CN1686334A - Hedyotis herba powder injection and its preparation method - Google Patents
Hedyotis herba powder injection and its preparation method Download PDFInfo
- Publication number
- CN1686334A CN1686334A CN 200510055292 CN200510055292A CN1686334A CN 1686334 A CN1686334 A CN 1686334A CN 200510055292 CN200510055292 CN 200510055292 CN 200510055292 A CN200510055292 A CN 200510055292A CN 1686334 A CN1686334 A CN 1686334A
- Authority
- CN
- China
- Prior art keywords
- hedyotidis diffusae
- herba hedyotidis
- ethanol
- polysaccharide
- herba
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Landscapes
- Medicinal Preparation (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
A powder injection for suppressing tumor is prepared from oldenlandia through extracting, purifying and mixing with medicinal auxiliaries.
Description
Affiliated technical field
The invention belongs to field of traditional Chinese medicine pharmacy, be specifically related to a kind of hedyotis herba powder injection and preparation method thereof.
Technical background
Herba Hedyotidis Diffusae has another name called Herba Hedyotidis Diffusae, Chinese Lobelia, Radix Picriae felterrae etc., dry herb for Rubiaceae cerastium plant Herba Hedyotidis Diffusae, effect such as have heat-clearing and toxic substances removing, activating blood circulation to dissipate blood stasis, dampness removing is treating stranguria, be used for treatment of diseases such as hepatitis, enteritis, pneumonia, tumor, its preparation Herba Hedyotidis Diffusae has heat-clearing and toxic substances removing, inducing diuresis and reducing edema effect, the infection and the post-operative infection that are used for the respiratory tract etc. due to damp and hot also can be used for the auxiliary treatment of cancer.
Herba Hedyotidis Diffusae contains effective ingredient such as anthraquinone class, flavonoid, cyclenes ether glycosides terpenoid, sterols, alkanes, polysaccharide, consult document, we learn that the Herba Hedyotidis Diffusae liposoluble constituent has unstability in aqueous solution, therefore BAIHUASHESHECAO ZHUSHEYE is in the preservation process, very high to environmental requirement, be unfavorable for the transportation and the application of BAIHUASHESHECAO ZHUSHEYE, and prolongation in time causes drug effect to descend; BAIHUASHESHECAO ZHUSHEYE can be used for the auxiliary treatment of cancer, liposoluble constituent has certain anti-tumor activity in the Herba Hedyotidis Diffusae, but its main anti-tumor active ingredient is a water soluble ingredient, have good antitumor activity (" the different extraction processes of Herba Hedyotidis Diffusae are to the influence of anti-tumor activity ", China Medicine University's journal, 2002 and from water soluble ingredient, isolate polysaccharide component, 33 (6): 510-513), therefore, should keep this active component in the preparation, and standard No. is WS
3Use methods such as 80% ethanol percolate extraction in the preparation method of-B-3176-98 BAIHUASHESHECAO ZHUSHEYE, not only expended a large amount of ethanol and time, and caused losing of the good polysaccharide component of anti-tumor activity, cause the wasting of resources.Therefore, to contain the ejection preparation of Herba Hedyotidis Diffusae polysaccharide, effective ingredient such as fat-soluble be a lot of medical workers' hope for research invention.
Consult document and patent, not retrieving with the Herba Hedyotidis Diffusae is the injectable powder of feedstock production.
Summary of the invention
For these reasons, the method that the present invention adopts ultrasonic alcohol extraction, alkaline ethanol precipitation, hydrochloric acid to regulate pH value obtains ethanol extract, the residue water extraction that extracts, the method for ultrafiltration obtain polysaccharide, add pharmaceutic adjuvant, be prepared into injectable powder, total flavones (in rutin) must not be less than the 0.60mg/ bottle in the control injectable powder, and the control polyoses content is not less than the 16.0mg/ bottle; The present invention adopts the method for supersound extraction, has shortened extraction time, has reduced consumption of ethanol, and this method extracts the good polysaccharide component of anti-tumor activity on the basis that has kept liposoluble constituent; The pharmacological results shows, compares with veriety with commercially available, has better pharmacological action.The present invention is achieved through the following technical solutions.
