Extract of immature exocarp of Juglans mandshurica Maxim., preparation method and medical use
A kind of extract, the technology of Qinglong, which is applied in the direction of medical formula, drug combination, anti-tumor drug, etc., can solve the problems of retention, lack of anti-tumor effect research, and unclear active ingredients, etc., to achieve H22 growth inhibition, excellent anti-cancer activity, The effect of novel structure
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Embodiment 1
[0024] Beiqinglongyi extract, the compound content containing general formula (I) is greater than 70%, and the structural formula of this compound is:
[0025]
[0026] The preparation of a kind of Beiqinglongyi extract is to take fresh Beiqinglongyi and soak it with ethanol for extraction, concentrate the extract, add water to disperse the concentrated solution, take the supernatant after centrifugation, pass the supernatant through the macroporous adsorption resin, and The adsorption resin is eluted with ethanol, the eluent is concentrated and filtered, and injected into dextran gel, the 40% ethanol eluate is collected, concentrated to dryness, and the content of Qinglongyisu A in the dried product is greater than 70%.
[0027] The preparation of a kind of Beiqinglongyi extract is that the fresh Beiqinglongyi is soaked and extracted with ethanol, which is to soak the fresh Beiqinglongyi with 8 to 10 times the amount of 75% to 95% ethanol for one week, extract three times....
Embodiment 2
[0034] Preparation of compound (I)
[0035] Material source: Beiqinglongyi is the immature fruit of Juglans Mandshurica MAXIM., which was collected in Wuchang County, Heilongjiang Province in mid-July. The plant specimens are collected in the Herbarium of Traditional Chinese Medicine, Heilongjiang Provincial Institute for Drug Control.
[0036]Extraction and separation: Soak fresh Beiqinglongyi with 75% ethanol for one week, extract three times in total, combine the extracts, concentrate under reduced pressure, and concentrate to a concentrated solution with a relative density of 1.10-1.14 (50°C), add 10 times the amount of the concentrated solution Disperse with water, centrifuge, take the supernatant, inject it into the treated macroporous adsorption resin (the ratio of concentrated solution to resin is 1:50), flow rate 10ml / min, wash with 3 times the column bed volume, 5 times Wash with 30% ethanol of column bed volume, collect 30% ethanol eluate, eluate is evaporated to dr...
Embodiment 3
[0038] Structure Determination of Compound (I)
[0039] Structure determination
[0040] UV spectrum was measured with Shimadzu UV-160 spectrophotometer, infrared spectrum was measured with JASCOFT / IR-300E (KBr tablet) spectrophotometer, optical rotation was measured with JASCO DIP-370digital polarimeter, ESI-MS was measured with LCQ mass analyzer, and JEOL Mstation spectrometer measures HR-FAB-MS, 1 H-and 13 C-NMR spectrum uses JEOL ECP-500 spectrometer, TMS as internal standard.
[0041] The physicochemical property of compound (I):
[0042] Compound (I) is an amorphous powder. IR(KBr)ν max : 3414, 2924, 2857, 2372, 1618, 1456, 1391, 1263, 1116, 618. UV(MeOH)λ max (logε): 209nm (3.52), 263nm (3.92), 344nm (4.41). [α] D 25 -21° (c=0.1, MeOH). 1 H-NMR (500MHz, CD 3 OD) and 13 C-NMR (125MHz, CD 3 OD) spectrum data are shown in Table 1. ESI-MS (positive) m / z 379.1[M+Na]; HR-FAB-MS (positive) m / z 379.1002[M+Na] (calculated value C 19 h 16 o 7 Na 379.1005).
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