CN104352562B - A kind of preparation method of schizonepeta general flavone and its application in antitumor - Google Patents
A kind of preparation method of schizonepeta general flavone and its application in antitumor Download PDFInfo
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Abstract
A kind of preparation method of schizonepeta general flavone, it is characterised in that：Schizonepeta dry aerial parts and its flower spike are taken, goes the removal of impurity, crushed 10 mesh sieves, coarse powder is made, dries, the concentration for adding 5 40 times of amounts is 10 95% ethanol solution, heating and refluxing extraction 13 times, 0.5 3 hours every time, filtering, merging filtrate, ethanol is reclaimed to without alcohol taste, it is 0.8 1.3 to be concentrated under reduced pressure into and survey relative density at room temperature, vacuum drying, produces schizonepeta extractive of general flavone crude product.High-purity cancer therapy drug fine work can be obtained by being further purified.The inventive method only needs certain density ethanol solution heating and refluxing extraction, purified using large pore resin absorption column, product stability and homogeneity are good, can be to be applied to large-scale industrial production to be provided with niche plinth, it is expected to develop as the PTS with extensive Clinical practice value and business development value using schizonepeta general flavone purified as raw material.
Description
Technical field
The invention belongs to field of medicaments, and by extraction, enrichment particularly to from Chinese medicine schizonepeta, it is total to obtain schizonepeta
Application in the preparation method and its anticancer of flavones.
Background technology
Tumour is a kind of common disease of serious threat human health, is one of three big killers of human health, searching has
The cancer therapy drug and method of effect, it is the important topic that world medicine faces.Chinese medicine is that motherland's medical use carrys out the strong of disease preventing and treating
Weapon, compared with chemical synthetic drug, Chinese medicine is in addition to having the advantages that convenient material drawing, cheap and toxic side effect is small, more
Importantly, mitigating clinical symptoms, life quality is improved, prevents relapse and metastasis, extends life cycle, pre- preventing tumor, improves and suffers from
Person's immunity, strengthen Radiotherapy chemotherapy sensitiveness, mitigate many aspects such as Radiotherapy chemotherapy adverse reaction and play an important role.Meanwhile
With the development of the society, the development of productivity, notice is increasingly turned to crude drug by modern from chemical combination patent medicine, it is desirable to from day
Developed in right medicine safer effective new drug with replacement the former, so as to reduce the generation of medicine source disease.Therefore, in development
Herbal medicine has not only passed on Chinese nation's elite of 1,100, it may have large market prospect and economic benefit.
Schizonepeta (fringe) is labiate schizonepeta Schizonepeta tenuifolia Briq. dry aerial parts
(drying flower spike).National most area is produced, cheap, is widely used.The traditional Chinese medical science thinks, schizonepeta (fringe) acrid flavour, slight bitter, property
It is micro- wet, return lung, Liver Channel, have inducing diaphoresis dissipate wind, promoting eruption, disappear sore and other effects, for catching a cold, headache, measles, rubella, sore from the beginning of.
Modern clinical research shows that schizonepeta (fringe) not only has the effect of antipyretic-antalgic, anti-inflammatory, antibacterial, also has calm anticonvulsion, enhancing to exempt from
Epidemic disease function, antitumor etc. act on.Contain plurality of active ingredients in schizonepeta (fringe), including volatile oil, flavones, monoterpene, triterpenic acid, have
Machine acid etc..At present, the research for schizonepeta (fringe) antitumor action is in the majority with volatile oil report, and is used as effective portion using flavonoids
The research that position is carried out then has no report.This experiment premenstruum (premenstrua) pharmacodynamic experiment proves, flavones is antitumor effective of schizonepeta (fringe)
Material composition, there is higher Development volue, therefore further extraction and purification process investigation, preferably optimised process bar are carried out to it
Part, to be laid the foundation for the research of the further pharmacological effect of schizonepeta (fringe) general flavone component.
