CN1283268C - Compound dandelion freeze dried powder injection and its preparation method - Google Patents
Compound dandelion freeze dried powder injection and its preparation method Download PDFInfo
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- CN1283268C CN1283268C CN 200510056774 CN200510056774A CN1283268C CN 1283268 C CN1283268 C CN 1283268C CN 200510056774 CN200510056774 CN 200510056774 CN 200510056774 A CN200510056774 A CN 200510056774A CN 1283268 C CN1283268 C CN 1283268C
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Abstract
The present invention discloses a compound freeze dry powder injection of dandehon herb and a preparation method thereof. The injection is prepared from the components (parts by weight): 1 to 3 parts of HP-beta-CD inclusion compound of volatile oil, 5 to 10 parts of extract product and auxiliary material suitable for medicine, wherein the volatile oil is extracted from heartleaf houttuynia herb and wild chrysanthemum, and the extract product is obtained by the extraction and the purification of dandelion, heartleaf houttuynia herb and wild chrysanthemum; the extract product comprises 30 to 50% of total falconoid, 0.5 to 0.8% of chlorogenic acid and 0.3 to 0.5% of caffeic acid. The present invention also discloses a preparation method. A content measuring result and a pharmacological experiment result show that the preparation of the present invention has higher content of effective components and stronge pharmacological action.
Description
Affiliated technical field
The invention belongs to technical field of traditional Chinese medicine pharmacy, be specifically related to a kind of compound dandelion freeze dried powder injection and preparation method thereof.
Background technology
Herba Taraxaci is the whole herb with root for Compositae herbaceos perennial Herba Taraxaci Taraxacum mongolicum Hand.Mazz. and multiple congener thereof.Herba Taraxaci bitter in the mouth, sweet, cold in nature, people liver stomach two warps.Have effects such as heat-clearing and toxic substances removing, dispersing swelling and dissipating binds and function of gallbladder promoting diuresis.Pharmacological evaluation shows, that Herba Taraxaci has is antibiotic, function of gallbladder promoting, be good for the stomach, effect such as lactogenesis and antitumor.Be used for diseases such as acute or chronic gastritis, mastitis, treatment carbuncle toxin, hepatitis, bronchitis, urinary tract infection clinically.
Herba Houttuyniae is the dry aerial parts of Saururaceae Houttuynia plant Herba Houttuyniae Houttuyniacordata Thunb, and acrid in the mouth, cool in nature has effects such as heat-clearing and toxic substances removing, eliminating carbuncle evacuation of pus, inducing diuresis for treating stranguria syndrome, be used for the lung abscess vomiting pus, the expectorant dyspnea of heat type is coughed, hematodiarrhoea, pyretic stranguria, carbuncle sore tumefacting virus.
Flos Chrysanthemi Indici is the head inflorescence of Compositae herbaceos perennial Herba Dendranthematis indici Chrysanthemum indicum L. etc.Nature and flavor hardship, suffering are slightly cold, and return lung, Liver Channel.The function heat-clearing and toxic substances removing, the kind diseases such as carbuncle, furunculosis, laryngopharynx swelling and pain, wind-fire acute conjunctivitis, skin pruritus of controlling have good hypotensive effect again simultaneously, can be used for the auxiliary treatment of hypertension.
FUFANG PUGONGYING ZHUSHEYE is prepared from through extraction by Herba Taraxaci, Herba Houttuyniae, Flos Chrysanthemi Indici three flavor Chinese medicines, has heat-clearing and toxic substances removing, dispelling wind cough-relieving effect, is used for anemopyretic cold, cough due to lung-heat.
Herba Taraxaci contains chlorogenic acid, caffeic acid and flavones ingredient, and the main effective ingredient of Herba Houttuyniae is a volatile oil, also contains flavone component, and contained chlorogenic acid, volatile oil and flavone compound is the main effective ingredient of its performance drug effect in the Flos Chrysanthemi Indici.And Herba Houttuyniae, Flos Chrysanthemi Indici have only extracted the volatile oil composition among the former preparation technology of FUFANG PUGONGYING ZHUSHEYE.Since contain compositions such as chlorogenic acid and volatile oil, unstable product quality, and to having relatively high expectations of preserving, preserving improper medicinal liquid can be because situations such as muddiness, precipitation, variable color appears in oxidation; Only content of total flavone is measured in the FUFANG PUGONGYING ZHUSHEYE quality standard, owing to all contain flavones ingredient in the Herba Taraxaci of FUFANG PUGONGYING ZHUSHEYE, Herba Houttuyniae, the Flos Chrysanthemi Indici, but its contained flavones ingredient structure and molecular weight are different, all do contrast and calculate content with rutin, scientific poor, only measure simultaneously the another kind of active component chlorogenic acid contents situation that flavones ingredient can not reflect that Herba Taraxaci and Flos Chrysanthemi Indici all contain, and " caffeinic content also not embodiment in preparation that Herba Taraxaci medical material of Chinese pharmacopoeia is measured; In addition injection has been owing to adopted three step alcohol deposition methods in the injection preparation technology, and the part effective ingredient can be along with the impurity precipitation that is wrapped together in the precipitate with ethanol process, and loss of effective components is big; Injection is to the stability requirement height, carry, store, broken easily when transporting, also result in hand cramps.
