CN104072515A - Extraction and purification method of Indian guassin X and application of Indian guassin X - Google Patents
Extraction and purification method of Indian guassin X and application of Indian guassin X Download PDFInfo
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- CN104072515A CN104072515A CN201410266367.8A CN201410266367A CN104072515A CN 104072515 A CN104072515 A CN 104072515A CN 201410266367 A CN201410266367 A CN 201410266367A CN 104072515 A CN104072515 A CN 104072515A
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K31/00—Medicinal preparations containing organic active ingredients
- A61K31/33—Heterocyclic compounds
- A61K31/335—Heterocyclic compounds having oxygen as the only ring hetero atom, e.g. fungichromin
- A61K31/365—Lactones
- A61K31/366—Lactones having six-membered rings, e.g. delta-lactones
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D493/00—Heterocyclic compounds containing oxygen atoms as the only ring hetero atoms in the condensed system
- C07D493/02—Heterocyclic compounds containing oxygen atoms as the only ring hetero atoms in the condensed system in which the condensed system contains two hetero rings
- C07D493/10—Spiro-condensed systems
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Abstract
The invention relates to an extraction and purification method of Indian guassin X and an application of Indian guassin X. The extraction and purification method comprises the following steps of pulverizing Indian quassia wood as a raw material, and extracting under reflux with ethanol, concentrating an extracting solution to obtain an extract, carrying out ultrasonic dissolving on the extract in an acid aqueous solution, standing, taking the supernatant, extracting with ethyl acetate to obtain an ethyl acetate extract and separating the extract by virtue of silica gel column chromatography to obtain the Indian guassin X. The method disclosed by the invention has the advantages of controllable quality and high content of active ingredients and is suitable for industrial production. The Indian guassin X prepared by the invention is particularly applied in the preparation of antitumor drug, especially the drugs for inhibiting neutrophils from adhering to endothelial cells induced by the tumor necrosis factor.
Description
Technical field
The present invention relates to method of purification and its medicinal use of a kind of compound, be specifically related to extracting and purifying method and its application in preparing antitumor drug of a kind of India quassin X.
Background technology
Tumour is a class common disease, the frequently-occurring disease that harm humans health is the most serious, and modal methods for the treatment of is operation, chemotherapy and radiation, and chemotherapy is because toxic side effect is large, affects patients ' life quality.In recent years, TCM on Tumor is called unique therapy, the traditional Chinese medical science think in the wet cohesion of stagnation of blood stasis, phlegm, hot poison accumulate, healthy tendency virtual loss is to lead the oncogenic interpretation of the cause, onset and process of an illness, according to the etiology and pathogenesis of tumour, regularity of occurrence and development, Traditional Chinese Drug Anticancer treatment mainly contains and strengthens the body resistance to consolidate the constitution, clearing heat and detoxicating, promoting blood circulation and removing blood stasis, four fundamentums of softening and resolving hard mass.The mechanism for the treatment of by Chinese herbs tumour is mainly to the direct inhibition of tumour cell and killing action, inhibition tumor-blood-vessel growth, suppresses telomerase activation, Cell differentiation inducing activity, adjusting cell signaling, anti-microtubule effect, immuno-potentiation, the effect of reverse multidrug resistance etc.The advantages such as Chinese medicine applicating history is long, cheap, medicine source extensive, good effect, hypotoxicity, the prospect in oncotherapy also will be more and more wider.
India quassin X is from Simarubaceae (Simarcubaceae) plant Indian quassia
quassia indica(Gaertn.) the separated a kind of quassin obtaining in Nooteboom, molecular formula is C
20h
26o
10, molecular weight is 426.42.Pharmacological research shows, India quassin X has anti-tumor activity, when concentration is 1 μ g/ml, suppresses neutrophilic leukocyte and adheres to the endotheliocyte of being induced by tumour necrosis factor; In addition, KB cell is to cytotoxic activity, IC50 is 0.60 μ g/ml.
At present, the rare antitumor drug that contains India quassin X in prior art, this present situation is urgently to be resolved hurrily.
Summary of the invention
For meeting clinical needs, expand medicine variety, treat better cancer, extracting and purifying method and its application method and application in preparing antitumor drug of a kind of India quassin X are provided.