One. process recipes
(1) gets Herba Hedyotidis Diffusae, pulverize, put into the supersound extraction jar, with concentration is ethanol extraction 10-15 minute of 70%-90%, extracting liquid filtering, and residue is standby, filtrate recycling ethanol adds crude drug amount 4-6 1% potassium hydroxide-alcoholic solution doubly to the greatest extent, leaves standstill, centrifugal, get supernatant, add hydrochloric acid and regulate pH value to 5, centrifugal, get supernatant, Rotary Evaporators concentrates, 30-40 ℃ of control temperature, cold drying obtains the Herba Hedyotidis Diffusae ethanol extract;
(2) get above-mentioned residue, drying, extracting in water 2-4 time, each 2-4 hour, merge extractive liquid, filtered, relative density is 1.05-1.10 when being concentrated to 50 ℃, with the filter element coarse filtration of 0.1um, filtrate is earlier 100000 hollow fiber column ultrafilter with molecular cut off, keeps permeate, the reuse molecular cut off is 3000 ultrafilter membrane bag ultrafiltration, keep circulation fluid, the circulation fluid drying obtains Herba Hedyotidis Diffusae polysaccharide;
(3) preparation prescription of the present invention is:
Herba Hedyotidis Diffusae ethanol extract 40-60 weight portion, Herba Hedyotidis Diffusae polysaccharide 16-23 weight portion, pharmaceutic adjuvant are weight portion 117-144;
(4) with Herba Hedyotidis Diffusae ethanol extract, polysaccharide, add the water for injection dissolving fully, to filter, filtrate adds pharmaceutic adjuvant, filters, sterilization, drying obtains hedyotis herba powder injection.
Two. the check and analysis experiment
1. the check and analysis of total flavones
The preparation of reference substance solution: precision takes by weighing at the control substance of Rutin 10mg of 120 ℃ of drying under reduced pressure to constant weight, puts in the 50ml measuring bottle, adds an amount of 70% ethanol, put that slight fever makes dissolving in the water-bath, put coldly, add 70% ethanol to scale, shake up, promptly get (containing anhydrous rutin 0.2mg among every 1ml).
The preparation of standard curve: precision is measured reference substance solution 0.0,1.0,2.0,3.0,4.0,5.0 and 6.0ml, put respectively in the 25ml measuring bottle, respectively add 70% ethanol to 6ml, add 5% sodium nitrite solution 1ml, shake up, placed 6 minutes, add 10% aluminum nitrate solution 1ml, shake up, placed 6 minutes, hydro-oxidation sodium test solution 10ml adds ethanol again to scale, shake up, placed 15 minutes, and, measured trap at the wavelength place of 507nm according to spectrophotography (appendix VB), with the trap is that vertical coordinate, concentration are abscissa, the drawing standard curve.
Algoscopy: precision takes by weighing injectable powder 100mg of the present invention, is added on the polyamide column (50 orders, the 2g that have handled well, internal diameter 12～15mm, wet method dress post) on, use the 50ml water elution, discard eluent, use 70% ethanol elution, collect the about 25ml of eluent, put in the 25ml measuring bottle, add 70% ethanol dilution, shake up to scale, precision is measured 5ml respectively, puts first, in two 25ml measuring bottles of second, add 5% sodium nitrite solution 1ml in the first bottle, shake up, placed 6 minutes, add 10% aluminum nitrate solution 1ml, shake up, placed 6 minutes, in first, each hydro-oxidation sodium test solution 10ml in two bottles of the second, add ethanol dilution again to scale, shake up, placed 15 minutes, according to spectrophotography, with the second bottle is blank, measure trap at the wavelength place of 507nm, read the amount of rutin the need testing solution, calculate from standard curve, that is, result of calculation sees Table 1:
2. polysaccharide check and analysis
Standard curve is drawn: the electronic balance precision takes by weighing the 100.0mg anhydrous glucose, in the rearmounted 500mL volumetric flask of dissolved in distilled water, add the distilled water standardize solution, shake up, promptly get the titer of 0.2mgmL-1, draw 0.0mL, 1.0mL, 5.0mL, 10.0mL, 15.0mL, 20.0mL glucose standard solution respectively to the 50mL volumetric flask with pipet, add distilled water and be settled to 20mL.Draw 1.0mL respectively to test tube with liquid-transfering gun, add 6% phenol solution 1.0mL, 95.5% concentrated sulphuric acid 5.0mL leaves standstill 10min, shakes up, and room temperature is surveyed absorbance in 490nm after placing 20min, obtains standard curve according to experimental result.
Conversion factor is measured: accurately take by weighing injectable powder 20.0mg of the present invention, place the 50mL volumetric flask, add the distilled water dilution and be settled to scale, shake up, accurately draw 1.0mL solution in test tube, the phenol solution 1.0mL of adding 6%, 95.5% concentrated sulphuric acid 5.0mL leaves standstill 10min, shakes up, room temperature is surveyed absorbance in 490nm after placing 20min, substitution standard curve equation gets free concentration of glucose in the polysaccharide, and (C * D), W is an injectable powder weight of the present invention in the formula to be calculated as follows conversion factor f:f=W/, C is a concentration of glucose, and D is the rare multiple of polysaccharide.Record f=2.134.
