CN100450502C - Active extract of lamtophlomis rotata and its preparing method and use - Google Patents
Active extract of lamtophlomis rotata and its preparing method and use Download PDFInfo
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Abstract
The present invention provides a lamiophlomis rotata kudo active extract and a preparation method thereof and the service application thereof, and the present invention relates to an active extract extracted by using lamiophlomis rotata kudo as raw material and containing total flavonoids and also relates to the preparation method and the service application of the active extract. In the present invention, extracting solution obtained after roots and / or whole herbs of lamiophlomis rotata kudo medicinal material are extracted by alcohol and water is further separated and purified to obtain the active extract; a dried product of the active extract comprises 50 to 80 wt% of total flavonoids and 1.0 to 5.0 wt% of luteolin by rutin. The active extract increases the therapeutic effect of the medicine and reduces patients's dosage each time; the active extract can be used for different pain and bleeding such as cut pain and bleeding after surgical operations, trauma fracture, etc.; the active extract can alleviate pain and can stop bleeding. The active extract added with allowable auxiliary material in pharmacy can be manufactured into any oral preparations and preferably manufactured into dripping pills. The preparation method is suitable for industrial bulk production.
Description
Technical field
The invention belongs to field of medicaments, relating in particular to single plant Radix Lamiophlomidis Rotatae is the activity extract that contains total flavones that raw material extracts.The invention still further relates to the Preparation method and use of this activity extract.
Background technology
Radix Lamiophlomidis Rotatae sheet and Radix Lamiophlomidis Rotatae capsule are a kind of traditional Chinese patent medicines, it is to be made by the herb of single plant Radix Lamiophlomidis Rotatae or root processing, record in Chinese Pharmacopoeia, it has promoting blood circulation and stopping pain, the function of removing stasis to stop bleeding is used for the edge of a knife pain, hemorrhage behind the multiple surgical operation, the surgery fracture, muscles and bones is sprained, rheumatic arthralgia and metrorrhagia, dysmenorrhea, gingival swelling and pain, hemorrhage etc.Chinese patent application number 02134169.9 discloses a kind of dispersible tablet of Radix Lamiophlomidis Rotatae, but these three kinds of preparations all are to adopt the water extract of Radix Lamiophlomidis Rotatae medical material to make, and there is the big shortcoming of dose in it, generally need oral one time 3, every 300mg three times on the one, is equivalent to the 9g crude drug.
Summary of the invention
The dosage form that the objective of the invention is to overcome existing common lamiophlomis root preparation is few, the shortcoming that dose is big, and the effective medicinal part of development and use Radix Lamiophlomidis Rotatae is made treatment is truly had curative effect, the novel drugs that taking dose is few.
For reaching the technical scheme that the object of the invention adopts be: adopt labiate Radix Lamiophlomidis Rotatae (Lamiophlomis rotata (Benth.) Kudo), comprise the activity extract that root and/or herb obtain through extraction, be to adopt the root of Radix Lamiophlomidis Rotatae medical material and/or the herb extracting solution after alcohol extraction or water are carried, further separation and purification obtains activity extract, the dry product of its activity extract contains total flavones, and to reach percent by weight in rutin be 50-80%, and containing luteolin, to reach percent by weight be 0.5-5.0%.
The assay method of total flavones is reference substance with reference to Chinese Pharmacopoeia appendix spectrophotometry with the rutin in the activity extract, measures trap at 500nm wavelength place, calculates content of total flavone.The assay method of luteolin is with reference to Chinese Pharmacopoeia appendix high effective liquid chromatography for measuring:
Chromatographic condition and system: with octadecylsilane chemically bonded silica is filler; With methanol-0.4% phosphoric acid solution (50: 50) is mobile phase; The detection wavelength is 350nm; Theoretical cam curve is calculated by the luteolin peak should be not less than 1500.With the luteolin is reference substance.
The preparation method of the activity extract of this Radix Lamiophlomidis Rotatae, be that the extracting solution that adopts the root of Radix Lamiophlomidis Rotatae medical material and/or herb to obtain by the general decoction and alcohol sedimentation technique of pharmaceutical technology or ethanol extract from water precipitation or alcohol percolation extraction method separates through a. macroporous resin adsorption or b. polyamide adsorbing separation or c. silica gel adsorption separate the solution that obtains, obtain activity extract after reclaiming solvent.
