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6 protocols using mat95xp high resolution mass spectrometer

1

Spectroscopic Analysis of Compounds

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Optical rotations were measured on a JASCO P-1020 digital polarimeter. UV spectra were recorded on a HITACHI UH 5300 UV spectrophotometer. ECD data were acquired on a J-815-150S Circular Dichroism spectrometer. IR spectra were recorded on a Nicolet-Nexus-470 spectrometer using KBr pellets. NMR spectra were acquired by a JEOL JEM-ECP NMR spectrometer (500 MHz for 1H and 125 MHz for 13C), using TMS as an internal standard. HRESIMS were measured on Agilent 1290 Infinity II UHPLC/6530 Q-TOF MS for compounds 1 and 2, and Thermo MAT95XP high resolution mass spectrometer for compound 3. Samples were analyzed and prepared on a Hitachi L-2000 HPLC system coupled with a Hitachi L-2455 photodiode array detector and using a semi-prepared C18 column (Kromasil 250 × 10 mm, 5 μm). Silica gel (Qing Dao Hai Yang Chemical Group Co.; 300–400 mesh) and Sephadex LH-20 (Amersham Biosciences) were used for column chromatography (CC). Precoated silica gel plates (Yan Tai Zi Fu Chemical Group Co.; G60, F-254) were used for thin-layer chromatography.
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2

Spectroscopic Analysis of Natural Compounds

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The melting point was measured on an X-5 melting point instrument and was uncorrected. Optical rotations were obtained with a PerkinElmer 341 automatic polarimeter. UV spectra were recorded with MeOH as the solvent using a Shimadzu UV-2450 spectrophotometer. IR spectra were determined on a Bruker Tensor 37 infrared spectrophotometer with KBr pellets. The 1D and 2D NMR spectra were obtained on a Bruker AM-400 NMR spectrometer with tetramethylsilane (TMS) as an internal reference. HREIMS were measured on a Thermo MAT95XP high-resolution mass spectrometer, and EIMS on a Thermo DSQ EIMS spectrometer. HRESIMS were acquired on a Shimadzu LCMS-IT-TOF instrument, and the ESIMS on an Agilent 1200 series LC-MS/MS system. RP-C18 silica gel (Fuji, 40–75 μm), MCI gel (CHP20P, 75–150 μm, Mitsubishi Chemical Corporation, Tokyo, Japan), silica gel (200–300 Mesh Marine Chemical Ltd., Qingdao, People’s Republic of China), and Sephadex LH-20 (GE Healthcare Bio-Sciences AB, Sweden) were used for column chromatography (CC). Semipreparative HPLC separations were carried out on a LC-20AT Shimadzu liquid chromatography system with a YMC-Pack ODS-A column and an Agilent SB-C18 column (250 × 9.4 mm, 5 μm) connected with an SPD-M20A diode array detector.
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3

Characterization of Natural Compounds

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Optical rotations were measured on an MCP 300 (Anton Paar) polarimeter at 28 °C. Melting points were measured on an X-4 micromelting point apparatus. IR spectrum was recorded on a Nicolet Nexus 670 in KBr discs and UV spectrum was recorded in MeOH solution on a PERSEE TU-1900 spectrophotometer. ECD data were obtained on a Chirascan CD spectrometer (Applied Photophysics). NMR spectra were recorded on a Bruker Avance 400 MHz spectrometer with tetramethylsilane as internal standard. EIMS on a DSQ EI-mass spectrometer (Thermo) and HREIMS data were measured on a MAT9-5XP high-resolution mass spectrometer (Thermo). Sephadex LH-20 and Silica gel (100-200 mesh, 200-300 mesh, Qing dao Marine Chemical Factory, Qingdao, Qingdao, People's Republic of China) were used for column chromatography. Analytical thin layer chromatography (TLC) was performed with GF254 plates (Qingdao Marine Chemical Factory). The reagents in the research process were analytical (Guangzhou chemical reagent factory). Single-crystal data were carried out on an Agilent Gemini Ultra diffractometer (Cu Kα radiation).
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4