Determination of polysaccharide: precision takes by weighing injectable powder 20.0mg of the present invention, uses dissolved in distilled water, to the 50mL volumetric flask, and the adding distil water standardize solution.Accurately draw the 1.0mL polysaccharide solution in test tube with pipet, add 6% phenol solution 1.0mL, add 95.5% concentrated sulphuric acid 5.0mL immediately, shake up, put 40 ℃ of heating in water bath 10min, room temperature leaves standstill behind the 20min in 490nm place photometry density value.The glucose content that the polysaccharide sample produces after the concentrated sulphuric acid hydrolysis will be calculated in the standard curve of the data substitution glucose solution of gained.Be calculated as follows the polyoses content in the sample: polyoses content (%)=C * D * fW * 100, C is for supplying concentration of glucose (mgmL-1) in the test agent in the formula, and D is the extension rate of test liquid, and f is a conversion factor, and W is for supplying test agent weight (mg).Experimental result sees Table 1:
Table 1 powder injection formulation active constituent content of the present invention detects
| Group | General flavone content (in rutin) mg/ bottle | Polyoses content mg/ bottle |
| 123 meansigma methodss | ??0.72 ??0.75 ??0.72 ??0.73 | ??20.16 ??20.87 ??20.45 ??20.49 |
According to above-mentioned same method, (three nine-day periods after the winter solstice enterprise group Anhui three nine-day periods after the winter solstice pharmaceutcal corporation, Ltd) carries out check and analysis to commercially available BAIHUASHESHECAO ZHUSHEYE, the results are shown in Table 2:
The commercially available BAIHUASHESHECAO ZHUSHEYE active constituent content of table 2 detects
| Group | General flavone content (in rutin) mg/ bottle | Polyoses content mg/ bottle |
| 123 meansigma methodss | ??0.58 ??0.57 ??0.55 ??0.57 | ??- ??- ??- ??- |
Annotate: representative does not detect among-the Biao
Conclusion: by above-mentioned check and analysis experiment, show that technology of the present invention makes that the alcohol extraction effective ingredient has improved more than 20% in the preparation, kept anti-tumor active ingredient polysaccharide component preferably, prove absolutely that technology of the present invention has practical significance.
Three. preparation stability is investigated
Experiment medicine: lyophilized injectable powder of the present invention (Tianzhijiao Medication Development Co., Ltd., Guangdong's laboratory provides) BAIHUASHESHECAO ZHUSHEYE (three nine-day periods after the winter solstice enterprise group Anhui three nine-day periods after the winter solstice pharmaceutcal corporation, Ltd)
Experimental technique: is 45%-55% with two kinds of preparations in humidity, temperature is to store 18 months under 18-25 ℃ the external environment, avoid sun exposure, take out two kinds of preparations at 0,3,6,12,18 month respectively and carry out check and analysis (detection method is the same), investigate preparation stability, experimental result sees Table 3:
Table 3 stability of formulation is investigated
| Group | 0 month general flavone content mg/ bottle | 3 months general flavone content mg/ bottles | 6 months general flavone content mg/ bottles | 12 months general flavone content mg/ bottles | 18 months general flavone content mg/ bottles |
| Commercially available BAIHUASHESHECAO ZHUSHEYE injectable powder of the present invention | ??0.56 ? ??0.74 | ??0.50 ? ??0.73 | ??0.39 ? ??0.68 | ??0.31 ? ??0.65 | ??0.29 ? ??0.61 |
Conclusion: by the aforementioned stable investigation, we can analyze, commercially available BAIHUASHESHECAO ZHUSHEYE in the time of 18 months loss of effective components nearly 50%, and injectable powder effective ingredient of the present invention has kept more than 80%, therefore, prove absolutely that preparation of the present invention has good stability.
Four. the comparison of process
Experimental technique: one group: carry out according to process of the present invention.
Two groups: according to standard No. is WS
3The preparation method of-B-3176-98 BAIHUASHESHECAO ZHUSHEYE is carried out.
Experimental technique: according to the method described above, get the Herba Hedyotidis Diffusae of equal in quality, carry out extraction separation after, drying is investigated ethanol consumption, extraction time, extraction ratio of effective constituents, experimental result sees Table 4:
Table 4 experimental technique relatively
| Group | Extraction time hour | Ethanol consumption liter | Total flavones extraction ratio % | Polysaccharide extract rate % |
| One group two groups | ??3.5 ??28.5 | ??10 ??89 | ??85.2 ??74.3 | ??86.4 ??- |
Annotate :-representative does not detect
Conclusion:, show that further technology of the present invention has practical significance by above-mentioned experiment.