The Radix Lamiophlomidis Rotatae medical material that adopts can be separately with its root or use herb separately, also can be that root and herb mix use by arbitrary proportion, with the mixed proportion of root and herb is 1: 0.1～5 for good, is 1: 0.5～2 better through the test of pesticide effectiveness with the mixed proportion of root and herb.
Reclaim the activity extract that obtains behind the solvent, in order to extend the shelf life and to prepare the convenience and the convenient transportation of medicine, its activity extract is good to make dry product, so reclaim the concentrate that obtains behind the solvent, further preferred employing spray drying makes the dry powder into activity extract.
Said isolation and purification method is considered the preferred macroporous resin adsorption separation method of production cost in the preparation method of above-mentioned activity extract, be that extracting solution with the Radix Lamiophlomidis Rotatae medical material passes through macroporous resin adsorption, liquid to be extracted is all by behind the resin column, water flushing resin column, to water elution liquid near colourless till, continue and carry out eluting, collect ethanol elution with 20～80% ethanol.The type of macroporous resin is a lot, can adopt polar resin, nonpolar or low pole resin, and preferred macroporous resin nonpolar or low pole is good, as HPD-100, HPD-450, WLD, AB-8, ZTC-5 etc.
Narrate preparation method of the present invention below:
One, extract: the said decoction and alcohol sedimentation technique of a. is to take by weighing medicinal material coarse powder, decocts with water 1～3 time, and decocting liquid is concentrated, and adds ethanol and regulates determining alcohol to 30～70%, leave standstill, treat that precipitation fully after, inclining supernatant, filter, medicinal liquid is concentrated into 1: 0.5～2 concentration of suitable medical material amount, and is standby;
B. said ethanol extract from water precipitation is to take by weighing medicinal material coarse powder, adds 40%～90% alcohol reflux, reclaims ethanol, and medicinal liquid concentrates, add the suitable quantity of water mixing and stirring, leave standstill, treat that precipitation fully after, inclining supernatant, and medicinal liquid is concentrated into 1: 0.5～2 concentration of suitable medical material amount, and is standby;
C. said alcohol percolation extraction method is to take by weighing the Radix Lamiophlomidis Rotatae medicinal material coarse powder, after adding soak with ethanol, carry out percolation, collect percolate, reclaim ethanol, medicinal liquid concentrates, and adds the suitable quantity of water mixing and stirring, leaves standstill, after treating that precipitation fully, inclining supernatant, and medicinal liquid is concentrated into 1: 0.5～2 concentration of suitable medical material amount, and is standby;
Two, the above-mentioned further separation and purification of extracting solution:
A. above-mentioned medicinal liquid is passed through macroporous resin adsorption, treat that medicinal liquid is all by behind the resin column, water flushing resin column, to water elution liquid near colourless till, continue and the material that adsorbs on the resin column is carried out eluting with 20～80% ethanol, collect ethanol elution, promptly obtain the activity extract of Chinese medicine Radix Lamiophlomidis Rotatae behind the decompression and solvent recovery; Macroporous resin can adopt nonpolar or the low pole resin, is good with HPD-100, HPD-450, WLD, AB-8, ZTC-5.(excessive certain density Radix Lamiophlomidis Rotatae extracting solution respectively by the good resin column of pretreatment of different model, is carried out dynamic adsorption.After crossing post, wash earlier that to be eluted to eluent closely colourless with water, the ethanol-eluting resin column of reuse 70% is with the ethanol elution evaporate to dryness.Calculate respectively than upper column quantity, than adsorbance, eluting rate and purity)
B. polyamide adsorbing separation: above-mentioned medicinal liquid is concentrated, adsorb by polyamide, with methanol or ethanol by 10% graded to 95% eluting, collect middle polarity position (30%～80% methanol or 30%～95% ethanol), promptly obtain the activity extract of Chinese medicine Radix Lamiophlomidis Rotatae behind the decompression and solvent recovery.