According to document report in recent years, existing process technology prepares schizonepeta (fringe) general flavone and has that purity is high, technique
The problems such as stability difference, this necessarily affects the composition composition for illustrating schizonepeta (fringe) general flavone and the detection of drug activity, also unfavorable
In large-scale industrial production and clinical practice, it is therefore necessary to which the purification process of schizonepeta (fringe) general flavone is studied.This reality
Test by preferred schizonepeta (fringe) general flavone optimum extraction process, then its purifying process is studied, purification process can make total Huang
Ketone enriched substance purity reaches more than 90%, ideal.This not only contributes to improve the steady of schizonepeta general flavone purity and its technique
It is qualitative, it is also beneficial to illustrate effective substance component and its clinical effect mechanism, and may be used in the exploitation of new drug.
According to literature survey, the research to schizonepeta (fringe) flavones at present is mainly in the majority with the effect of its resisiting influenza virus, and its
There is not been reported for antitumor action research.The present invention by unexpected antitumor experiment demonstrate general flavone also have it is obvious antitumor
Effect, the exploitation for input anti-cancer agent later lay the foundation.
The content of the invention
It is an object of the present invention to provide a kind of preparation method of schizonepeta general flavone, and its application as cancer-resisting substance.
The technical scheme of use is：
Schizonepeta is labiate Chinese medicine, (Schizonepeta tenuifolia Briq.).The present invention is to use chaste tree
The dry aerial parts of mustard and flower spike is dried as raw material, extract the extraction purification thing of the active ingredient of schizonepeta, active ingredient is
Total flavonoid, there is antitumor efficacy.Specifically：
A kind of preparation method of schizonepeta general flavone, it is characterised in that：
1st, schizonepeta dry aerial parts and its flower spike are taken, goes the removal of impurity, crushed 10 mesh sieves, coarse powder is made, is dried, is added
The ethanol solution that the 5-40 times of concentration measured is 10-95%, heating and refluxing extraction 1-3 times, each 0.5-3 hours, filtering, merge filter
Liquid, for recovery ethanol to without alcohol taste, it is 0.8-1.3 to be concentrated under reduced pressure into and survey relative density at room temperature, vacuum drying, it is always yellow to produce schizonepeta
Ketone extract crude product.
2nd, schizonepeta extractive of general flavone crude product is diluted with water, is diluted to 0.1-0.4g crude drug amounts/ml decoction, upper HPD-
400 macroporous resin columns, medicinal material/wet resin are 0.5-1.5g/ml than upper column quantity, and first rinsing 1-5BV column volumes with water cleans, then uses
The ethanol solution that concentration is 30-90% elutes 1-20BV column volumes, concentration, obtains concentrate, then is diluted with water to 0.1-0.4g lifes
Medicine/ml decoction, using decoction/wet resin as 0.5-1.5g/ml upper props, with 1-5BV ions, then with 1-20BV, concentrate and be
30-90% ethanol elution, recovery ethanol produce schizonepeta extractive of general flavone fine work, schizonepeta general flavone purity to without alcohol taste>
90%.
The schizonepeta extractive of general flavone of the present invention can prepare a variety of formulations, and can add pharmaceutically acceptable assistant agent and load
Body is applied to the research and development of clinical anti-cancer new drug.
Schizonepeta chromocor extract through the clinical trial certificate present invention has good anticancer effect.
The present invention by pharmacological effect it is demonstrated experimentally that schizonepeta (fringe) general flavone purified is with the rising of purity, it is antitumor
Curative effect is more and more significant, it was demonstrated that schizonepeta (fringe) general flavone purified can be used as a kind of effective cancer therapy drug.
The process of preparing of the present invention is simple, effective ingredient recovery rate is high, it is evident in efficacy, accurately and reliably, can be more
The effect of comprehensively ensureing Chinese medicine and quality, and with original directly using compared with medicinal material decocting liquid, under the effect of identical, this
The purified that preparation method is obtained has the advantages of taking dose is small.