In data-searching, find no the report that closes compound dandelion freeze dried powder injection.
Summary of the invention
Based on above reason, research worker of the present invention is according to the character of the effective ingredient of contained medical material in the compound dandelion, extraction and purification process is improved, the extraction that makes effective ingredient more comprehensively, content is higher, impurity content still less, merge with extract after volatile oil made clathrate, make lyophilized injectable powder and also improved stability of formulation, the present invention also improves the quality standard of preparation, chlorogenic acid and caffeinic content have been measured, make the quality controllability of preparation stronger, The pharmacological results shows that compound dandelion freeze dried powder injection of the present invention has better pharmacological action.
The objective of the invention is to disclose a kind of active component, good effect, steady quality, convenient compound dandelion freeze-dried powder that uses of being rich in.
Another object of the present invention provides the preparation method of above-mentioned compound dandelion freeze-dried powder.
The present invention is achieved through the following technical solutions.
One, preparation method
(1) raw material medicines in portions by weight consists of: Herba Taraxaci 8-12 part, Herba Houttuyniae 8-12 part, Flos Chrysanthemi Indici 8-12 part.
(2) get Herba Houttuyniae, Flos Chrysanthemi Indici medical material, soaked 1 hour, extract volatile oil with steam distillation, the volatile oil of collecting is slowly added in HP-β-CD saturated aqueous solution, 50 ℃ of-60 ℃ of heat-retaining conditions stirred 2-4 hour down, continued under the room temperature to stir 3 hours, and cold preservation is spent the night, filter, vacuum drying obtains clathrate.
(3) Herba Taraxaci and Herba Houttuyniae, Flos Chrysanthemi Indici medicinal residues add the water extraction 2 times that 6-10 doubly measures, each 1 hour again; Merge decoction liquor twice, leave standstill, filter, filtrate is concentrated into the extractum that relative density is 1.20-1.24, adds ethanol and makes and contain the alcohol amount and reach 60%-70%, left standstill 12 hours, filter, decompression filtrate recycling ethanol is not to there being the alcohol flavor, and thin up is to solution: medical material is 1: 1, medicinal liquid is crossed the macroporous adsorptive resins of having handled well, behind the water elution with 3-5 times of column volume, reuse 4-6 doubly measures column volume 40%-70% ethanol elution earlier, merges ethanol elution, decompression recycling ethanol also concentrates, thin up is to solution: medical material is 1: 0.5, is that the ultrafilter membrane of 5000-20000 carries out ultrafiltration, ultrafiltrate concentrating under reduced pressure and vacuum drying with molecular cut off, pulverize, obtain extract.
(4) get above-mentioned clathrate, extract and add the dissolving of injection water, filter, add pharmaceutic adjuvant, add the injection water, regulate pH value to 7.0-7.5 to ormal weight, filtering with microporous membrane, fill, lyophilization, promptly.
In the preparation of compound dandelion freeze dried powder injection, adopt steam distillation to extract volatile oil in Herba Houttuyniae, the Flos Chrysanthemi Indici after, (HP-β-CD) carries out enclose to the reuse hydroxypropyl.HP-β-CD is water miscible clathrate, and it is good to make the injectable powder dissolubility with the volatile oil of its enclose, easily absorb during injection, and the bioavailability height, the patient keenly feels little, is easy to by the acceptance of patient's happiness; And volatile oil is carried out enclose with HP-β-CD, and make it in the process of preparation, storage, transportation, be difficult for oxidation by air and go bad, increased the stability of volatile oil, improved curative effect.Herba Taraxaci and Flos Chrysanthemi Indici all contain flavone compound and chlorogenic acid, Herba Houttuyniae also contains the part chromocor compound, Herba Taraxaci also contains caffeic acid etc., therefore will extract Herba Houttuyniae, Flos Chrysanthemi Indici and Herba Taraxaci merging water extraction behind the volatile oil, we adopt classical decoction and alcohol sedimentation technique after removing partial impurities, with macroporous adsorbent resin extract has been carried out separation and purification again, main effective ingredient general flavone content is 35%-50% in the compound dandelion extract after purified, chlorogenic acid content is 0.5%-0.8%, and caffeic acid content is 0.3%-0.5%.Simultaneously after the lyophilizing labile element chlorogenic acid of preparation and volatile oil because volatile oil is isolated the minimizing that influences each other of chlorogenic acid and volatile oil, and ingredient exists with solid state, also improved stability of formulation mutually by enclose.