C. silica gel adsorption separates: above-mentioned medicinal liquid is concentrated, and by silica gel adsorption, to 100% methanol, graded is to 10% methanol again by 4: 1 graded of chloroform-methanol for eluant; Or by 3: 1 graded of chloroform-ethanol to 95% ethanol, graded is to 10% ethanol again.(its eluant scope is: 2: 1 graded of chloroform-methanol are to 100% methanol, and graded is to 30% methanol again to collect the position of medium and high polarity; Or by 2: 1 graded of chloroform-ethanol to 95% ethanol, graded is to 30% ethanol again), the concentrate behind the decompression and solvent recovery promptly obtains the activity extract of Chinese medicine Radix Lamiophlomidis Rotatae.
Medicinal liquid 200ml with the alcohol extracting-water precipitating process is extracted passes through HPD-100 resin, 60～200 order silica gel and 60～200 order polyamide respectively.Carry out separation and purification by separately separation method.Collect eluent, survey general flavone content.And, measure the general flavone content in the dry substance with behind the eluent evaporate to dryness.
Three kinds of isolation and purification method experimental results
| Adsorption stuffing | Eluent general flavone content (mg) | Dry substance general flavone content (%) |
| The HPD-100 resin | 1386.1 | 72.38 |
| 60～200 order silica gel | 1126.2 | 77.62 |
| 60～200 order polyamide | 1287.4 | 79.13 |
Three, spray drying
With the above-mentioned ethanol elution that obtains through separation, reclaim ethanol, when being evaporated to relative density 1.05-1.1, spray drying is collected xeraphium, is the dry powder of the activity extract of Radix Lamiophlomidis Rotatae.
Another object of the present invention is the edge of a knife pain, hemorrhage after the activity extract of this Radix Lamiophlomidis Rotatae is used to prepare the treatment surgical operation, exogenous injury, and muscles and bones is sprained, rheumatic arthralgia and metrorrhagia, dysmenorrhea, gingival swelling and pain, sick medicine such as hemorrhage.
Said medicine can be with conventional method of Chinese medicinal, adds the adjuvant that pharmaceutically allows and makes the medicine of any oral formulations such as tablet, dispersible tablet, granule, capsule, mixture, oral liquid, syrup, pill etc., wherein preferred drop pill.The weight of each component is in its drop pill: 1 part in Radix Lamiophlomidis Rotatae activity extract dry powder, 0.5～4 part of Polyethylene Glycol.
Carry out the test of pesticide effectiveness with Radix Lamiophlomidis Rotatae extract below activity extract of the present invention and purposes are described.
One. analgesic experiment:
1, mice acetic acid twisting method:
Animal: healthy Kunming kind white mice, body weight 18-22g, male and female half and half.
Test method: animal is divided into blank group, 7 sample sets and positive drug matched group at random, weigh, labelling, successive administration 3 days, after the last administration 30 minutes, lumbar injection 0.6% acetic acid 0.1ml/ only, observe cause in 10 minutes turn round the body number of times.
Result: see the following form
Table 1 is turned round the different extracts of body measuring to the analgesic effect of mice (X ± SD)
| Group | Dosage (g/kg) | Number of animals | Turn round the body number of times | P |
| Normal control | 12 | 42.33±9.3 | ||
| Dolantin | 0.05 | 12 | 10.5±3.8 | ＜0.01 |
| Pharmacopeia Radix Lamiophlomidis Rotatae capsule sample (Guangzhou factory product) | 1.2 | 12 | 29.8±8.8 | ＞0.05 |
| Radix Lamiophlomidis Rotatae root extract dry powder | 0.06 | 12 | 18.16±6.3 | ＜0.01 |
| Radix Lamiophlomidis Rotatae herb extract dry powder | 0.06 | 12 | 23.08±7.3 | ＜0.01 |
| Radix Lamiophlomidis Rotatae root: the extract dry powder of 1: 0.1 mixture of herb | 0.06 | 12 | 18.56±5.3 | ＜0.01 |
| Radix Lamiophlomidis Rotatae root: the extract dry powder of 1: 1 mixture of herb | 0.06 | 12 | 10.58±3.8 | ＜0.01 |
| Radix Lamiophlomidis Rotatae root: the extract dry powder of 1: 2 mixture of herb | 0.06 | 12 | 17.24±6.8 | ＜0.01 |
| Radix Lamiophlomidis Rotatae root: the extract dry powder of 1: 5 mixture of herb | 0.06 | 12 | 19.34±4.9 | ＜0.01 |
Show that each extract of Radix Lamiophlomidis Rotatae of the present invention all can reduce the writhing response number of times of mice, analgesic activity is arranged, and the analgesic effect of the activity extract of Radix Lamiophlomidis Rotatae root and herb mixture is better, has compared notable difference with normal group.