Spectroscopic Analysis of Organic Compounds

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Optical rotations were measured on a JASCO P-1020 digital polarimeter. CD spectra were recorded on a MOS-450 spectrometer. IR spectra were recorded on a Bruker EQUINOX 55 spectrometer using KBr pellets. 1H and 13C spectra were recorded on a JEOL Eclips-600 spectrometer at 600 MHz for 1H and 150 MHz for 13C in DMSO-d6. Chemical shifts δ are reported in ppm, using TMS as internal standard and coupling constants (J) are in Hz. HRESIMS were measured on a Thermo MAT95XP High Resolution mass spectrometer. Silica gel (Qing Dao Hai Yang Chemical Group Co., Qingdao, China; 200–300 mesh), octadecylsilyl silica gel (Unicorn; 45–60 μm) and Sephadex LH-20 (Amersham Biosciences, Uppsala, Sweden) were used for column chromatography (CC). Precoated silica gel plates (G60, F-254, Yan Tai Zi Fu Chemical Group Co., Qingdao, China) were used for thin layer chromatography (TLC). Semi-preparative HPLC was performed on a Waters 1525 system using a semi-preparative C18 (Kromasil 7 μm, 10 × 250 mm) column coupled with a Waters 2996 photodiode array detector, at a flow rate of 2.0 mL/min.
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5

Spectroscopic Analysis of Novel Compounds

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Melting points were determined on a Fisher-Johns hot-stage apparatus and were uncorrected. UV data were measured on a UV-240 spectrophotometer (Shimadzu, Beijing, China). HRMS (ESI) were determined with a Q-TOF high-resolution mass spectrometer (Waters). HREIMS data were measured on a MAT95XP high-resolution mass spectrometer (Thermo). IR spectrum was recorded using Bruker Vector spectrophotometer 22. Optical rotation was recorded using a an MCP300 (Anton Paar, Shanghai, China). CD data were recorded with a J-810 spectropolarimeter (JASCO, Tokyo, Japan). The NMR data were recorded on a Bruker Avance 600 spectrometer (Bruker, Beijing, China) at 600 MHz for 1H and 125 MHz for 13C, respectively. All chemical shifts (δ) are given in ppm with reference to TMS, and coupling constants (J) are given in Hz. Column chromatography (CC) was carried out on silica gel (200–300 mesh, Marine Chemical Factory, Qingdao, China) and sephadex LH-20 (Amersham Pharmacia, Piscataway, NJ, USA). Solvents were distilled prior to use. Semipreparative HPLC was performed on a Waters Breeze HPLC system using a Phenomenex Luna (Phenomenex, Torrance, CA, USA) C18 column (250 × 10 mm, 5 μm), flow rate, 2.0 mL/min.
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6

Spectroscopic Analysis of Natural Compounds

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Optical rotations were measured on a WZ-1 polarimeter (Shimadzu, Tokyo, Japan) at 25°C. Ultraviolet spectra (UV) spectra were measured with a Unico UV/vis 2802 PCS spectrophotometer (Unico Instrument Co., Ltd., Shanghai, China) . CD spectra were recorded on a JASCO J-810 circular dichroism spectrometer (Jasco, Tokyo, Japan).
NMR experiments were conducted on a JEOL JEM-ECP NMR spectrometer (500 MHz for 1 H and 125 MHz for 13 C). HRESIMS was performed on a Thermo MAT95XP High Resolution mass spectrometer. High-performance liquid chromatography (HPLC) separation was carried out on a Hitachi L-2000 prep-HPLC system equippedwith Hitachi L-2455 photodiode array detector (Hitachi, Tokyo, Japan). The HPLC column used was a 150 mm × 7.8 mm i.d., 7 μm, Kromasil C18 column (Akzo Nobel, Amsterdam, Holland). Silica gel (100-200 and 200-300 mesh) , octadecylsilyl silica gel (45-60 μm) and Sephadex LH-20 were used for column chromatography. TLC silica gel GF 254 plates were used for thin layer chromatography (TLC).
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