An extracting and purifying method of India quassin X, is characterized in that, it comprises the following steps:
(1) take India's quassia as raw material, pulverize, use 60-80% ethanolic soln refluxing extraction 2-3 time, each 0.5-1h, the concentrated medicinal extract that to obtain of extracting solution;
(2) medicinal extract is used to aqueous acid ultrasonic dissolution, standing, get supernatant liquor, be extracted with ethyl acetate and obtain acetic acid ethyl ester extract;
(3) by extract dissolve with methanol, adopt silica gel column chromatography, ethyl acetate-methanol mixed solvent is 1:1-5 wash-out by volume, Fractional Collections, thin-layer chromatography is followed the tracks of inspection knowledge, merges the flow point that contains India quassin X, concentrating under reduced pressure, natural crystallization, obtains white India quassin X crystallization.
In the present invention, the 6-10 that the described ethanolic soln consumption of step (1) is medicinal material weight doubly.
In the present invention, the described aqueous acid of step (2) is 0.5% acetic acid aqueous solution, and consumption is for measuring 3-4 times for medicinal extract weight.
In the present invention, the described silica gel of step (3) is 200-300 order.
Test shows to adopt the inventive method to extract purifying India quassin X, and its purity is more than 80%, and product yield is compared with general extraction and improved 2-3 doubly.
The invention still further relates to the resulting plant milk extract of extracting and purifying method of the present invention.
The invention further relates to described plant milk extract and adhere to the application in the endotheliocyte medicine of being induced by tumour necrosis factor at preparation inhibition neutrophilic leukocyte.
The pharmacologically active of India quassin X of the present invention has obtained checking by following test.
Test cell strain:
HeLa: human cervical carcinoma cell strain; HEC-1: people's Endometrial carcinoma cell line; T-98 and U251-SP: the strain of human brain neuroglial cytoma; HLE: human hepatoma cell strain; MM1-CB and HMV-1: human melanoma cell strain.
India quassin X inhibition neutrophilic leukocyte adheres to the endotheliocyte of being induced by tumour necrosis factor and tests:
Experimental technique: tetrazolium father-in-law salt-neutrophilic leukocyte adherence inhibition laboratory method
In the D-MEM/hams substratum that contains 10% foetal calf serum, by tested cell furnishing density, be 2 * 10
6cell/ml.By above-mentioned tumor cell line suspension inoculation in 96 well culture plates, every hole 50 μ l, (each 50 μ l of PBS0, solvent control 0.1% dimethyl sulfoxide (DMSO), positive control cis-platinum (DDP) and different concns monomeric compound establish 3 multiple holes for every group to add respectively blank phosphate buffered saline buffer.Being placed in saturated humidity, 37 ℃ and 5%CO2 incubator cultivates 48 hours, in cultivation, finish first 4 hours, each culture hole adds 5mg/ml tetrazolium father-in-law salt (MTT) 10 μ l, after cultivation finishes, discard culture supernatant, the centrifugal rear supernatant discarded of suspension cell, the busy reaction stop solution 150 μ l that add, standing 1 hour, by microplate reader, survey 490nmO.D value, and calculate neutrophilic leukocyte adherence inhibition rate.
The compounds of this invention is dissolved in DMSO, and the ultimate density after interpolation is below 0.1%.Only to add the cultivation of DMSO and in contrast.
Experimental result: the neutrophilic leukocyte adherence inhibition rate of the compounds of this invention represents as following table 1 with the result with respect to contrast (add DMSO).
The neutrophilic leukocyte adherence inhibition rate % of table 1 India quassin X
| India quassin X concentration (μ M) | HeLa | HEC-1 | T-98 | U251-SP | HLE | MM1-CB | HMV-1 |
| 100 | 56 | 64 | 71 | 63 | 68 | 86 | 85 |
| 10 | 42 | 7 | 29 | 20 | 14 | 41 | 27 |
| 1 | 20 | 6 | 12 | 4 | 2 | 2 | 5 |
More than test shows, India quassin X has the activity that good inhibition neutrophilic leukocyte adheres to the endotheliocyte of being induced by tumour necrosis factor, and it can be applied in preparing antitumor drug.