The ultrafilter membrane isolation technics is a kind of emerging separation method, it can the selective screening by molecular weight removes protein, tannin, resin, impurity that the starch equimolecular quantity is bigger, keep required effective ingredient, this method is carried out at room temperature, mild condition, the separation efficiency height, it is a kind of method of energy-conserving and environment-protective, research worker of the present invention will further be carried out purification with ultrafilter membrane with the compound recipe Rhizoma Corydalis Decumbentis extract behind the purification by macroporous resin, and screen the molecular weight of the ultrafilter membrane that is suitable for extract of the present invention.The present invention handles with ultrafiltration technology, can further remove impurity, improves the purity of effective site, thereby improves the quality of the pharmaceutical preparations, and the utilization of ultrafiltration technology simultaneously also has certain effect for the removal of pyrogen.The molecular weight of the ultrafilter membrane that the present invention adopts is 5000-20000.
Contain the clathrate 1-3 weight portion of the HP-β-CD of the volatile oil that Herba Houttuyniae, Flos Chrysanthemi Indici extract in the preparation of the present invention, Herba Taraxaci, Herba Houttuyniae, Flos Chrysanthemi Indici are through extracting the extract 5-10 weight portion that purification obtains.
Two, assay analysis
1, content of total flavone is measured in the compound dandelion preparation
1.1 instrument and reagent day island proper Tianjin UV-3000A ultraviolet spectrophotometer.FUFANG PUGONGYING ZHUSHEYE (Zhong Mountain, Jiangxi Pharmaceutical Co., Ltd); Compound dandelion freeze dried powder injection of the present invention (Tianzhijiao Medication Development Co., Ltd., Guangdong's laboratory provides); Control substance of Rutin (Nat'l Pharmaceutical ﹠ Biological Products Control Institute); Methanol, sodium nitrite, aluminum nitrate, sodium hydroxide reagent are analytical pure, and water is tri-distilled water (self-control).
1.2 reference substance solution preparation precision takes by weighing control substance of Rutin 100mg, put in the 50ml measuring bottle, add methanol 30ml, put that slight fever makes dissolving in the water-bath, put cold, add methanol and be diluted to scale, shake up, precision is measured 10ml, put in the 100ml volumetric flask, add methanol and be diluted to scale, shake up, promptly get the control substance of Rutin solution of 0.2mg/ml.
1.3 the above-mentioned reference substance solution 0 of the accurate absorption of standard curve preparation, 1.00,2.00,3.00,4.00,5.00,6.00ml, put respectively in the 25ml volumetric flask, respectively add water to 6ml, add 5% sodium nitrite solution 1ml respectively, shake up, add 1% aluminum nitrate solution 1ml respectively after placing 6min, shake up, place 6min, add 4% sodium hydroxide solution 10ml more respectively, add water to scale again, shake up, place 15min, measuring absorption value A at the 500nm place according to spectrophotography, with absorption value A concentration is carried out regression Calculation, regression equation is: Y=0.124x-0.0034, r=0.998.
1.4 this product powder is got in the preparation of need testing solution, the accurate title, decide, and gets about 0.5g, put in the tool plug conical flask, the accurate methanol 20ml that adds claims to decide weight, supersound process 40min is put coldly, claims to decide weight again, supply the weight that subtracts mistake with methanol, shake up, centrifugal (12000rpm) 10min gets supernatant liquid filtering, get subsequent filtrate, promptly.
1.5 the mensuration of total flavones precision is respectively measured need testing solution 5ml and is put in the 25ml volumetric flask, sighting target directrix curve method is measured, colour developing, measure the A value everywhere at the 500nm wavelength, in addition precision is measured need testing solution 5ml and is put in the 25ml volumetric flask, and adding distil water is to scale, shake up, measure the A value everywhere at the 500nm wavelength, get the trap difference twice, by the regression equation calculation general flavone content.The results are shown in Table 1.
Total flavones in table 1 preparation (in anhydrous rutin) assay
| Batch | Content (mg/ props up) | |
| FUFANG PUGONGYING ZHUSHEYE | Compound dandelion freeze dried powder injection of the present invention | |
| 1 2 3 | 20.0 18.5 18.0 | 45.0 43.0 45.4 |
2, the assay of chlorogenic acid in the compound dandelion preparation
Reference literature (reach the clouds etc., the HPLC method is measured chlorogenic acid contents in the Herba Taraxaci. and Chinese herbal medicine .1998,29 (8): 521-522) method is measured, and the results are shown in Table 2.
Determination of chlorogenic acid in table 2 preparation
| Batch | Content (mg/ props up) | |
| FUFANG PUGONGYING ZHUSHEYE | Compound dandelion freeze dried powder injection of the present invention | |
| 1 2 3 | 0.54 0.52 0.51 | 0.76 0.87 0.71 |
3, caffeinic assay in the compound dandelion preparation
With reference to " caffeinic content assaying method is measured under 2000 editions one Herba Taraxaci medical material item of Chinese pharmacopoeia, the results are shown in Table 3.
