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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

Active Publication Date: 2009-07-01
黑龙江天宏药业股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the basic research on its pharmacodynamic substances has not been carried out in depth, and the literature reports mostly stay on the pharmacological effects of its crude extract and lack the antitumor effect of its active ingredients (Ji Yubin, Ma Hongtu, Yang Bo, Ji Chenfeng. Bei Qinglongyi Research on anti-tumor effect of different extraction parts. Chinese Herbal Medicine, 2004, 35(10): 1145-1147), but the active ingredients of the existing Beiqinglongyi extract are not clear, and the quantitative indicators are lacking, which makes it difficult to further elucidate the pharmacological mechanism

Method used

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  • Extract of immature exocarp of Juglans mandshurica Maxim., preparation method and medical use
  • Extract of immature exocarp of Juglans mandshurica Maxim., preparation method and medical use
  • Extract of immature exocarp of Juglans mandshurica Maxim., preparation method and medical use

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Experimental program
Comparison scheme
Effect test

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).

[0...

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PUM

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Abstract

The invention provides a north Qinglongyi extract, preparation method and medicinal use. The active ingredient of the existing North Qinglongyi extract is not clear lacks of quantitative index, therefore the mechanism of pharmacological effects is difficulty to expatiate. The anti-tumor active ingredient of the existing North Qinglongyi extract is prepared using alcohol extraction method combined with macroporous resin and gel chromatography technique. The north Qinglongyi extract comprises compound of general formula (I) with more than 70 percent, the compound of structural formula is described above. This invention is applied to the medical field.

Description

Technical field: [0001] The invention relates to a preparation method of an extract mainly composed of Qinglongyisu A, a new compound isolated from Beiqinglongyi, and its use in the preparation of antitumor drugs. Background technique: [0002] Cancer is a serious disease that threatens human life. Therefore, research on anticancer drugs has always been a hot spot in the world. Compared with chemical drugs, traditional Chinese medicine anti-tumor is unique in improving immunity and reducing mutagenic toxicity. Therefore, it is necessary to find anti-tumor traditional Chinese medicine with definite curative effect from the motherland's treasure house of medicine, clarify the material basis of its efficacy, and then develop a high-efficiency and low-toxicity drug. The new drug has become the focus of many years of research in the field of traditional Chinese medicine. [0003] Beiqinglongyi is the immature fruit of Juglans Mandshurica MAXIM., a plant of the family Juglans. It...

Claims

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Application Information

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IPC IPC(8): A61K36/52A61P35/00C07C62/38C07C51/47A61K131/00
Inventor 刘丽娟李巍
Owner 黑龙江天宏药业股份有限公司
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