Compound, and preparation method and application thereof
A technology for separation and purification of compounds, applied in biochemical equipment and methods, methods based on microorganisms, microorganisms, etc., can solve the problem of few studies on metabolites, and achieve the effect of extensive development and application prospects
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Embodiment 1
[0026] Embodiment 1, the preparation of compound
[0027] 1.1. Fermentation
[0028] The Xylaria sp. strain HCCB03890 was solidly fermented with a rice medium, the fermentation temperature was 27-30° C., and the fermentation time was 28-35 days.
[0029] 1.2. Separation and purification
[0030] The fermented rice product obtained in 1.1 was extracted with ethyl acetate, and then separated on a column with vacuum silica gel, eluted with ethyl acetate, and concentrated to obtain a crude sample.
[0031] Then, use Diane P680 liquid chromatography (preparative column YMC-ODS C-18, 5 μm, 20 × 250mm) to separate (0-40min with 20%-100% methanol elution, flow rate 8ml / min), to obtain crude Sample.
[0032] The obtained crude sample was further separated by semi-preparative liquid chromatography (the semi-preparative column was Agilent ZORBAX SB-C18, 5 μm, 9.4mm × 250mm) (0-25min with 18% acetonitrile isocratic elution, 25-45min with 18% ~35% acetonitrile gradient elution, flow ra...
Embodiment 2
[0033] Example 2 , Compound structure identification
[0034] The compound obtained in Example 1 is detected by positive ion electrospray mass spectrometry, and the spectrum is as follows figure 1 As shown, it shows that the quasi-molecular ion peak is: m / z 357.1186[M+H] + , the corresponding molecular formula is C 16 h 21 o 9 , adopt Bruker Avance II-400 type superconducting nuclear magnetic resonance instrument to measure the hydrogen spectrum of sample ( figure 2 ), carbon spectrum ( image 3 ) and NMR (MeOH-d 6 , 400MHz), and the NMR data are shown in Table 1.
[0035] Table 1. NMR data of compounds
[0036]
[0037]
[0038] Through analysis, the ownership of all carbon atoms and hydrogen atoms of the compound was determined, and the structure of the compound was obtained as follows:
[0039]
[0040] The molecular formula of this compound is C 16 h 20 o 9 , the molecular weight is 356, the chemical Chinese name is 2-methyl-7-(3,4,5-trihydroxy-6(hyd...
Embodiment 3
[0043] Embodiment 3, the biological activity of compound
[0044] The cells used in this example (all derived from the Cell Bank of the Type Culture Collection Committee of the Chinese Academy of Sciences, and the Cell Resource Center of the Shanghai Institutes for Biological Sciences, the Chinese Academy of Sciences) are: A549 (human non-small cell lung cancer cells), MDA-MB-231 ( human breast cancer cells), PANC-1 (human pancreatic cancer cells).
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