Caffeic acid assay in table 3 preparation
| Batch | Content (mg/ props up) | |
| FUFANG PUGONGYING ZHUSHEYE | Compound dandelion freeze dried powder injection of the present invention | |
| 1 2 3 | 0.23 0.20 0.21 | 0.31 0.28 0.30 |
Above assay presentation of results, total flavones in the compound dandelion freeze dried powder injection of the present invention and chlorogenic acid, caffeic acid content are apparently higher than the total flavones of FUFANG PUGONGYING ZHUSHEYE and chlorogenic acid, caffeic acid content.Illustrate that preparation method of the present invention is more reasonable, science has more practicality more.
4, total flavones and chlorogenic acid, caffeinic assay in the extract
Determining instrument, reagent and method are the same.Compound dandelion extract of the present invention is by preparation method gained of the present invention; FUFANG PUGONGYING ZHUSHEYE extract (preparing gained) according to the method for making in the FUFANG PUGONGYING ZHUSHEYE; The results are shown in Table 4,5,6.
Total flavones in table 4 extract (in anhydrous rutin) assay
| Batch | Content (%) | |
| The FUFANG PUGONGYING ZHUSHEYE extract | Compound dandelion freeze dried powder injection extract of the present invention | |
| 1 2 3 | 21.0 22.5 20.8 | 40.5 45.6 38.1 |
Determination of chlorogenic acid in table 5 extract
| Batch | Content (%) | |
| The FUFANG PUGONGYING ZHUSHEYE extract | Compound dandelion freeze dried powder injection extract of the present invention | |
| 1 2 3 | 0.46 0.48 0.45 | 0.75 0.61 0.58 |
Caffeic acid assay in table 6 extract
| Batch | Content (%) | |
| The FUFANG PUGONGYING ZHUSHEYE extract | Compound dandelion freeze dried powder injection extract of the present invention | |
| 1 2 3 | 0.24 0.22 0.22 | 0.32 0.36 0.41 |
Above assay presentation of results, effective ingredient total flavones in the compound dandelion extract that preparation method of the present invention obtains and chlorogenic acid, caffeinic percentage composition total flavones and the chlorogenic acid, caffeinic percentage composition in the FUFANG PUGONGYING ZHUSHEYE extract.Illustrate that the extract purity that preparation method of the present invention makes is higher, technology more rationally, science.
Three, pharmacology embodiment
Reagent; Normal saline (Tianzhijiao Medication Development Co., Ltd., Guangdong's laboratory provides)
FUFANG PUGONGYING ZHUSHEYE (Zhong Mountain, Jiangxi Pharmaceutical Co., Ltd)
Compound dandelion freeze dried powder injection of the present invention (Qianluchun Science and Technology Co., Ltd., Beijing's laboratory provides).
Animal: New Zealand white rabbit, body weight 1000-1250g male and female half and half; Kunming mouse, body weight 18-22g, male and female half and half, rat, body weight 180-220g, male and female half and half.
Antibacterial: streptococcus pneumoniae, escherichia coli, staphylococcus aureus, Pseudomonas aeruginosa and Shigella flexneri are provided by Beijing University of Chinese Medicine.
1. bacteriostatic test
With streptococcus pneumoniae (10
10Individual/ml), escherichia coli (10
5Individual/ml), staphylococcus aureus (10
5Individual/ml), Pseudomonas aeruginosa (10
5Individual/ml) and Shigella flexneri (10
5Individual/ml), separate application is on the medicine ware flat board of thick about 6mm, and the hole that breaks into the about 6mm of diameter then therein is some.Fill it up with compound dandelion lyophilized powder solution and FUFANG PUGONGYING ZHUSHEYE, cultivated 24 hours for 37 ℃, observe the inhibition zone size, the results are shown in Table 7.
Table 7 bacteriostatic experiment result
| Antibacterial | FUFANG PUGONGYING ZHUSHEYE (mm) | Compound dandelion freeze dried powder injection of the present invention (mm) |
| Streptococcus pneumoniae (10 10Individual/ml) escherichia coli (10 5Individual/ml) staphylococcus aureus (10 5Individual/ml) Pseudomonas aeruginosa (10 5Individual/ml) Shigella flexneri (10 5Individual/ml) | 9 7 7 7 8 | 15 13 14 13 15 |
Compound dandelion freeze dried powder injection of the present invention and FUFANG PUGONGYING ZHUSHEYE all can form the inhibition zone of certain diameter to above antibacterial, show stronger bacteriostasis, but the bacteriostasis of compound dandelion freeze dried powder injection of the present invention is obviously strong than FUFANG PUGONGYING ZHUSHEYE.
2. separate heat test:
Choose 35 of healthy new zealand white rabbits, body weight is 1000-1250g, male and female half and half, the same day was surveyed the anus temperature 3 times in experiment, averaged as normal body temperature, then in back subcutaneous injection 5% sterilised yeast suspension 5ml/kg, select 30 of the New Zealand white rabbit of body temperature rise more than 0.8 ℃ after 5 hours, be divided into the blank group at random, FUFANG PUGONGYING ZHUSHEYE group, compound dandelion freeze dried powder injection group of the present invention, 10 of every treated animals.Intraperitoneal injection, dosage are 2g crude drug/kg (capacity is 1ml), and the blank group waits the capacity normal saline.Respectively surveyed body temperature 1 time respectively at 1,2,3 hour after the administration, relatively the difference of each treated animal body temperature drop-out value the results are shown in Table 8.