Three. pharmacology embodiment
Embodiment 1
Xylol causes the influence of mice auricular concha inflammation
Experiment medicine: lyophilized injectable powder of the present invention (Tianzhijiao Medication Development Co., Ltd., Guangdong's laboratory provides) BAIHUASHESHECAO ZHUSHEYE (three nine-day periods after the winter solstice enterprise group Anhui three nine-day periods after the winter solstice pharmaceutcal corporation, Ltd)
Normal saline (Tianzhijiao Medication Development Co., Ltd., Guangdong's laboratory provides)
Laboratory animal: Kunming mouse (20 ± 2) g, male and female dual-purpose.
Experimental technique: 30 of mices, be divided into 3 groups, 10 every group, with the solution of injectable powder of the present invention with the identical crude drug amount of water for injection dissolving with BAIHUASHESHECAO ZHUSHEYE, give the mouse tail vein administration according to 0.3g crude drug/kg dosage, every day 1 time, administration 3 days, normal saline group administration capacity 0.5ml/ is only, every day 1 time, administration 3 days, 1h after the last administration, get dimethylbenzene 0.05ml/ only evenly be applied to left ear before and after the two sides cause inflammation, behind the 15min, put to death animal, cut auricular concha, two ears are overlapping, get disk with diameter for the 8mm card punch, weighing, the difference that left and right sides ear weighs is obtained the inhibitory rate of intumesce of administration group as the swelling degree.The results are shown in Table 5:
Table 5 xylol causes the influence of mice auricular concha inflammation
| Group | Number of animals (only) | Swelling degree (mg) | Suppression ratio (%) |
| Normal saline BAIHUASHESHECAO ZHUSHEYE injectable powder of the present invention | ??10 ??10 ??10 | ??21.63±6.3 ??16.24±5.2 **??10.22±4.1 **[ *] | ??- ??24.9 ??52.8[ *] |
Annotate: compare with the normal saline group
*P＜0.01, compare with positive controls [
*] P＜0.05
Embodiment 2
Influence to mouse lymphocyte propagation and antibody generation
Laboratory animal: 24 of kunming mices, body weight 18～22g, male and female are not limit.
Experiment medicine: lyophilized injectable powder of the present invention (Tianzhijiao Medication Development Co., Ltd., Guangdong's laboratory provides)
BAIHUASHESHECAO ZHUSHEYE (three nine-day periods after the winter solstice enterprise group Anhui three nine-day periods after the winter solstice pharmaceutcal corporation, Ltd)
Normal saline (Tianzhijiao Medication Development Co., Ltd., Guangdong's laboratory provides)
Experimental technique: get mice, random packet, 12 every group.Administration group tail intravenously administrable, dosage is 0.3g crude drug/kg, matched group gives normal saline 0.5ml/ time; Test 5d and respectively 5% sheep red blood cell (SRBC) 0.2ml injection is respectively organized in the mouse peritoneal, the blood-letting of 11d eyeball, the cervical vertebra dislocation is put to death, and routine is got spleen, carries out the splenocyte counting then, transfers cell concentration to 1 * 10
7/ ml, extracting spleen cell 1ml, 1: 10 fresh guinea pig serum (complement) 1ml, 0.2% sheep red blood cell (SRBC) 1ml, mixing, 37 ℃ of water-bath 1h, the centrifugal 10min of 1500rpm, get supernatant and survey the A value in full-automatic microplate reader 450nm wavelength place with 96 porocyte culture plates, as the QHS response value, experimental result sees Table 6:
The different preparations of table 6 are to the influence of mouse lymphocyte propagation and antibody generation
| Group | Number of animals only | Spleen lymphocyte proliferation | ??QHS |
| Normal saline BAIHUASHESHECAO ZHUSHEYE injectable powder of the present invention | ??12 ??12 ??12 | ??0.137±0.011 ??0.455±0.035 *??0.512±0.024 ** | ??0.137±0.033 ??0.077±0.006 *??0.051±0.004 ** |
Annotate:
*P＜0.01,
*P＜0.05
Embodiment 3
To mice S
180The tumor growth inhibitory action
Laboratory animal: healthy mice, body weight 16-20g, male and female are respectively done.
