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10 protocols using 6220 lc tof ms

1

NMR and Mass Spectrometry Analysis

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1H and 13C NMR spectra were recorded using a Bruker Advance 600 spectrometer. Mass spectra were obtained with an Agilent 6220 LC-TOF-MS. Semi-preparative HPLC was performed using Shimadzu LC-10AT pumps coupled with a Sedex 75 Evaporative Light Scattering Detector (ELSD), a Shimadzu SPD M10A diode array detector, a SCL-10A system controller, and a Cogent Bidentate C18 column (250 × 10 mm or 75 × 4.6 mm).
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2

Comprehensive Characterization of Organic Compounds

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Optical rotations were recorded on a JASCO P-2000 polarimeter. IR and UV spectra were measured on MIDAC M-series FTIR and Shimadzu UV-1201 spectrophotometers, respectively. ECD analysis was performed on a JASCO J-810 spectropolarimeter with a 0.1cm cell in MeOH at room temperature under the following conditions: speed 50 nm/min, time constant 1 s, band width 2.0 nm. 1H and 13C NMR spectra were recorded on a Bruker Avance 500 spectrometer in CDCl3 with TMS as internal standard. Mass spectra were obtained on JEOL JMS-HX-110 and Agilent 6220 LC-TOF-MS. Preparative HPLC was performed using Shimadzu LC-10AT pumps coupled with a semi-preparative Varian Dynamax C18 column (5 μm, 250x10 mm), a Shimadzu SPD M10A diode array detector (DAD) and a SCL-10A system controller.
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3

Spectroscopic Characterization of Compounds

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Optical rotations were recorded on a JASCO P-2000 polarimeter. UV and IR spectroscopic data were measured on a Shimadzu UV-1201 spectrophotometer and a MIDAC M-series FTIR spectrophotometer, respectively. ECD spectra were obtained on a JASCO J-815 spectrometer. NMR spectra were recorded in CDCl3 on Bruker Avance 500 or 600 spectrometers. The chemical shifts are given in δ (ppm), and coupling constants (J) are reported in Hz. Mass spectra were obtained on an Agilent 6220 LC-TOF-MS in the positive ion mode.
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4

Spectroscopic Characterization of Organic Compounds

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Optical rotations were recorded on a JASCO P-2000 polarimeter. UV and IR spectroscopic data were measured on a Shimadzu UV-1201 spectrophotometer and a MIDAC M-series FTIR spectrophotometer, respectively. CD spectra were obtained on a JASCO J-815 circular dichroism spectrometer. NMR spectra were recorded in CDCl3 on Bruker Avance 500 or 600 spectrometers. The chemical shifts are given in δ (ppm), and coupling constants (J) are reported in Hz. Mass spectra were obtained on an Agilent 6220 LC-TOF-MS in the positive ion mode.
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5

Comprehensive Analytical Characterization

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Optical rotations were obtained using a JASCO P-2000 polarimeter. ECD spectra were acquired on JASCO J-815 spectrometer. UV spectra were measured on a Shimadzu UV-1201 spectrophotometer. NMR spectra were recorded on a Bruker Avance 500 spectrometer with deuterated solvent as indicated. High resolution electrospray ionization mass spectra (HRESIMS) were obtained on an Agilent 6220 LC-TOF-MS in the positive ion mode. Unless otherwise stated, HPLC was carried out on a Phenomenex Luna 5μ C18 4.6 x 250 mm column at a flow rate of 1 mL/min.
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6

Spectroscopic Analysis of Compound Characterization

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Optical rotations were recorded on a JASCO P-2000 polarimeter. UV spectra were measured on a Shimadzu UV-1201 spectrophotometer. IR spectra were measured on a MIDAC M-series FTIR spectrometer. NMR spectra were recorded in CDCl3 on a Bruker Avance 500 spectrometer. Chemical shifts are given in δ (ppm), and coupling constants are reported in Hz. Mass spectra were obtained on an Agilent 6220 LC-TOF-MS in the positive ion mode. Open column chromatographies were performed using Sephadex LH-20 (3 × 50 cm, 150 g) and C18 (2.5 × 10 cm, 40–63 µm, 45 g). Semi-preparative HPLC was performed on a Shimadzu LC-10AT instrument with a semipreparative C18 Varian Dynamax column (5 µm, 250 ×10 mm).
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7

Analytical Characterization of Compounds

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Optical rotations were recorded on a JASCO P-2000 polarimeter. UV and IR spectroscopic data were measured on a Shimadzu UV-1201 spectrophotometer and a MIDAC M-series FTIR spectrophotometer, respectively. CD spectra were obtained on a JASCO J-815 circular dichroism spectrometer. NMR spectra were recorded in CDCl3 on Bruker Avance 500 or 600 spectrometers. The chemical shifts are given in δ (ppm), and coupling constants (J) are reported in Hz. Mass spectra were obtained on an Agilent 6220 LC-TOF-MS in the positive-ion mode.
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8

Comprehensive Characterization of Isolated Compounds

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IR and UV spectra were measured on MIDAC M-series FTIR and Shimadzu UV-1201 spectrophotometers, respectively. 1D and 2D NMR spectra were recorded on a Bruker Avance 500 spectrometer in CD3OD; chemical shifts are given in δ (ppm), and coupling constants are reported in Hz. Mass spectra were obtained on an Agilent 6220 LC-TOF–MS in the positive ion mode. Optical rotations were recorded on a JASCO P-2000 polarimeter. Open column chromatography was performed using Sephadex LH-20 and silica gel (40–63 µm, Silicycle Co. USA). HPLC was performed on a Shimadzu LC-10AT instrument with a semipreparative C18 (Phenomenex Luna column, 5 µm, 250 Χ10 mm), a Shimadzu SPD M10A diode array detector, and a SCL-10A system controller. All isolated compounds were purified to 95 % purity or better, as judged by HPLC (both UV and ELSD detection) before determining bioactivity.
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9

Characterization of Chemical Compounds

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Optical rotations were recorded on a JASCO P-2000 polarimeter. UV
spectroscopic data were measured on a Shimadzu UV-1201 spectrophotometer. NMR
spectra were recorded in CDCl3 on Bruker Avance 500 or 600
spectrometers. Chemical shifts are given in δ (ppm), and
coupling constants (J) are reported in Hz. Mass spectra were
obtained on an Agilent 6220 LC-TOF-MS in the positive ion mode.
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10

Analytical Techniques for Natural Product Isolation

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Optical rotations were recorded on a JASCO P-2000 polarimeter. UV spectra were measured on a Shimadzu UV-1201 spectrophotometer. IR spectra were measured on a MIDAC M-series FTIR spectrometer. NMR spectra were recorded in CDCl3 on a Bruker Avance 500 spectrometer. Chemical shifts are given in δ (ppm), and coupling constants are reported in Hz. Mass spectra were obtained on an Agilent 6220 LC-TOF-MS in the positive ion mode. Open column chromatographies were performed using Sephadex LH-20 (I.D.×L 3×50 cm) and Si-diol (I.D.×L 2.5 ×35 cm, 40–63 µm). HPLC separation was performed on a Shimadzu LC-10AT instrument with a semipreparative C18 Phenomenex Luna column (5 µm, 250 × 10 mm).
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