The refrigeration function of table 8 pair New Zealand white rabbit
| Group | Normal body temperature (℃) | 5h body temperature after the pyrogenicity (℃) | The body temperature drop-out value (℃) | ||
| 1 | 2 | 3 | |||
| Matched group FUFANG PUGONGYING ZHUSHEYE compound dandelion freeze dried powder injection of the present invention | 39.26±0.16 39.20±0.17 39.25±0.20 | 40.30±0.35 40.21.±0.31 40.27±0.36 | 0.04±0.09 0.27±0.10 0.55±0.18 * | 0.132±0.08 0.55±0.14 * 0.92±0.12 ** | 0.34±0.15 0.70±0.16 *0.95±0.21 ** |
Annotate: compare with the normal saline group
*P＜0.05,
*P＜0.01
Conclusion: above experimental result shows that compound dandelion freeze dried powder injection of the present invention has than better refrigeration function.
3, antitussive test
Get 30 of mices, male and female half and half, be divided into 3 groups at random, grouping and medication are with 2, dosage is 4g crude drug/kg (capacity is 0.2ml), and 75min places the 1L beaker respectively with mice after the administration, gives 30% ammonia atomization spraying 5s, observing and write down it coughs first and incubation period and 2min indegree, result such as table 9 occur.
Table 9 pair mice antitussive pain result of the test (X ± SD)
| Group | Time incubation period (s) | The cough number of times |
| Matched group FUFANG PUGONGYING ZHUSHEYE compound dandelion freeze dried powder injection of the present invention | 14.08±14.28 48.12±3.80 * 57.50±4.60 ** | 14.25±8.8 7.50±2.6 * 3.67±3.3 ** |
Annotate: compare with matched group:
*P＜0.05
*P＜0.01
4. analgesic test
4.1 the mice hot plate is caused the influence of pain effect
Get 30 of female mices, be divided into 3 groups at random, be blank group, FUFANG PUGONGYING ZHUSHEYE group, compound dandelion injectable powder group of the present invention, blank group 0.2ml normal saline lumbar injection, administration group lumbar injection 2g crude drug/kg, successive administration 3 days, 1h is individually fixed in each Mus in 55 ± 0.5 ℃ the hot-plate instrument after the last administration, to lick the indicator reaction of metapedes as " pain ", mice the results are shown in Table 10 to the response time of hot plate pain after the observation administration:
4.2 the influence of the writhing response that Dichlorodiphenyl Acetate causes
Get 30 of mices, male and female half and half, grouping and medication are with 4.1, successive administration 3 days, and 1h after the last administration, lumbar injection 0.6% acetum 0.2ml/20g body weight is observed the mouse writhing number of times in the 10min, the results are shown in Table 10:
Table 10 analgesic test result (X ± SD)
| Group | The hot plate pain response time (s) | Turn round the body number of times |
| Matched group FUFANG PUGONGYING ZHUSHEYE compound dandelion freeze dried powder injection of the present invention | 11.0±4.3 14.8±3.9 * 18.6±4.7 ** | 28.4±3.9 2.9±2.5 * 16.4±3.2 ** |
Annotate: compare with matched group:
*P＜0.05
*P＜0.01
Result of the test shows that the analgesic activity of compound dandelion injectable powder of the present invention is more more remarkable than FUFANG PUGONGYING ZHUSHEYE.
5. antiinflammatory test
5.1 on Carrageenan causes the influence of rat toes swelling
Get 30 of rats respectively, male and female half and half, be divided into matched group, FUFANG PUGONGYING ZHUSHEYE group and compound dandelion freeze dried powder injection group of the present invention, blank group 0.2ml normal saline lumbar injection, administration group lumbar injection 1.5g crude drug/kg immediately to the carrageenin solution of rat toes injection 0.1ml 1%, measures rat toes swelling volume after the administration after 1 hour, and calculate and suppress the swelling percentage by volume, the results are shown in Table 11:
Table 11 antiinflammatory result of the test (X ± SD)
| Group | Suppression ratio |
| Matched group FUFANG PUGONGYING ZHUSHEYE compound dandelion freeze dried powder injection of the present invention | 3.10±0.9 38.5±4.5 ** 57.0±5.2 **Δ |
Annotate: * * and matched group are relatively
*Compare with the FUFANG PUGONGYING ZHUSHEYE group P＜0.01
ΔP＜0.05
5.2 influence to mouse ear caused by dimethylbenzene xylene inflammation:
Get 30 of mices, male and female half and half, grouping and medication are with 4.1,30min after the last administration, dimethylbenzene 0.02ml is applied to mice left side ear, and mice is put to death in dislocation behind the 1h, cuts two ears, punching is weighed, and is the swelling degree with left ear and auris dextra sheet weight difference, the results are shown in Table 12.