The present inventor according to clinic need schizonepeta (fringe) general flavone enriched substance is prepared as each formulation and can
Add pharmaceutically acceptable assistant agent and carrier and supply selection of clinical application.
Specific embodiment：
Embodiment one
A kind of preparation method of schizonepeta general flavone, including following processing steps：
Schizonepeta (fringe) medicinal material drying is taken to crushed 10 mesh sieves to constant weight, precision weighs 5.0g, using traditional extraction condition,
Extraction experiment is carried out as follows, and each method is parallel two parts.
EtOH Sonicate extraction method adds 75% ethanol 100mL in sample, room temperature ultrasonic extraction 1h, and filtration, filter residue adds
100mL75% ethanol ultrasonic extraction 1h again, filtration, merging filtrate, concentration, it is dried under vacuum to constant-quality.
Ethanol reflux extraction adds 75% ethanol 100mL in sample, refluxing extraction 1h, and filtration, filter residue adds 100mL75%
Ethanol refluxing extraction 1h again, filtration, merging filtrate, concentration, it is dried under vacuum to constant-quality.
Water reflux extraction adds 100mL water in sample, refluxing extraction 1h, and filtration, filter residue adds 100mL water refluxing extraction again
1h, filtration, merging filtrate, concentration, it is dried under vacuum to constant-quality.
Measurement result the results are shown in Table 1.
The overall merit of the schizonepeta of table 1 (fringe) flavones Different Extraction Method
As a result show, when alcohol reflux extraction method is extracted, extraction general flavone content is higher in schizonepeta (fringe), therefore establishes schizonepeta
The optimum extracting method of (fringe) flavones is alcohol reflux extraction method.
The orthogonal of embodiment two
4 solvent load, extraction time, extraction time and volume fraction of ethanol factors are chosen, each factor selects 3 water
Flat, factor level is shown in Table 2.Schizonepeta (fringe) medicinal material drying is taken to crushed 10 mesh sieves to constant weight, weigh coarse powder 5.0g and put 250mL circles
In the flask of bottom, by orthogonal arrage arrangement, appropriate respective volume fraction ethanol solution, water-bath refluxing extraction are added, recovery ethanol must carry
Take thing.Tested by L9 (3 4) orthogonal arrage arrangement, influence of each factor to extraction effect, examination are investigated by index of general flavone content
Test and arrange and the results are shown in Table 3, variance analysis is shown in Table 4.
The preferred orthogonal test factor level of the schizonepeta of table 2 (fringe) general flavone Effect of Alcohol Extracting Procedureto Total
The preferred orthogonal test arrangement of the schizonepeta of table 3 (fringe) total flavone extracting process
The general flavone recovery rate variance analysis of table 4
Note：F0.05(2,2)=19；p*<0.05
As a result show, using general flavone as index, the factor order that analysis shows directly perceived influence schizonepeta extracting flavonoids effect is B
>D>A>C.Using the minimum factor C of extreme difference as error term, variance analysis is carried out, factor B has a significant impact, and other factors are then without aobvious
Work property influences.With reference to production cycle and cost consideration, it is A to determine optimum extraction process2B2C1D3, i.e. solvent load is 15 times of amounts,
Volume fraction of ethanol is 75% ethanol, refluxing extraction 1h, is extracted 3 times.
Embodiment three
First, the checking test of optimize technique
According to Optimized Extraction Process, i.e. 75% ethanol, 20 times of dosages, extract 3 times, each 1h, carry out 3 checking tests.Carry
The average content for taking thing general flavone is 8.93%, RSD% 1.02%, illustrates the process stabilizing.
2nd, purifying process optimizes
The preparation of example IV upper prop solution
Schizonepeta (fringe) coarse powder 5.0g is weighed, it is accurately weighed, extracted by above-mentioned optimum extraction process, add 20 times of amounts 75%
Ethanol, refluxing extraction 3 times, each 1h merge No. 3 extract solutions, recovery ethanol to without alcohol taste, be diluted with water into 0.1g (crude drug)/
ML decoction, ultrasound make dissolving, produce.
