Dibenzyl dimer compound and method and application for extracting and separating compound from dendrobium stems
A technology of bibenzyl dimer and Dendrobium nobile can be used in organic chemistry, drug combination, antineoplastic drugs, etc., and can solve problems such as complex and diverse chemical components
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Embodiment 1
[0027] The method for extracting and separating the above-mentioned bibenzyl dimer compounds from Dendrobium nobile of the present invention comprises the following steps:
[0028] 1) Take 5.0 kg of dried stems of Dendrobium nobile, after pulverization, reflux extraction with 95% ethanol for 4 times, combine the extracts for 4 times, and concentrate the extracts under reduced pressure to obtain 0.5 kg of ethanol extract;
[0029] 2) Disperse the ethanol extract in step 1) with 0.5% hydrochloric acid aqueous solution and stir thoroughly, then filter to obtain the acid-water insoluble matter. The acid water-insoluble matter was sequentially extracted 4 times with petroleum ether, petroleum ether: ethyl acetate 1:1 volume, and ethyl acetate respectively, and concentrated under reduced pressure to obtain extracts of various parts;
[0030] 3) Separate the extract from the ethyl acetate part in step 2) by silica gel column chromatography, and wash with petroleum ether-ethyl acetate...
Embodiment 2
[0033] Embodiment 2: The difference with Embodiment 1 is that
[0034] The concentration of aqueous ethanol used for reflux extraction in step 1) is 85% for reflux extraction twice; step 2) for extraction twice; step 4) for methanol with a concentration of 95%; step 5) for acetonitrile with a concentration of 50%, The detection wavelength is 240nm, 260nm. All the other steps are the same as in Example 1, and the beneficial effects described in the present invention can also be obtained.
Embodiment 3
[0035] Embodiment 3: The difference with Embodiment 1 is that
[0036] The concentration of aqueous ethanol used for reflux extraction in step 1) is 70% reflux extraction for 4 times; step 2) for extraction 4 times; step 4) with a concentration of 90% methanol; step 5) with a concentration of 70% acetonitrile, The detection wavelength is 240nm, 260nm. All the other steps are the same as in Example 1, and the beneficial effects described in the present invention can also be obtained.
[0037] The present invention carries out the condition of TLC identification: developer is sherwood oil-ethyl acetate system and dichloromethane-methanol system, chromogenic agent a: observe fluorescence under ultraviolet lamp (254nm); chromogenic agent b: iodine cylinder color development .
[0038] Structural identification: The spectroscopic techniques used mainly include nuclear magnetic resonance spectroscopy ( 1 H-NMR, 13 C-NMR, HSQC, HMBC) and mass spectrometry (HR-ESI-MS) identified t...
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