Table 12 pair mouse ear caused by dimethylbenzene xylene inflammation influence result (X ± SD)
| Group | Swelling degree difference (mg) | Suppression ratio (%) |
| Matched group FUFANG PUGONGYING ZHUSHEYE group compound dandelion freeze dried powder injection of the present invention | 7.9±1.4 4.1±1.1 3.2±1.0 | 48.1±5.3 ** 59.5±6.0 **Δ |
Annotate: compare with matched group:
*Compare with the FUFANG PUGONGYING ZHUSHEYE group P＜0.01
ΔP＜0.05
The result shows that compound dandelion freeze dried powder injection antiinflammatory action of the present invention is significantly better than FUFANG PUGONGYING ZHUSHEYE.
Six, preparation embodiment
Embodiment 1:
(1) prescription of crude drug is: Herba Taraxaci 1000g, Herba Houttuyniae 1000g, Flos Chrysanthemi Indici 1000g.
(2) get Herba Houttuyniae, Flos Chrysanthemi Indici medical material, soaked 1 hour, extract volatile oil with steam distillation, the volatile oil of collecting is slowly added in HP-β-CD saturated aqueous solution, 50 ℃ of-60 ℃ of heat-retaining conditions stirred 2 hours down, continued under the room temperature to stir 3 hours, and cold preservation is spent the night, filter, vacuum drying obtains clathrate 15g.
(3) water extraction of Herba Taraxaci and Herba Houttuyniae, the Flos Chrysanthemi Indici medicinal residues amount of redoublining is 2 times, each 1 hour; Merge decoction liquor twice, leave standstill, filter, filtrate is concentrated into the extractum that relative density is 1.20-1.24, adds ethanol and makes and contain the alcohol amount and reach 60%, left standstill 12 hours, filter, decompression filtrate recycling ethanol is not to there being the alcohol flavor, and thin up is to solution: medical material is 1: 1, medicinal liquid is crossed the macroporous adsorptive resins of having handled well, behind the water elution with 3 times of column volumes, 4 times of amounts of reuse column volume, 70% ethanol elution merges ethanol elution earlier, decompression recycling ethanol also concentrates, thin up is to solution: medical material is 1: 0.5, is that 5000 ultrafilter membrane carries out ultrafiltration, ultrafiltrate concentrating under reduced pressure and vacuum drying with molecular cut off, pulverize, obtain extract 65g.
(4) preparation prescription is: volatile oil clathrate compound 15g, extract 65g, mannitol 40g.
(5) get above-mentioned volatile oil clathrate compound, extract and add the dissolving of injection water, filter, add mannitol, add the injection water, regulate pH value to 7.0-7.5 to ormal weight, filtering with microporous membrane, fill, lyophilization promptly gets 500.
Embodiment 2:
(1) prescription of crude drug is: Herba Taraxaci 1000g, Herba Houttuyniae 1000g, Flos Chrysanthemi Indici 1000g.
(2) get Herba Houttuyniae, Flos Chrysanthemi Indici medical material, soaked 1 hour, extract volatile oil with steam distillation, the volatile oil of collecting is slowly added in HP-β-CD saturated aqueous solution, 50 ℃ of-60 ℃ of heat-retaining conditions stirred 3 hours down, continued under the room temperature to stir 3 hours, and cold preservation is spent the night, filter, vacuum drying obtains clathrate 20g.
(3) Herba Taraxaci and Herba Houttuyniae, Flos Chrysanthemi Indici medicinal residues add the water extraction 2 times of 8 times of amounts, each 1 hour again; Merge decoction liquor twice, leave standstill, filter, filtrate is concentrated into the extractum that relative density is 1.20-1.24, adds ethanol and makes and contain the alcohol amount and reach 65%, left standstill 12 hours, filter, decompression filtrate recycling ethanol is not to there being the alcohol flavor, and thin up is to solution: medical material is 1: 1, medicinal liquid is crossed the macroporous adsorptive resins of having handled well, behind the water elution with 4 times of column volumes, 5 times of amounts of reuse column volume, 60% ethanol elution merges ethanol elution earlier, decompression recycling ethanol also concentrates, thin up is to solution: medical material is 1: 0.5, is that 10000 ultrafilter membrane carries out ultrafiltration, ultrafiltrate concentrating under reduced pressure and vacuum drying with molecular cut off, pulverize, obtain extract 70g.
(4) preparation prescription is: volatile oil clathrate compound 20g, extract 70g, dextran 60g.
(5) get above-mentioned volatile oil clathrate compound, extract and add the dissolving of injection water, filter, add dextran, add the injection water, regulate pH value to 7.0-7.5 to ormal weight, filtering with microporous membrane, fill, lyophilization promptly gets 500.
Embodiment 3:
(1) prescription of crude drug is: Herba Taraxaci 1000g, Herba Houttuyniae 1000g, Flos Chrysanthemi Indici 1000g.