The Resin sieving selection result of embodiment five
10 kinds of macroreticular resins of Integrated comparative the results are shown in Table 5, finally select to 2 indexs of adsorbance and resolution factor of general flavone
Select larger low pole HPD-400 purifying resins schizonepeta (fringe) flavones of specific surface area.
59 kinds of macroreticular resins of table adsorb and parsed feature for schizonepeta (fringe) flavone compound
The investigation of the sample solution concentration of embodiment six
Select 5 concentration liquids 0.1,0.2,0.3,0.4,0.5g (crude drug)/mL, the amount of sequentially adding be 100,50,33,
25th, 20mL, after carrying out Dynamic Adsorption under the same conditions with 2BV/h flow velocity, rinsed with 2BV distilled water by 4BV/h, to flushing
Liquid molish reactions are feminine gender.Eluted again with 70% ethanol, it is closely colourless to be eluted to eluent.Eluent is collected, point
Other constant volume determines general flavone adsorbance in accordance with the law in 50mL measuring bottles, the results showed that, in the range of finite concentration, macroporous absorption tree
The adsorbance of fat reduces with the increase of sample solution concentration, may be sticked due to being on the increase with the increase of concentration, precipitation
Degree also constantly increase, blocks resin column, causes the reduction of resin adsorption amount.Therefore, from the sample that concentration is 0.1g (crude drug)/mL
Solution is adsorbed.
The sample solution pH of embodiment seven investigation
Take decoction (pH=5.0) 50mL that 6 parts of concentration are 0.1g (crude drug)/mL, regulation pH value is to 3.0,4.0,5.0,
6.0th, 7.0,8.0, Dynamic Adsorption is carried out with 2BV/h flow velocity, determines general flavone adsorbance in accordance with the law.As a result show, sample solution
PH value be adsorbed with large effect to schizonepeta (fringe) general flavone, adsorbance is relatively low during pH=3.0, because sample solution acidity is too
By force, flavone compound is easily changed into salt of pretending, and is not easy to be adsorbed[8], the adsorbance of general flavone is maximum during pH=5.0, because this
When acidity can just flavone compound is kept molecular forms in the solution, it is easily adsorbed.Therefore, sample solution adsorbs
Optimal pH be 5, therefore in following experiment, sample solution selects the direct upper prop of stoste.
Embodiment eight is revealed curve and investigated
Taking liquid 150mL, by above-mentioned condition upper prop, Fractional Collections absorption efflux (10mL/ sections), 15 parts altogether, determine
Schizonepeta (fringe) general flavone content (mg/g) in each fraction, the results showed that, when loading volume is 80mL, general flavone starts to leak,
Accordingly, it is determined that numerical value maximum applied sample amount is the 8th part, i.e. resin is 0.8g/mL (medicinal material/wet resin) than upper column quantity.
Embodiment nine elutes the investigation of determining alcohol
Taking liquid 80mL presses above-mentioned condition upper prop, anti-to flushing liquor molish with 2BV distilled water flushings after absorption
It should be negative.Eluted respectively with 30%, 50%, 60%, 70%, 80% and 90% ethanol 50mL again.Eluent is collected, it is fixed
It is dissolved in 50mL measuring bottles, determines the content of general flavone in accordance with the law.As a result show, the general flavone of 70%, 80%, 90% ethanol elution contains
Amount be respectively 84.67,84.34 and 84.11mg/g, be more or less the same, accordingly, it is considered to save solvent, it is determined that using 70% ethanol as
Eluting solvent.
Embodiment ten elutes alcohol dosage and investigated
Taking liquid 80mL presses above-mentioned condition upper prop, anti-to flushing liquor molish with 2BV distilled water flushings after absorption
It should be negative.Eluted again with 70% ethanol, collect 15 parts of eluents (10mL/ parts), determine the content of eluent general flavone.