2, hot plate method:
Animal: healthy Kunming kind white mice, body weight 18-22g all is male.
Test method: animal is divided into blank, 7 sample sets and positive drug matched group at random, weighs, labelling, and each organized according to dosage successive administration 7 days, and list of references uses hot plate method, measures the mice pain threshold of last administration respectively.
Result: see Table 2
Table 2 hot plate method is measured different extracts to the analgesic effect of mice (X ± SD)
| Group | Dosage (g/kg) | Number of animals | Lick the sufficient time (S) | P |
| Normal control | 12 | 15.4±8.6 | ||
| Dolantin | 0.05 | 12 | 35.9±15.2 | ＜0.01 |
| Pharmacopeia Radix Lamiophlomidis Rotatae capsule sample (Guangzhou factory product) | 1.2 | 12 | 21.8±12.9 | ＞0.05 |
| Radix Lamiophlomidis Rotatae root extract dry powder | 0.06 | 12 | 25.8±6.30 | ＜0.05 |
| Radix Lamiophlomidis Rotatae herb extract dry powder | 0.06 | 12 | 26.6±19.8 | ＜0.05 |
| Radix Lamiophlomidis Rotatae root: 1: 0.1 mixed extract dry powder of herb | 0.06 | 12 | 26.8±11.3 | ＜0.05 |
| Radix Lamiophlomidis Rotatae root: 1: 1 mixed extract dry powder of herb | 0.06 | 12 | 33.2±18.6 | ＜0.01 |
| Radix Lamiophlomidis Rotatae root: 1: 2 mixture extract dry powder of herb | 0.06 | 12 | 27.2±7.2 | ＜0.05 |
| Radix Lamiophlomidis Rotatae root: 1: 5 mixture extract dry powder of herb | 0.06 | 12 | 25.2±18.6 | ＜0.05 |
The result shows that the analgesic effect of activity extract of Radix Lamiophlomidis Rotatae is better, and is obvious with blank group contrast difference, and analgesic activity is all arranged.
Two, hemostasis experiment
1. cut the tail method: the results are shown in Table 3:
The different extracts of table 3 are to the influence in normal mouse bleeding time (X ± SD)
| Group | Dosage (g/kg) | Number of animals | Bleeding stopping period (S) | P |
| Normal control | 12 | 100.1±20.1 | ||
| Pharmacopeia Radix Lamiophlomidis Rotatae capsule sample (Guangzhou factory product) | 1.2 | 12 | 85.6±20.8 | ＞0.05 |
| Radix Lamiophlomidis Rotatae root extract dry powder | 0.06 | 12 | 73.3±23.0 | ＜0.05 |
| Radix Lamiophlomidis Rotatae herb extract dry powder | 0.06 | 12 | 80.4±18.4 | ＜0.05 |
| Radix Lamiophlomidis Rotatae root: 1: 0.1 mixture extract dry powder of herb | 0.06 | 12 | 75.2±16.2 | ＜0.05 |
| Radix Lamiophlomidis Rotatae root: 1: 1 mixture extract dry powder of herb | 0.06 | 12 | 62.62±18.6 | ＜0.01 |
| Radix Lamiophlomidis Rotatae root: 1: 2 mixture extract dry powder of herb | 0.06 | 12 | 74.61±12.3 | ＜0.05 |
| Radix Lamiophlomidis Rotatae root: 1: 5 mixture extract dry powder of herb | 0.06 | 12 | 79.25±8.9 | ＜0.05 |
Animal: get healthy Kunming kind white mice, body weight 18-22g, male and female half and half.