(2) get Herba Houttuyniae, Flos Chrysanthemi Indici medical material, soaked 1 hour, extract volatile oil with steam distillation, the volatile oil of collecting is slowly added in HP-β-CD saturated aqueous solution, 50 ℃ of-60 ℃ of heat-retaining conditions stirred 4 hours down, continued under the room temperature to stir 3 hours, and cold preservation is spent the night, filter, vacuum drying obtains clathrate 25g.
(3) Herba Taraxaci and Herba Houttuyniae, Flos Chrysanthemi Indici medicinal residues add the water extraction 2 times of 10 times of amounts, each 1 hour again; Merge decoction liquor twice, leave standstill, filter, filtrate is concentrated into the extractum that relative density is 1.20-1.24, adds ethanol and makes and contain the alcohol amount and reach 70%, left standstill 12 hours, filter, decompression filtrate recycling ethanol is not to there being the alcohol flavor, and thin up is to solution: medical material is 1: 1, medicinal liquid is crossed the macroporous adsorptive resins of having handled well, behind the water elution with 5 times of column volumes, 6 times of amounts of reuse column volume, 50% ethanol elution merges ethanol elution earlier, decompression recycling ethanol also concentrates, thin up is to solution: medical material is 1: 0.5, is that 20000 ultrafilter membrane carries out ultrafiltration, ultrafiltrate concentrating under reduced pressure and vacuum drying with molecular cut off, pulverize, obtain extract 80g.
(4) preparation prescription is; Volatile oil clathrate compound 25g, extract 80g, lactose 35g.
(5) get above-mentioned volatile oil clathrate compound, extract and add the dissolving of injection water, filter, add lactose, add the injection water, regulate pH value to 7.0-7.5 to ormal weight, filtering with microporous membrane, fill, lyophilization promptly gets 500.
Embodiment 4:
(1) prescription of crude drug is: Herba Taraxaci 800g, Herba Houttuyniae 800g, Flos Chrysanthemi Indici 800g.
(2) get Herba Houttuyniae, Flos Chrysanthemi Indici medical material, soaked 1 hour, extract volatile oil with steam distillation, the volatile oil of collecting is slowly added in HP-β-CD saturated aqueous solution, 50 ℃ of-60 ℃ of heat-retaining conditions stirred 3 hours down, continued under the room temperature to stir 3 hours, and cold preservation is spent the night, filter, vacuum drying obtains clathrate 10g.
(3) Herba Taraxaci and Herba Houttuyniae, Flos Chrysanthemi Indici medicinal residues add the water extraction 2 times of 8 times of amounts, each 1 hour again; Merge decoction liquor twice, leave standstill, filter, filtrate is concentrated into the extractum that relative density is 1.20-1.24, adds ethanol and makes and contain the alcohol amount and reach 70%, left standstill 12 hours, filter, decompression filtrate recycling ethanol is not to there being the alcohol flavor, and thin up is to solution: medical material is 1: 1, medicinal liquid is crossed the macroporous adsorptive resins of having handled well, behind the water elution with 4 times of column volumes, 5 times of amounts of reuse column volume, 50% ethanol elution merges ethanol elution earlier, decompression recycling ethanol also concentrates, thin up is to solution: medical material is 1: 0.5, is that 10000 ultrafilter membrane carries out ultrafiltration, ultrafiltrate concentrating under reduced pressure and vacuum drying with molecular cut off, pulverize, obtain extract 50g.
(4) preparation prescription is: volatile oil clathrate compound 10g, extract 50g, mannitol 40g, lactose 20g.
(5) get above-mentioned volatile oil clathrate compound, extract and add the dissolving of injection water, filter, add pharmaceutic adjuvant, add the injection water, regulate pH value to 7.0-7.5 to ormal weight, filtering with microporous membrane, fill, lyophilization promptly gets 500.
Embodiment 5:
(1) prescription of crude drug is: Herba Taraxaci 1200g, Herba Houttuyniae 1200g, Flos Chrysanthemi Indici 1200g.
(2) get Herba Houttuyniae, Flos Chrysanthemi Indici medical material, soaked 1 hour, extract volatile oil with steam distillation, the volatile oil of collecting is slowly added in HP-β-CD saturated aqueous solution, 50 ℃ of-60 ℃ of heat-retaining conditions stirred 2 hours down, continued under the room temperature to stir 3 hours, and cold preservation is spent the night, filter, vacuum drying obtains clathrate 30g.
(3) Herba Taraxaci and Herba Houttuyniae, Flos Chrysanthemi Indici medicinal residues add the water extraction 2 times of 10 times of amounts, each 1 hour again; Merge decoction liquor twice, leave standstill, filter, filtrate is concentrated into the extractum that relative density is 1.20-1.24, adds ethanol and makes and contain the alcohol amount and reach 60%, left standstill 12 hours, filter, decompression filtrate recycling ethanol is not to there being the alcohol flavor, and thin up is to solution: medical material is 1: 1, medicinal liquid is crossed the macroporous adsorptive resins of having handled well, behind the water elution with 3 times of column volumes, 6 times of amounts of reuse column volume, 55% ethanol elution merges ethanol elution earlier, decompression recycling ethanol also concentrates, thin up is to solution: medical material is 1: 0.5, is that 10000 ultrafilter membrane carries out ultrafiltration, ultrafiltrate concentrating under reduced pressure and vacuum drying with molecular cut off, pulverize, obtain extract 100g.