The present invention provides a kind of new selection for preparing antitumor drug.
India quassin X of the present invention is when preparing antitumor drug, can take India quassin X according to conventional formulation method is active constituents of medicine, add suitable pharmaceutical carrier, make various pharmaceutical dosage forms, as tablet, capsule, dripping pill, injection, controlled release agent etc.
When being used for the treatment of tumor disease, the consumption of oral preparations generally can be controlled in and takes India quassin X200-500mg every day.The consumption of other formulations can be with reference to this consumption.Drug usage consumption of the present invention, is also not limited solely to this, and clinicist also can determine according to patient's particular case the usage and dosage of medicine.
embodiment:
The following examples can illustrate in greater detail the present invention, but do not limit in any form the present invention.
Embodiment 1
The extraction purifying (1) of India quassin X be take India's quassia as raw material, pulverizes 10 times of 80% ethanolic soln refluxing extraction of use medicinal material weight 3 times, each 0.5h, the concentrated medicinal extract that to obtain of extracting solution; (2) by 4 times of 0.5% acetic acid aqueous solution ultrasonic dissolution for medicinal extract, standing, get supernatant liquor, be extracted with ethyl acetate and obtain acetic acid ethyl ester extract; (3) by extract dissolve with methanol, adopt 300 order silica gel column chromatographies, ethyl acetate-methanol mixed solvent is 1:1,1:3,1:5 wash-out by volume, Fractional Collections, thin-layer chromatography is followed the tracks of inspection knowledge, merges the flow point that contains India quassin X, concentrating under reduced pressure, nature crystallization, obtains white India quassin X crystallization, and content is 90.2%.
Embodiment 2
Medicinal granule of the present invention adds ethanol to make tamanori the made India of embodiment 1 quassin X, adds starch to make weighting agent, granulation.
Embodiment 3
Medicinal tablet of the present invention, by the made India of embodiment 1 quassin X, adds starch, dextrin, Magnesium Stearate etc., is mixed and made into wet grain, compressing tablet, Mei Pianhan India quassin X200mg.
Claims (6)
- The extracting and purifying method of 1.Yi Zhong India quassin X, is characterized in that, it comprises the following steps:(1) take India's quassia as raw material, pulverize, use 60-80% ethanolic soln refluxing extraction 2-3 time, each 0.5-1h, the concentrated medicinal extract that to obtain of extracting solution;(2) medicinal extract is used to aqueous acid ultrasonic dissolution, standing, get supernatant liquor, be extracted with ethyl acetate and obtain acetic acid ethyl ester extract;(3) by extract dissolve with methanol, adopt silica gel column chromatography, ethyl acetate-methanol mixed solvent is 1:1-5 wash-out by volume, Fractional Collections, thin-layer chromatography is followed the tracks of inspection knowledge, merges the flow point that contains India quassin X, concentrating under reduced pressure, natural crystallization, obtains white India quassin X crystallization.
- 2. extracting and purifying method as claimed in claim 1, is characterized in that ethanolic soln consumption described in step (1) is 6-10 times of medicinal material weight.
- 3. extracting and purifying method as claimed in claim 1, is characterized in that described in step (2), aqueous acid is 0.5% acetic acid aqueous solution, and consumption is for measuring 3-4 times for medicinal extract weight.
- 4. extracting and purifying method as claimed in claim 1, is characterized in that described in step (3), silica gel is 200-300 order.
- 5. the resulting plant milk extract of extracting and purifying method as described in claim 1 ~ 4 any one.
- 6. plant milk extract as claimed in claim 5 adheres to the application in the endotheliocyte medicine of being induced by tumour necrosis factor at preparation inhibition neutrophilic leukocyte.
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| CN201410266367.8A CN104072515A (en) | 2014-06-16 | 2014-06-16 | Extraction and purification method of Indian guassin X and application of Indian guassin X |
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| CN201410266367.8A CN104072515A (en) | 2014-06-16 | 2014-06-16 | Extraction and purification method of Indian guassin X and application of Indian guassin X |
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2014
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