Test method: animal is divided into blank, 7 sample sets at random, weigh, labelling, successive administration 7 days, fixing after the last administration, measure Mus tail length and labelling, respectively that mouse tail point 3mm place is cross-section after 30-40 minute, treating that blood overflows voluntarily picks up counting, inhale to dehematize with filter paper every 30s and drip, stop naturally, calculate the bleeding time until blood.
The result shows that the haemostatic effect of activity extract of Radix Lamiophlomidis Rotatae is better, and is obvious with blank group contrast difference, and anastalsis is all arranged.
2, slide method
Animal: get healthy Kunming kind white mice, body weight 18-22g, male and female half and half.
Test method: animal is divided into blank, 7 sample sets at random, weigh, labelling, each sample mice is established 3 oral doses, after the last administration 30 minutes, each eyeball of mouse blood in the microscope slide two ends, using manual time-keeping immediately, whether have the blood streak produce, the record clotting time if observing every 30 seconds.Result: see Table 4
The different extracts of table 4 are to the influence of normal clotting time of mice (X ± SD)
| Group | Dosage (g/kg) | Number of animals | Clotting time (S) | P |
| Normal control | 12 | 135.83±19.77 | ||
| Pharmacopeia Radix Lamiophlomidis Rotatae capsule sample (Guangzhou factory product) | 1.2 | 12 | 102.50±8.29 | ＜0.01 |
| Radix Lamiophlomidis Rotatae root extract dry powder | 0.06 | 12 | 95.8±6.30 | ＜0.01 |
| Radix Lamiophlomidis Rotatae herb extract dry powder total flavones | 0.06 | 12 | 111.67±9.86 | ＞0.01 |
| Radix Lamiophlomidis Rotatae root: 1: 0.1 mixture extract dry powder of herb | 0.06 | 12 | 97.3±8.58 | ＜0.01 |
| Radix Lamiophlomidis Rotatae root: 1: 1 mixture extract dry powder of herb | 0.06 | 12 | 75.42±24.19 | ＜0.01 |
| Radix Lamiophlomidis Rotatae root: 1: 2 mixture extract dry powder of herb | 0.06 | 12 | 89.42±14.13 | ＜0.01 |
| Radix Lamiophlomidis Rotatae root: 1: 5 mixture extract dry powder of herb | 0.06 | 12 | 105.42±24.19 | ＞0.01 |
The result shows that activity extract provided by the invention is compared the clotting time that can obviously shorten mice with matched group.
The invention has the beneficial effects as follows:
1, the crude extract of medical material is purified to effective site further the separation, has improved curative effect of medication, reduced each dose of patient.
2, the characteristics of this medicine are: be used for the edge of a knife pain, hemorrhage behind the surgical operation, and exogenous injury, muscles and bones is sprained, rheumatic arthralgia and metrorrhagia, dysmenorrhea, gingival swelling and pain, hemorrhage etc., but not only pain relieving but also can stop blooding.
3, preparation method provided by the invention is suitable for industrialized mass production.