Tumor strain: mice S
180
Experiment medicine: lyophilized injectable powder of the present invention (Tianzhijiao Medication Development Co., Ltd., Guangdong's laboratory provides)
BAIHUASHESHECAO ZHUSHEYE (three nine-day periods after the winter solstice enterprise group Anhui three nine-day periods after the winter solstice pharmaceutcal corporation, Ltd)
Normal saline (Tianzhijiao Medication Development Co., Ltd., Guangdong's laboratory provides) experimental technique: get and inoculate the mice S that goes down to posterity
180, in homogenizer, add normal saline, make mice S
180The tumor homogenate, again with normal saline 1: 3 dilution, getting 0.2ml then, to inject oxter, a mice left side subcutaneous, weighed in 24 hours, mice tail every day intravenously administrable once, dosage is 0.3g crude drug/kg, totally 14 days.Next day is put to death mice in drug withdrawal, and the subcutaneous tumors piece is peeled off in the also carefulness of weighing, and takes by weighing tumor in the EM50 electronic balance and weighs, and calculate tumour inhibiting rate, sees Table 7:
Two kinds of preparations of table 7 are to mice S
180The tumor growth inhibitory action
| Group | Number of animals only | Tumor body weight mg | Tumour inhibiting rate % |
| Normal saline BAIHUASHESHECAO ZHUSHEYE injectable powder of the present invention | ??10 ??10 ??10 | ??1.4123 ??1.2355 ??0.9975 | ??100 ??12.5 ??29.4 * |
Annotate: compare with the normal saline group
*P＜0.05
Conclusion: show that by above pharmacological evaluation lyophilized injectable powder of the present invention has better pharmacological action.
Four. preparation embodiment
Embodiment 1
(1) gets Herba Hedyotidis Diffusae 2000 grams, pulverize, put into the supersound extraction jar, with concentration is 70% ethanol extraction 10 minutes, extracting liquid filtering, and residue is standby, filtrate recycling ethanol adds the 1% potassium hydroxide-alcoholic solution of 4 times of crude drug amounts to the greatest extent, leaves standstill, centrifugal, get supernatant, add hydrochloric acid and regulate pH value to 5, centrifugal, get supernatant, Rotary Evaporators concentrates, 30 ℃ of control temperature, cold drying obtains the Herba Hedyotidis Diffusae ethanol extract;
(2) get above-mentioned residue, drying, extracting in water 2 times, each 2 hours, merge extractive liquid, filtered, relative density is 1.05 when being concentrated to 50 ℃, with the filter element coarse filtration of 0.1um, filtrate is earlier 100000 hollow fiber column ultrafilter with molecular cut off, keeps permeate, the reuse molecular cut off is 3000 ultrafilter membrane bag ultrafiltration, keep circulation fluid, the circulation fluid drying obtains Herba Hedyotidis Diffusae polysaccharide;
(3) preparation prescription of the present invention is:
Herba Hedyotidis Diffusae ethanol extract 40 grams, Herba Hedyotidis Diffusae polysaccharide 16 grams, pharmaceutic adjuvant lactose are 144 grams;
(4) with Herba Hedyotidis Diffusae ethanol extract, polysaccharide, add the water for injection dissolving fully, to filter, filtrate adds pharmaceutic adjuvant, filters, sterilization, drying obtains 1000 bottles of hedyotis herba powder injections.(injectable powder total flavones of the present invention (in rutin) content 0.60mg/ bottle, polyoses content 16.0mg/ bottle.)
Embodiment 2
(1) gets Herba Hedyotidis Diffusae 2000 grams, pulverize, put into the supersound extraction jar, with concentration is 90% ethanol extraction 15 minutes, extracting liquid filtering, and residue is standby, filtrate recycling ethanol adds the 1% potassium hydroxide-alcoholic solution of 6 times of crude drug amounts to the greatest extent, leaves standstill, centrifugal, get supernatant, add hydrochloric acid and regulate pH value to 5, centrifugal, get supernatant, Rotary Evaporators concentrates, 40 ℃ of control temperature, cold drying obtains the Herba Hedyotidis Diffusae ethanol extract;
(2) get above-mentioned residue, drying, extracting in water 4 times, each 4 hours, merge extractive liquid, filtered, relative density is 1.10 when being concentrated to 50 ℃, with the filter element coarse filtration of 0.1um, filtrate is earlier 100000 hollow fiber column ultrafilter with molecular cut off, keeps permeate, the reuse molecular cut off is 3000 ultrafilter membrane bag ultrafiltration, keep circulation fluid, the circulation fluid drying obtains Herba Hedyotidis Diffusae polysaccharide;
(3) preparation prescription of the present invention is:
Herba Hedyotidis Diffusae ethanol extract 60 grams, Herba Hedyotidis Diffusae polysaccharide 23 grams, pharmaceutic adjuvant sucrose are 117 grams;
(4) with Herba Hedyotidis Diffusae ethanol extract, polysaccharide, add the water for injection dissolving fully, to filter, filtrate adds pharmaceutic adjuvant, filters, sterilization, drying obtains 1000 bottles of hedyotis herba powder injections.(injectable powder total flavones of the present invention (in rutin) content 0.81mg/ bottle, polyoses content 23.0mg/ bottle.)