As a result show, the general flavone content that No. 8 ethanol elutions of fraction (80mL) 70% get off is significantly lower than fraction 7, but with fraction 9 and its
Later each fraction is more or less the same, and shows now to elute substantially completely.Calculated by every section of fraction 10mL, eluent dosage is
80mL, equivalent to 8 times resin column volumes, so eluent optimum amount is 8BV.
11 purifying process confirmatory experiments of embodiment
3 parts of HPD-400 macroporous absorbent resins accurately are measured, fill post respectively, adsorbed by above-mentioned preferable process conditions,
Elution, that is, weigh 8.0g schizonepeta (fringe) medicinal material, with the concentration of 0.1g/mL (raw medicinal herbs), resin after optimum extraction process extracts
It is 0.8g/mL (medicinal material/wet resin) upper prop than upper column quantity, with 2BV ions, with the ethanol elutions of 9BV 70%, collects elution
Liquid, volatilize, determine general flavone content, calculated purity and yield, the results are shown in Table 6.
The process certification result of table 6
Embodiment 12 is secondarily purified and its confirmatory experiment
Schizonepeta (fringe) general flavone average yield is equal after purification for the first time>85%, be appropriate for it is secondarily purified, therefore use it is above-mentioned
Optimal purification process carries out secondary purification with macroreticular resin, it is same it is parallel do 3 parts, determine general flavone content, calculated purity and
Yield.
7 secondarily purified experimental result of table
Embodiment 13 purifies forward and backward general flavone antitumor cell pharmacy in vitro research
Caco-2 cancer cell suspensions are prepared, growth period of taking the logarithm, cell in good condition, are disappeared with 0.25% trypsase
Change, 5 × 10 are configured to culture medium4Individual cell/mL cell suspension, is inoculated in 96 well culture plates, per the μ L of hole 100.37 DEG C,
5%CO2Cell 24h is cultivated in incubator.According to conventional administration dosage combination paste-forming rate and general flavone purity, schizonepeta (fringe) is returned
Stream extract, a purified product and secondarily purified product are configured to contain crude drug amount with the DMEM nutrient solutions containing 10% calf serum
Consistent decoction, through 0.22 μm of membrane filtration, each group sets 10 multiple holes, and 100 μ L decoctions are added per hole, and normal cancer is thin
Born of the same parents' group is used as blank control group, and control group adds equivalent fresh medium.37 DEG C, 5%CO2Continue to cultivate cell in incubator.Training
After supporting 24h, the MTT that adds people newly to prepare, per the μ L of hole 20,37 DEG C of CO are put2Culture acts on 4h in incubator, carefully sucks supernatant,
Dimethyl sulfoxide (DMSO) 150 μ L are added, after gently vibrating 5min on the oscillator, absorbance is surveyed at 492nm with ELIASA
(OD values).10 hole average values are taken, inhibiting rate are calculated, according to formula：Cell inhibitory rate=(1- experimental groups OD values/control group OD values)
× 100%, equally test it is parallel do 3 parts, experimental result the results are shown in Table 8 in terms of average value.
Influence of the different group decoctions of table 8 to Caco-2 cells optical density and inhibiting rate
| Group | OD492 | MTT inhibiting rates % |
| Model group | 0.905±0.005 | —— |
| Refluxing extraction thing group | 0.455±0.006 | 49.75 |
| Purified product group | 0.264±0.008** | 70.84 |
| Secondarily purified product group | 0.125±0.009** | 86.17 |
Note：p**<0.01。
Test result indicates that refluxing extraction thing group, a purified product group, secondarily purified product group are to exponential phase
Caco-2 inhibition rate of tumor cell is respectively 49.75,70.84,86.17%, it was demonstrated that schizonepeta (fringe) general flavone purified is to Caco-
2 tumour cells have obvious inhibitory action, and as the raising of purity, inhibiting rate dramatically increase (p**<0.01), in purity according to
Bad relation, further prove that schizonepeta (fringe) general flavone purified can suppress tumour cell growth, to develop into PTS later
Lay the foundation.