Set forth technical scheme of the present invention below in conjunction with embodiment
The specific embodiment
One, extract three kinds of processes of Radix Lamiophlomidis Rotatae medical material:
Embodiment 1, decoction and alcohol sedimentation technique: take by weighing the herb of Radix Lamiophlomidis Rotatae and the coarse powder of root (1: 1), mix homogeneously decocts with water 2 times, merges each time decocting liquid, concentrates, and adds ethanol and regulates determining alcohol to 60%, leaves standstill.After treating that precipitation fully, inclining supernatant, filters, and medicinal liquid is concentrated into 1: 2 concentration of suitable medical material amount, and is standby;
Embodiment 2, ethanol extract from water precipitation: take by weighing the herb of Radix Lamiophlomidis Rotatae and the coarse powder of root (1: 1), mix homogeneously adds 60% alcohol reflux 3 times, merges alcohol extract, reclaims ethanol, and medicinal liquid is concentrated into relative density 1.0-1.2, adds the suitable quantity of water mixing and stirring, leaves standstill.After treating that precipitation fully, inclining supernatant, filters, and medicinal liquid is concentrated into 1: 2 concentration of suitable medical material amount, and is standby;
Embodiment 3, alcohol percolation extraction method: take by weighing the herb of Radix Lamiophlomidis Rotatae and the coarse powder of root (1: 1), mix homogeneously, add 70% soak with ethanol after, carry out diafiltration with 5ml/ minute speed, collect percolate, reclaim ethanol, medicinal liquid is concentrated into relative density 1.2, adds the suitable quantity of water mixing and stirring, leaves standstill.After treating that precipitation fully, inclining supernatant, filters, and medicinal liquid is concentrated into 1: 2 concentration of suitable medical material amount, and is standby;
With the medicinal liquid of embodiment 1,2, the 3 three kind of process for extracting macropore resin isolation eluting that used the same method respectively, be condensed into extractum after reclaiming ethanol, spray drying obtains dry powder, and measurement result sees the following form;
Three kinds of extracting method measurement results of table 5
| Process | Inventory | Concentrated solution | Dry powder | General flavone content |
| Embodiment 1 | 20Kg | 40L | 1015g | 70.3％ |
| Embodiment 2 | 20Kg | 40L | 982g | 74.1％ |
| Embodiment 3 | 20Kg | 40L | 935g | 67.9％ |
Two, further isolation and purification method
Embodiment 4, the further separation and purification of extraction concentrated solution of getting the foregoing description 2:
Above-mentioned medicinal liquid 200ml is carried out dynamic adsorption by AB-8 macroporous resin 15g, flow velocity is about 1ml/min, treat that medicinal liquid is all by behind the resin column, water flushing resin column, to water elution liquid near colourless till, continuously the material that adsorbs on the resin column is carried out eluting with 70% ethanol, elution flow rate is 1ml/min, collect ethanol elution, promptly obtain the activity extract of Radix Lamiophlomidis Rotatae behind the decompression and solvent recovery.
Embodiment 5, the further separation and purification of extraction concentrated solution of getting the foregoing description 2:
Above-mentioned medicinal liquid 200ml is carried out dynamic adsorption by HPD-100 macroporous resin 15g, treat medicinal liquid all by behind the resin column, water flushing resin column, to water elution liquid near colourless till, continue and with 20% ethanol the material that adsorbs on the resin column is carried out eluting, other is operated with embodiment 4.
Embodiment 6, the further separation and purification of extraction concentrated solution of getting the foregoing description 2:
Above-mentioned medicinal liquid 200ml is carried out dynamic adsorption by WLD macroporous resin 15g, treat that medicinal liquid is all by behind the resin column, water flushing resin column, to water elution liquid near colourless till, continue and the material that adsorbs on the resin column is carried out eluting with 80% ethanol, collect ethanol elution, other is operated with embodiment 4.
Embodiment 7, the further separation and purification of extraction concentrated solution of getting the foregoing description 2:
Above-mentioned medicinal liquid 200ml is carried out dynamic adsorption by HPD-450 macroporous resin 15g, treat medicinal liquid all by behind the resin column, water flushing resin column, to water elution liquid near colourless till, continue and with 50% ethanol the material that adsorbs on the resin column is carried out eluting, other is operated with embodiment 4.
Embodiment 8, the further separation and purification of extraction concentrated solution of getting the foregoing description 2:
Above-mentioned medicinal liquid 200ml is carried out dynamic adsorption by the ZTC-5 macroporous resin, treat medicinal liquid all by behind the resin column, water flushing resin column, to water elution liquid near colourless till, continue and with 50% ethanol the material that adsorbs on the resin column is carried out eluting, other is operated with embodiment 4.
Embodiment 9, the further separation and purification of extraction concentrated solution of getting the foregoing description 2:
Above-mentioned medicinal liquid 200ml is carried out dynamic adsorption by AB-8 macroporous resin 15g, treat medicinal liquid all by behind the resin column, water flushing resin column, to water elution liquid near colourless till, continue and with 50% ethanol the material that adsorbs on the resin column is carried out eluting, other is operated with embodiment 4.