(4) preparation prescription is: volatile oil clathrate compound 30g, extract 100g, glucose 30g.
(5) get above-mentioned volatile oil clathrate compound, extract and add the dissolving of injection water, filter, add glucose, add the injection water, regulate pH value to 7.0-7.5 to ormal weight, filtering with microporous membrane, fill, lyophilization promptly gets 500.
Claims (1)
1. compound dandelion freeze dried powder injection, it is characterized in that it is that the extract 5-10 weight portion and the pharmaceutic adjuvant of Herba Taraxaci, Herba Houttuyniae, Flos Chrysanthemi Indici co-extracted are prepared from by the HP-beta-CD inclusion 1-3 weight portion of the volatile oil of Herba Houttuyniae, Flos Chrysanthemi Indici co-extracted; General flavone content is 35%-50% in the extract, and chlorogenic acid content is 0.5%-0.8%, and caffeic acid content is 0.3%-0.5%; Its preparation method is:
(1) raw material medicines in portions by weight consists of: Herba Taraxaci 8-12 part, Herba Houttuyniae 8-12 part, Flos Chrysanthemi Indici 8-12 part;
(2) get Herba Houttuyniae, Flos Chrysanthemi Indici medical material, soaked 1 hour, extract volatile oil with steam distillation, the volatile oil of collecting is slowly added in HP-β-CD saturated aqueous solution, 50 ℃ of-60 ℃ of heat-retaining conditions stirred 2-4 hour down, continued under the room temperature to stir 3 hours, and cold preservation is spent the night, filter, vacuum drying obtains clathrate;
(3) Herba Taraxaci and Herba Houttuyniae, Flos Chrysanthemi Indici medicinal residues add the water extraction 2 times that 6-10 doubly measures, each 1 hour again; Merge decoction liquor twice, leave standstill, filter, filtrate is concentrated into the extractum that relative density is 1.20-1.24, adds ethanol and makes and contain the alcohol amount and reach 60%-70%, left standstill 12 hours, filter, decompression filtrate recycling ethanol is not to there being the alcohol flavor, and thin up is to solution: medical material is 1: 1, medicinal liquid is crossed the macroporous adsorptive resins of having handled well, behind the water elution with 3-5 times of column volume, reuse 4-6 doubly measures column volume 40%-70% ethanol elution earlier, merges ethanol elution, decompression recycling ethanol also concentrates, thin up is to solution: medical material is 1: 0.5, is that the ultrafilter membrane of 5000-20000 carries out ultrafiltration, ultrafiltrate concentrating under reduced pressure and vacuum drying with molecular cut off, pulverize, obtain extract;
(4) get above-mentioned clathrate, extract and add the dissolving of injection water, filter, add pharmaceutic adjuvant, add the injection water, regulate pH value to 7.0-7.5 to ormal weight, filtering with microporous membrane, fill, lyophilization, promptly.
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| CN 200510056774 CN1283268C (en) | 2005-03-25 | 2005-03-25 | Compound dandelion freeze dried powder injection and its preparation method |
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| CN 200510056774 CN1283268C (en) | 2005-03-25 | 2005-03-25 | Compound dandelion freeze dried powder injection and its preparation method |
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| CN102018793B (en) * | 2010-12-23 | 2012-07-25 | 魏明黎 | Medicine and rectum drop detoxification solution used for treating tumour and drop appliance of rectum drop detoxification solution |
| CN102894437A (en) * | 2011-07-25 | 2013-01-30 | 江西食方食坊中药食品有限公司 | Honeysuckle-lotus plumule beverage with functions of heat clearing and pathogenic fire reducing, and preparation method thereof |
| CN103181972A (en) * | 2011-12-30 | 2013-07-03 | 广西壮族自治区花红药业股份有限公司 | Tablet or capsule of traditional Chinese medicine for treating wind-heat type common cold and upper respiratory infection, and preparation method thereof |
| CN103432262A (en) * | 2013-08-23 | 2013-12-11 | 甘孜藏族自治州畜牧业科学研究所 | Tibetan veterinary medicine and preparation method thereof |
| CN105287682B (en) * | 2014-06-18 | 2019-12-06 | 鲁南制药集团股份有限公司 | preparation method of dandelion extract |
| CN105646194B (en) * | 2014-11-21 | 2018-05-15 | 中国人民解放军第二军医大学 | The preparation and application of artemisia anomalas extract 3,4- dihydroxycinnamic acids |
| CN105125706A (en) * | 2015-08-04 | 2015-12-09 | 苏州泽达兴邦医药科技有限公司 | Dandelion-containing traditional Chinese medicinal composition with functions of clearing away heat and toxic materials, relieving sore-throat and eliminating phlegm and preparation method |
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