Embodiment 3
(1) gets Herba Hedyotidis Diffusae 2000 grams, pulverize, put into the supersound extraction jar, with concentration is 75% ethanol extraction 12 minutes, extracting liquid filtering, and residue is standby, filtrate recycling ethanol adds the 1% potassium hydroxide-alcoholic solution of 5 times of crude drug amounts to the greatest extent, leaves standstill, centrifugal, get supernatant, add hydrochloric acid and regulate pH value to 5, centrifugal, get supernatant, Rotary Evaporators concentrates, 35 ℃ of control temperature, cold drying obtains the Herba Hedyotidis Diffusae ethanol extract;
(2) get above-mentioned residue, drying, extracting in water 3 times, each 3 hours, merge extractive liquid, filtered, relative density is 1.08 when being concentrated to 50 ℃, with the filter element coarse filtration of 0.1um, filtrate is earlier 100000 hollow fiber column ultrafilter with molecular cut off, keeps permeate, the reuse molecular cut off is 3000 ultrafilter membrane bag ultrafiltration, keep circulation fluid, the circulation fluid drying obtains Herba Hedyotidis Diffusae polysaccharide;
(3) preparation prescription of the present invention is:
Herba Hedyotidis Diffusae ethanol extract 45 grams, Herba Hedyotidis Diffusae polysaccharide 18 grams, pharmaceutic adjuvant mannitol are 137 grams;
(4) with Herba Hedyotidis Diffusae ethanol extract, polysaccharide, add the water for injection dissolving fully, to filter, filtrate adds pharmaceutic adjuvant, filters, sterilization, drying obtains 1000 bottles of hedyotis herba powder injections.(injectable powder total flavones of the present invention (in rutin) content 0.68mg/ bottle, polyoses content 17.3mg/ bottle.)
Embodiment 4
(1) gets Herba Hedyotidis Diffusae 2000 grams, pulverize, put into the supersound extraction jar, with concentration is 80% ethanol extraction 14 minutes, extracting liquid filtering, and residue is standby, filtrate recycling ethanol adds the 1% potassium hydroxide-alcoholic solution of 5 times of crude drug amounts to the greatest extent, leaves standstill, centrifugal, get supernatant, add hydrochloric acid and regulate pH value to 5, centrifugal, get supernatant, Rotary Evaporators concentrates, 38 ℃ of control temperature, cold drying obtains the Herba Hedyotidis Diffusae ethanol extract;
(2) get above-mentioned residue, drying, extracting in water 2 times, each 3 hours, merge extractive liquid, filtered, relative density is 1.09 when being concentrated to 50 ℃, with the filter element coarse filtration of 0.1um, filtrate is earlier 100000 hollow fiber column ultrafilter with molecular cut off, keeps permeate, the reuse molecular cut off is 3000 ultrafilter membrane bag ultrafiltration, keep circulation fluid, the circulation fluid drying obtains Herba Hedyotidis Diffusae polysaccharide;
(3) preparation prescription of the present invention is:
Herba Hedyotidis Diffusae ethanol extract 50 grams, Herba Hedyotidis Diffusae polysaccharide 20.5 grams, pharmaceutic adjuvant mannitol, lactose 129.5 grams;
(4) with Herba Hedyotidis Diffusae ethanol extract, polysaccharide, add the water for injection dissolving fully, to filter, filtrate adds pharmaceutic adjuvant, filters, sterilization, drying obtains 1000 bottles of hedyotis herba powder injections.(injectable powder total flavones of the present invention (in rutin) content 0.71mg/ bottle, polyoses content 18.4mg/ bottle.)
Embodiment 5
(1) gets Herba Hedyotidis Diffusae 2000 grams, pulverize, put into the supersound extraction jar, with concentration is 85% ethanol extraction 14 minutes, extracting liquid filtering, and residue is standby, filtrate recycling ethanol adds the 1% potassium hydroxide-alcoholic solution of 6 times of crude drug amounts to the greatest extent, leaves standstill, centrifugal, get supernatant, add hydrochloric acid and regulate pH value to 5, centrifugal, get supernatant, Rotary Evaporators concentrates, 38 ℃ of control temperature, cold drying obtains the Herba Hedyotidis Diffusae ethanol extract;
(2) get above-mentioned residue, drying, extracting in water 4 times, each 4 hours, merge extractive liquid, filtered, relative density is 1.07 when being concentrated to 50 ℃, with the filter element coarse filtration of 0.1um, filtrate is earlier 100000 hollow fiber column ultrafilter with molecular cut off, keeps permeate, the reuse molecular cut off is 3000 ultrafilter membrane bag ultrafiltration, keep circulation fluid, the circulation fluid drying obtains Herba Hedyotidis Diffusae polysaccharide;
(3) preparation prescription of the present invention is:
Herba Hedyotidis Diffusae ethanol extract 55 grams, Herba Hedyotidis Diffusae polysaccharide 22.8 grams, pharmaceutic adjuvant mannitol, sucrose, lactose are 122.2 grams;
(4) with Herba Hedyotidis Diffusae ethanol extract, polysaccharide, add the water for injection dissolving fully, to filter, filtrate adds pharmaceutic adjuvant, filters, sterilization, drying obtains 1000 bottles of hedyotis herba powder injections.(injectable powder total flavones of the present invention (in rutin) content 0.79mg/ bottle, polyoses content 21.4mg/ bottle.)