The results are shown in following table.
| Embodiment | Dry powder (g) | General flavone content (%) | Content of luteolin (%) |
| 4 | 5.54 | 79.36 | 4.10 |
| 5 | 5.38 | 67.21 | 1.83 |
| 6 | 4.25 | 70.87 | 3.12 |
| 7 | 5.67 | 53.11 | 0.62 |
| 8 | 3.71 | 50.12 | 2.39 |
| 9 | 5.68 | 76.26 | 2.86 |
Three, spray drying
Embodiment 10, the extraction concentrated solution that the foregoing description 2 is obtained are crossed the ethanol elution behind the macroporous resin, method is as embodiment 4, reclaim ethanol, when being evaporated to relative density 1.05-1.1, spray drying is collected xeraphium, promptly obtains the dry powder 982g of Radix Lamiophlomidis Rotatae activity extract, content of total flavone is 74.1%, content of luteolin 2.12%
Spray drying condition: 85 ℃ of inlet temperature; 135 ℃ of leaving air temps.
Content of total flavone is measured and the content of luteolin assay method is seen Chinese Pharmacopoeia.
Set forth purposes of the present invention with embodiment below.
Embodiment A, tablet:
Take by weighing dry powder 150 grams of the Radix Lamiophlomidis Rotatae activity extract that embodiment 10 makes, mixes pulverizings in right amount, mistake 100 mesh sieves, ethanol wet granulation, an amount of magnesium stearate mixed pressuring plate of adding behind the dry granulate with 95% with 15% carboxymethyl starch sodium, PVP etc.Make 1000, every heavily about 0.3g, oral, each a slice, every day 3 times.
Embodiment B, capsule:
Take by weighing the dry powder 150g of the Radix Lamiophlomidis Rotatae activity extract that embodiment 10 makes, add an amount of adjuvant, cross 100 mesh sieves, dry pressing or wet granulation, oven dry pours into capsule No. 1, makes 1000, every heavily about 0.25g, each 1, every day 3 times.
Embodiment C, dispersible tablet
Take by weighing dry powder 150 grams of the Radix Lamiophlomidis Rotatae activity extract that embodiment 10 makes, mix pulverizing with 10% carboxymethyl starch sodium, cross 100 mesh sieves, add an amount of low substituted hydroxy-propyl methylcellulose, with polyvinylpyrrolidone ethanol liquid system soft material, wet granulation adds an amount of magnesium stearate mixed pressuring plate behind the dry granulate.Make 1000, every heavily about 0.3g, oral, each a slice, every day 3 times.Press the inspection of Chinese Pharmacopoeia method disintegration, sample should disintegrate in 3 minutes.
Embodiment D, oral liquid
Take by weighing behind the concentrated solution after embodiment 3 extracts the about 15g of extractum that the method separation and purification with embodiment 4 obtains, add the small amount of thermal water dissolution, stir evenly, add an amount of simple syrup, add water to 1000ml, regulate pH value to 6～7, filtration, embedding is sterilized, promptly.Specification: 10ml/ props up, and is oral, and each one, every day 3 times.
Embodiment E, drop pill
Get the dry powder 250g of the Radix Lamiophlomidis Rotatae activity extract of embodiment 10, pulverize, cross 120 mesh sieves, join in the mixed liquor of the fused polyethylene glycol 6000 of about 350g and 4000, fully mix, on the drop pill machine, drip and make 10000 drop pill, every heavily about 60mg with 70～90 ℃ fluid temperature.Oral, each 6, every day 3 times.
Embodiment F, syrup:
Take by weighing behind the concentrated solution after embodiment 3 extracts the about 15g of extractum that the method separation and purification with embodiment 4 obtains, add the small amount of thermal water dissolution, stir evenly, add an amount of simple syrup, add water to 1000ml, regulate pH value to 6～7, filtration, embedding is sterilized, promptly.Specification: the 100ml/ bottle, oral, each oral 10ml, every day 3 times.
Embodiment G, granule
Take by weighing behind the concentrated solution after embodiment 3 extracts the about 75g of extractum that the method separation and purification with embodiment 4 obtains, add an amount of lactose and dextrin mix homogeneously, wet granulation, dry granulate, branch is packed.Make 1000g, every bag 2g.Oral, each bag, every day 3 times.