Conclusion
The process of preparing of the present invention is simple, process stabilizing, effective ingredient DNA purity high (more than 90%), treats
Effect significantly, accurately and reliably, can more fully ensure the effect of Chinese medicine and quality, and to have taking dose small etc. excellent for preparation method
Point.
In addition, schizonepeta (fringe) the general flavone purified prepared by the present invention has obvious suppress to Caco-2 tumour cells
Effect, it is expected to be prepared into a variety of formulations, develop as there is extensive Clinical practice as raw material using schizonepeta (fringe) general flavone purified
The PTS of value and business development value.
Claims (4)
- A kind of 1. preparation method of schizonepeta general flavone, it is characterised in that：（1）, take schizonepeta dry aerial parts and its flower spike, go the removal of impurity, crushed 10 mesh sieves, coarse powder is made, dry, add 5- The concentration of 40 times of amounts is 10-95% ethanol solution, heating and refluxing extraction 1-3 times, each 0.5-3 hours, is filtered, merging filtrate, Ethanol is reclaimed to without alcohol taste, it is 0.8-1.3 to be concentrated under reduced pressure into and survey relative density at room temperature, vacuum drying, produces schizonepeta general flavone Extract crude product；（2）Schizonepeta extractive of general flavone crude product obtained by step 1 is diluted with water, is diluted to 0.1-0.4g crude drug amounts/ml's Decoction, upper HPD-400 macroporous resin columns, medicinal material/wet resin are 0.5-1.5g/ml than upper column quantity, first rinse 1-5BV cylinders with water Product removal of impurities, then the ethanol solution for being 30-90% with concentration elute 1-20BV column volumes, concentration, obtain concentrate, then be diluted with water to 0.1-0.4g crude drugs/ml decoction, using decoction/wet resin as 0.5-1.5g/ml upper props, with 1-5BV ions, then use 1- 20BV, concentrates the ethanol elution for 30-90%, and recovery ethanol produces schizonepeta extractive of general flavone fine work, schizonepeta is total to without alcohol taste Flavones purity>90%.
- 2. the preparation method of a kind of schizonepeta general flavone according to claim 1, it is characterised in that the concentration of alcohol is 75%, addition is 20 times of raw medicinal herbs amounts, refluxing extraction 3 times, extracts 1h every time.
- A kind of 3. preparation method of schizonepeta general flavone according to claim 1, it is characterised in that：Sample solution concentration is 0.1g Crude drug amount/ml, pH value 5, elution concentration of alcohol are 70%.
- A kind of 4. preparation method of schizonepeta general flavone according to claim 1, it is characterised in that obtained general flavone pair The tumour cells of Caco -2 have obvious inhibitory action, and the cancer therapy drug of a variety of formulations can be made.
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| CN110353153B (en) * | 2019-06-05 | 2021-03-26 | 中国农业科学院北京畜牧兽医研究所 | Schizonepeta mediator for improving degradation rate of laccase on mycotoxin and application thereof |
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Non-Patent Citations (4)
| Title |
|---|
| 大孔吸附树脂法富集纯化荆芥穗总黄酮的工艺研究;黄志宏;《中药材》;20100930(第09期);第1476-1480页 * |
| 大孔树脂分离纯化荆芥中的总黄酮;陈静，等;《中国药业》;20110331;第20卷(第3期);第30页右栏第1段，第31页左栏第1-4段 * |
| 大孔树脂吸附分离荆芥总黄酮工艺研究;罗伟华;《中国现代药物应用》;20120930(第09期);第69-70页 * |
| 荆芥挥发油抗肿瘤作用的研究;臧林泉等;《广西中医药》;20060430(第04期);第60-62页 * |
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