, USA) polarimeter. For ECD spectra, Chirascan circular dichroism spectrometer (Applied Photophysics, Leatherhead Surrey, UK) was used. NMR spectra were acquired by a Bruker Avance spectrometer (Bruker, Billerica, MA, USA) at 700 MHz for 1H and 175 MHz for 13C. HRESIMS spectra were recorded on a Bruker miXis TOF-QII mass spectrometer (Bruker, Billerica, MA, USA). X-ray diffraction intensity data were measured on an Agilent Xcalibur Nova single-crystal diffractometer (Santa Clara, CA, USA) using Cu Kα radiation. TLC and column chromatography were performed on plates precoated with silica gel GF254 (10–40 μm) and over silica gel (200–300 mesh) (Qingdao Marine Chemical Factory, Qingdao, China), respectively. Spots were detected on TLC (Qingdao Marine Chemical Factory, Qingdao, China) under 254 nm UV light. Semi-preparative HPLC was performed using an ODS column (YMC-pack ODS-A, YMC Co., Ltd., Kyoto, Japan, 10 mm × 250 mm, 5 μm).
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5

Characterization of Natural Product Compounds

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Optical rotations were measured on a PerkinElmer MPC 500 (Waltham, MA, USA) polarimeter. UV and ECD spectra were recorded on a Chirascan circular dichroism spectrometer (Applied Photophysics, Leatherhead Surrey, UK). IR spectra were performed on an IR Affinity-1 spectrometer (Shimadzu, Kyoto, Japan). The NMR spectra were obtained on a Bruker Avance spectrometer (Bruker, Billerica, MA, USA) operating at 500 and 700 MHz for 1H NMR and 125 and 175 MHz for 13C NMR, using tetramethylsilane as an internal standard. HRESIMS spectra were collected on a Bruker miXis TOF-QII mass spectrometer (Bruker, Billerica, MA, USA). 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, Qingdao, China) and Sephadex LH-20 (Amersham Biosciences, Uppsala, Sweden), respectively. All solvents employed were of analytical grade (Tianjin Fuyu Chemical and Industry Factory, Tianjin, China). Semipreparative HPLC was carried out using an ODS column (YMC-pack ODS-A, YMC Co., Ltd., 10 × 250 mm, 5 μm, 2.5 mL/min). The artificial sea salt was a commercial product (Guangzhou Haili Aquarium Technology Company, Guangzhou, China).
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6

Characterization of Natural Compounds

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The NMR spectra were obtained on a Bruker Avance spectrometer (Bruker, Billerica, MA, USA) operating at 500 and 700 MHz for 1H NMR, and 125 and 175 MHz for 13C NMR, using tetramethylsilane as an internal standard. High-resolution mass spectra were recorded on a Bruker miXis TOF-QII mass spectrometer (Bruker, Billerica, MA, USA). Optical rotations were measured on a PerkinElmer MPC 500 (Waltham, MA, USA) polarimeter. UV and ECD spectra were recorded on a Chirascan circular dichroism spectrometer (Applied Photophysics, Leatherhead Surrey, UK). The 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, Qingdao, China), Sephadex LH-20 (Amersham Pharmacia Biotech AB, Uppsala, Sweden), and semi-preparative HPLC using an ODS column (YMC-pack ODS-A, YMC Co., Ltd., Kyoto, Japan, 10 mm × 250 mm, 5 µm). All solvents employed were of analytical grade. The sea salt (Guangzhou Haili Aquarium Technology Company, Guangzhou, China) was a commercial product.
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7

Detailed Analytical Techniques for Research

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Optical rotations were measured on a PerkinElmer MPC 500 (PerkinElmer, Waltham, MA, USA) polarimeter. The UV spectra were obtained with a Shimadzu UV-2600 PC spectrometer (Shimadzu, Kyoto, Japan). IR spectra were determined with an IR Affinity-1 spectrometer (Shimadzu, Kyoto, Japan). NMR spectra were recorded on a Bruker Avance spectrometer (Bruker, Billerica, MA, USA) operating at 500 MHz and 700 MHz for 1H NMR and 125 MHz and 175 MHz for 13C NMR used tetramethylsilane as an internal standard. HRESIMS spectra were acquired on a Bruker miXis TOF-QII mass spectrometer (Bruker, Billerica, MA, USA). 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, Qingdao, China), respectively. Spots were detected on TLC (Qingdao Marine Chemical Factory, Qingdao, China) under 254 nm UV light. All solvents employed were analytical grade (Tianjin Fuyu Chemical and Industry Factory, Tianjin, China). Semipreparative HPLC was performed using an ODS column (YMC-pack ODS-A, YMC Co., Ltd., 10 × 250 mm, 5 μm, Kyoto, Japan). Artificial sea salt was a commercial product (Guangzhou Haili Aquarium Technology Company, Guangzhou, China).
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