Claims (5)
1, a kind of activity extract of Radix Lamiophlomidis Rotatae, be by labiate Radix Lamiophlomidis Rotatae medical material, comprise root or the dry herb extracting solution after ethanol extract from water precipitation extracts, through further separating the activity extract that obtains, it is characterized in that: the root and/or the extracting solution of herb after ethanol extract from water precipitation extracts that adopt the Radix Lamiophlomidis Rotatae medical material, extracting solution is closely colourless through the non-polar macroporous resin absorption back water eluting of HPD-100 type, continuous 20% ethanol elution of using; Or extracting solution is closely colourless through the non-polar macroporous resin absorption back water eluting of WLD type, continues the ethanol elution with 80%; Or extracting solution is closely colourless through the non-polar macroporous resin absorption back water eluting of ZTC-5 type, continues the ethanol elution with 20%; Or extracting solution through AB-8 type low pole macroporous resin adsorption after, the water eluting is closely colourless, and is continuous with 50% or 70% ethanol elution; Collect ethanol elution, obtain activity extract after reclaiming solvent, the dry product of its activity extract contains total flavones, and to reach percent by weight in rutin be 50～80%, and containing luteolin, to reach percent by weight be 1.83-4.10%.
2, a kind of preparation method of the activity extract as the said Radix Lamiophlomidis Rotatae of claim 1, adopt the root of Radix Lamiophlomidis Rotatae medical material and/or the extracting solution that herb obtains by the general ethanol extract from water precipitation of pharmaceutical technology, it is characterized in that: extracting solution is all behind the non-polar macroporous resin post by the HPD-100 type, water flushing resin column, to water elution liquid near colourless till, continuous 20% ethanol elution of using; Or extracting solution is all by water flushing resin column behind the non-polar macroporous resin post of WLD type, to water elution liquid near colourless till, continuous with 80% ethanol elution; Or extracting solution is all by water flushing resin column behind the non-polar macroporous resin post of ZTC-5 type, to water elution liquid near colourless till, continuous with 20% ethanol elution; Or extracting solution is all by after the AB-8 type low pole macroporous resin column, water flushing resin column, to water elution liquid near colourless till, continuous with 50% or 70% ethanol elution; Collect ethanol elution, obtain activity extract behind the recovery solvent.
3, according to the preparation method of the activity extract of the said Radix Lamiophlomidis Rotatae of claim 2, it is characterized in that: said Radix Lamiophlomidis Rotatae medical material is the mixture of its root and herb, and mixed proportion is 1: 0.1～5.
4, according to the preparation method of the activity extract of the said Radix Lamiophlomidis Rotatae of claim 3, it is characterized in that: said Radix Lamiophlomidis Rotatae medical material is the mixture of its root and herb, and mixed proportion is 1: 0.5～2.
5, according to the preparation method of the activity extract of the said Radix Lamiophlomidis Rotatae of claim 2, it is characterized in that: reclaim the concentrate that obtains behind the solvent, further carry out the dry powder that spray drying makes activity extract.
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| CN100540014C (en) * | 2005-06-10 | 2009-09-16 | 广州陈李济药厂 | A kind of plant extract and its Preparation method and use |
| CN101380356B (en) * | 2008-10-14 | 2012-12-19 | 沈阳药科大学 | Tibetan medicine Duyiwei total flavone extract and extraction method and use thereof |
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| CN1502328A (en) * | 2002-11-26 | 2004-06-09 | 李雪晶 | Lamiophlomis rotate dispersion table preparation process |
| CN1526421A (en) * | 2003-03-07 | 2004-09-08 | 周美华 | Prepn of single ingredient granule |
| CN1562310A (en) * | 2004-04-20 | 2005-01-12 | 成都优他制药有限责任公司 | Soft capsule preparation of Tibet medicine 'unique taste' |
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| CN1502328A (en) * | 2002-11-26 | 2004-06-09 | 李雪晶 | Lamiophlomis rotate dispersion table preparation process |
| CN1526421A (en) * | 2003-03-07 | 2004-09-08 | 周美华 | Prepn of single ingredient granule |
| CN1562310A (en) * | 2004-04-20 | 2005-01-12 | 成都优他制药有限责任公司 | Soft capsule preparation of Tibet medicine 'unique taste' |
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