Shixiantao extract, its preparation method and its application in the preparation of medicine

A technology of fairy peach and medicine, applied in the field of Shixiantao extract, its preparation and its application in the preparation of medicines, to achieve the effects of increasing radiosensitivity, reducing tumor growth, and having no cytotoxicity

Inactive Publication Date: 2012-02-22
NIHON UNIVERSITY +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] So far, there have been few studies on Shixiantao, and no studies and reports have been found on the exact active ingredients of Shixiantao

Method used

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  • Shixiantao extract, its preparation method and its application in the preparation of medicine
  • Shixiantao extract, its preparation method and its application in the preparation of medicine
  • Shixiantao extract, its preparation method and its application in the preparation of medicine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Example 1: Preparation of extract and determination of compound structure

[0035]10.2Kg of the whole herb of Shixiantao was crushed, 55 liters of 70% ethanol (ethanol: water = 7: 3) was added, and left at room temperature for 12 hours. After about an hour of heating cycle, the extract is obtained. The extracted Shixiantao powder was extracted again with 55 L of 70% ethanol, and mixed with the extract obtained before. This solution was concentrated under reduced pressure at 40° C. to obtain 789.6 g of a brown powder extract.

[0036] Take 785.1g of the powder extract and dissolve it in 3L of water, then extract with 2L each of n-hexane, ethyl acetate and butanol in sequence. The extract of ethyl acetate was selected and concentrated under reduced pressure at 40° C. to obtain 220.1 g of brown powder.

[0037] Take 200.4 g of the ethyl acetate extract and separate it with a silica gel column (Wako gel C-300, 6.5×25 cm). Use n-hexane:ethyl acetate=100:0, 95:5, 90:10, 8...

Embodiment 2

[0041] Embodiment 2: Determine the structure of physical and chemical parameters and compounds

[0042] The properties and molecular weight of compounds (1)-(10) are shown in Table 1; compounds (1) and (2) 13 C-NMR, 1 The data of H-NMR is shown in Table 2, compound (3), (4), (5), (6), (7), (8), (9), (10) 13 C-NMR data are shown in Table 3, 1 H-NMR data are shown in Table 4.

[0043] And finally determined the structural formula of the relevant compound by the above data.

[0044] Table 1:

[0045] 1 2 3 4 5 Properties EI-MS(m / z) HR-EI-MS(m / z) Measured value Calculated value Molecular weight Molecular formula UVλ max MeOH nm(logε) IRV max KBr cm -1 Red Oil 242 242.09453 242.09428 242.1 C 15 h 14 o 3 208(4.40) 3311, 2929 2828, 1588 1493, 1193 1156, 966 Red Oil 242 242.09446 242.09443 242.1 C 15 h 14 o 3 208(4.42) 3389, 2935 2840, 1591 1454, 1153 1056, 957 White needle crystal 242 242.09430 242.09428 242.1 C 15 h ...

Embodiment 3

[0057] Embodiment 3: Inhibition of NO production test

[0058] The inhibitory effect on NO production (the effect of inhibiting NO production) of macrophages stimulated by interferon-r and lipopolysaccharide was determined by the following experimental method. And the inhibitory effect of NO production was evaluated based on the IC50 (μm) of the inhibitory effect.

[0059] Materials used:

[0060] RAW 264.7 cells (Dainippon Pharmaceutical Co., Ltd.)

[0061] N-1-naphthaleneethylenediamine hydrochloride (1g Wako Pure Chemical Industries)

[0062] Sulfa (500g Wako Pure Chemical Industries)

[0063] Ham's F12 Medium (SIGMA N488 500mL)

[0064] IFN-γ (Geneyme / Techne 100μg)

[0065] Lipopolysaccharide (LPS, 055:B5 10mg, Sigma)

[0066] Phosphoric acid (500ml Wako Pure Chemical Industries)

[0067] DMSO (500ml Wako Pure Chemical Industries)

[0068] 96-well microtiter plate (50 / box Sumitomo Bakelite, trade name [8096R])

[0069] experiment method:

[0070] RAW264.7 cells,...

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Abstract

The present invention relates to the extract of shixiantao, its preparation method and its application in the preparation of medicine. The method for extracting the active compound from shixiantao comprises the following steps: 1) the extract of shixiantao is concentrated under reduced pressure and dried with ethanol to obtain extract; 2) sequentially extracting the extract with n-ethane, ethyl acetate and n-butanol; 3) eluting the extract of ethyl acetate with methanol through a chromatographic column. 4) The eluate collected in step 3) is further separated and refined by high-pressure liquid chromatography to obtain the active compound. The general formula of the extracted active compound (3-10) is that the active compound (1) is: the active compound (2) is: the compound or its salt, enantiomer, racemate, tautomer extracted from Shixiantao Body or physiological functional derivatives can be used to prepare medicines for treating or preventing inflammatory diseases.

Description

technical field [0001] The invention relates to the extract of shixiantao, its preparation method and its application in the preparation of medicines, in particular to extracting four active compounds from shixiantao. [0002] Background technique [0003] Daily inflammatory diseases that plague people include joint inflammation such as osteoarthritis, rheumatoid arthritis, rheumatoid spondylitis, gouty arthritis, etc.; inflammatory skin diseases such as eczema, psoriasis, dermatitis, etc.; Uveitis, conjunctivitis, etc.; lung diseases such as asthma, bronchitis, acute respiratory distress syndrome, etc.; bacteremia, that toxemia, aphthous ulcers, gingivitis, pancreatitis, etc.; Ileitis, atrophic gastritis, ulcerative colitis, celiac disease, peptic ulcer, irritable bowel syndrome such as mucosal inflammation caused by Helicobacter pylori infection or gastrointestinal tract caused by non-steroidal anti-inflammatory drugs illness and so on. [0004] The mechanism of various ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C43/243C07C43/253C07C41/36
CPCC07C43/243C07C43/253C07C41/36C07C2602/26
Inventor 王珏北中进
Owner NIHON UNIVERSITY
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