Embodiment 6
(1) gets Herba Hedyotidis Diffusae 20000 grams, pulverize, put into the supersound extraction jar, with concentration is 80% ethanol extraction 14 minutes, extracting liquid filtering, and residue is standby, filtrate recycling ethanol adds the 1% potassium hydroxide-alcoholic solution of 5 times of crude drug amounts to the greatest extent, leaves standstill, centrifugal, get supernatant, add hydrochloric acid and regulate pH value to 5, centrifugal, get supernatant, Rotary Evaporators concentrates, 35 ℃ of control temperature, cold drying obtains the Herba Hedyotidis Diffusae ethanol extract; (2) get above-mentioned residue, drying, extracting in water 3 times, each 3 hours, merge extractive liquid, filtered, relative density is 1.08 when being concentrated to 50 ℃, with the filter element coarse filtration of 0.1um, filtrate is earlier 100000 hollow fiber column ultrafilter with molecular cut off, keeps permeate, the reuse molecular cut off is 3000 ultrafilter membrane bag ultrafiltration, keep circulation fluid, the circulation fluid drying obtains Herba Hedyotidis Diffusae polysaccharide;
(3) preparation prescription of the present invention is:
Herba Hedyotidis Diffusae ethanol extract 508 grams, Herba Hedyotidis Diffusae polysaccharide 204 grams, pharmaceutic adjuvant mannitol, lactose 1288 grams;
(4) with Herba Hedyotidis Diffusae ethanol extract, polysaccharide, add the water for injection dissolving fully, to filter, filtrate adds pharmaceutic adjuvant,, filter, sterilization, drying obtains 10000 bottles of hedyotis herba powder injections.(injectable powder total flavones of the present invention (in rutin) content 0.74mg/ bottle, polyoses content 19.4mg/ bottle.)
Claims (3)
1. a hedyotis herba powder injection is characterized in that it is by Herba Hedyotidis Diffusae ethanol extract 40-60 weight portion, Herba Hedyotidis Diffusae polysaccharide 16-23 weight portion, and pharmaceutic adjuvant is formed for the 117-144 weight portion; Its feature also is to control this injectable powder total flavones (in rutin) must not be less than the 0.60mg/ bottle, and the control polyoses content is not less than the 16.0mg/ bottle.
2. a kind of hedyotis herba powder injection according to claim 1, it is characterized in that the method that adopts ultrasonic alcohol extraction, alkaline ethanol precipitation, hydrochloric acid to regulate pH value obtains ethanol extract, the residue that extracts obtains polysaccharide through the method for water extraction, ultrafiltration, adds pharmaceutic adjuvant, is prepared into injectable powder.
3. according to the preparation method of the described a kind of hedyotis herba powder injection of claim 1, its feature may further comprise the steps:
(1) gets Herba Hedyotidis Diffusae, pulverize, put into the supersound extraction jar, with concentration is ethanol extraction 10-15 minute of 70%-90%, extracting liquid filtering, and residue is standby, filtrate recycling ethanol adds crude drug amount 4-6 1% potassium hydroxide-ethanol solution doubly to the greatest extent, leaves standstill, centrifugal, get supernatant, add hydrochloric acid and regulate pH value to 5, centrifugal, get supernatant, Rotary Evaporators concentrates, 30-40 ℃ of control temperature, cold drying obtains the Herba Hedyotidis Diffusae ethanol extract;
(2) get above-mentioned residue, drying, extracting in water 2-4 time, each 2-4 hour, merge extractive liquid, filtered, relative density is 1.05-1.10 when being concentrated to 50 ℃, with the filter element coarse filtration of 0.1um, filtrate is earlier 100000 hollow fiber column ultrafilter with molecular cut off, keeps permeate, the reuse molecular cut off is 3000 ultrafilter membrane bag ultrafiltration, keep circulation fluid, the circulation fluid drying obtains Herba Hedyotidis Diffusae polysaccharide;
(3) with Herba Hedyotidis Diffusae ethanol extract, polysaccharide, add the water for injection dissolving fully, to filter, filtrate adds pharmaceutic adjuvant, filters, sterilization, drying obtains hedyotis herba powder injection.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB200510055292XA CN100387262C (en) | 2005-03-18 | 2005-03-18 | Hedyotis herba powder injection and its preparation method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB200510055292XA CN100387262C (en) | 2005-03-18 | 2005-03-18 | Hedyotis herba powder injection and its preparation method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1686334A true CN1686334A (en) | 2005-10-26 |
| CN100387262C CN100387262C (en) | 2008-05-14 |
Family
ID=35304376
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB200510055292XA Expired - Fee Related CN100387262C (en) | 2005-03-18 | 2005-03-18 | Hedyotis herba powder injection and its preparation method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN100387262C (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111484564A (en) * | 2019-01-27 | 2020-08-04 | 复旦大学 | Spreading hedyotis herb polysaccharide, preparation method thereof and application thereof in preparing anticomplement medicines |
-
2005
- 2005-03-18 CN CNB200510055292XA patent/CN100387262C/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111484564A (en) * | 2019-01-27 | 2020-08-04 | 复旦大学 | Spreading hedyotis herb polysaccharide, preparation method thereof and application thereof in preparing anticomplement medicines |
| CN111484564B (en) * | 2019-01-27 | 2022-07-08 | 复旦大学 | Spreading hedyotis herb polysaccharide, preparation method thereof and application thereof in preparing anticomplement medicines |
Also Published As
| Publication number | Publication date |
|---|---|
| CN100387262C (en) | 2008-05-14 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN1872106A (en) | Application of wild basil circle leaves in treating disease of virulence cold | |
| CN1813910A (en) | Medicinal composition with blood sugar reducing action and its preparing method | |
| CN103191289B (en) | Synchronous preparation method of four effective parts in medicine pair of common anemarrhena rhizome and amur corktree bark and application thereof | |
| CN101057890A (en) | Traditional Chinese medicinal composition for treating coronary heart disease and its preparation method, preparations and its application | |
| CN1686377A (en) | Chuankezhi (pant treating) powder injection and its preparation method | |
| CN1686334A (en) | Hedyotis herba powder injection and its preparation method | |
| CN1990500A (en) | Liver-fibrosis-resistant asiatic centella triterpenoid saponin and its preparation process | |
| CN101084979B (en) | Medicinal preparation for cancer auxiliary treatment and its preparation method | |
| CN1803179A (en) | Traditional Chinese medicine composition and its preparation method and quality control method | |
| CN1216896C (en) | Echinocystic acid preparation, medicinal preparation and new use as medicine | |
| CN1264529C (en) | Freeze-dried 'Shenqifuzheng' powder for injection and its preparing process | |
| CN1903213A (en) | Traditional Chinese medicine preparation with functions of immunological regulation for anti-chemical damage | |
| CN100584345C (en) | Distillage of Ardisia chinensis Benth of possessing function of antivirus, extraction method and application | |
| CN1290557C (en) | Medicine for treating cataract and preparation method thereof | |
| CN1891283A (en) | Chinese medicine composition, and its preparing method and quality control method | |
| CN1264506C (en) | Pharmaceutical combination containing red sage root element and preparation method thereof | |
| CN101053587A (en) | Medicinal composition for treating tumor and preparation method and quality control method thereof | |
| CN101912565B (en) | Turmeric and astragalus capsules for treating diabetes and incipient diabetic nephropathy | |
| CN104950101A (en) | Checking method for Chinese medicine injection trace resin | |
| CN106420850B (en) | Compositions extracted from gingko biloba leaves and its preparing the application in Shu Xuening injection | |
| CN100344312C (en) | Prepn process of granule for treating children's hyperkinesia and its quality control method | |
| CN104721294A (en) | Preparation method of total flavonoids of clematis filamentosa Dunn and application of total flavonoids of clematis filamentosa Dunn to drug for treating myocardial ischemia | |
| CN108159109A (en) | Radix Astragali flavone extract is preparing the application in treating Neuroleptic Leukocytopenia disease drug | |
| CN1278698C (en) | Freeze dried injection of seeding of autumnal sowthistle-leaf ixeris and preparation method thereof | |
| CN1297278C (en) | Medicinal composition containing salvianolic acid B, total ara-saponin and camphol and its preparation and use |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C57 | Notification of unclear or unknown address | ||
| DD01 | Delivery of document by public notice |
Addressee: Zhang Zhengsheng Document name: Notification of Termination of Patent Right |
|
| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20080514 |