CN1616038A - Wild chrysanthemum flower freeze-dried powder injection and its preparing method - Google Patents
Wild chrysanthemum flower freeze-dried powder injection and its preparing method Download PDFInfo
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Abstract
The freeze dried wild chrysanthemum flower powder for injection consists of HP-beta-CD included volatile wild chrysanthemum flower oil, wild chrysanthemum flower extract and medicinal supplementary material. The volatile oil is prepared through vapor distillation process and included with HP-beta-CD for high stability, easy absorption and high bioavailability. The wild chrysanthemum flower extract is obtained through water extraction, alcohol deposition and macroporous resin separation and purification, and has total flavone content higher than 50 % and chlorogenic acid content higher than 0.6 % in its main effective components. The present invention also discloses the preparation process, content measurement result and pharmacological result. The preparation of the present invention has high effective component content and high pharmacological effect.
Description
Affiliated technical field
The invention belongs to technical field of traditional Chinese medicine pharmacy, be specifically related to a kind of Wild chrysanthemum flower freeze-dried powder injection and preparation method thereof.
Background technology
Flos Chrysanthemi Indici is the head inflorescence of Compositae herbaceos perennial Herba Dendranthematis indici etc., calls the bitter heart of a lotus seed.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." book on Chinese herbal medicine converges and says " claims that it can " removing blood stasis be soothing the liver, separates furuncle and looses malicious.Stagnated blood in housewife people's abdomen, the red furuncle of the capable fire-toxin of Xie Tian.Wash the skin ulcer scabies, can remove the wind parasite killing again ".Contained chlorogenic acid, volatile oil and flavone compound is the main effective ingredient of its performance drug effect in the Flos Chrysanthemi Indici.The preparation that has gone on the market has Flos Chrysanthemi Indici granule, Flos Chrysanthemi Indici suppository and Flos Chrysanthemi indici injection (WS-11041 (ZD-1041)-2002), wherein injection has heat-clearing toxin-expelling functions, is used for fever caused by exogenous pathogenic factors, conjunctival congestion and swelling pain, has sore throat, upper respiratory tract infection, acute tonsillitis belongs to merit person on the pyretic toxicity.Flos Chrysanthemi indici injection is owing to contain chlorogenic acid and volatile oil composition, and unstable product quality to having relatively high expectations of preserving, is preserved improper medicinal liquid and can be occurred situations such as muddiness, precipitation, variable color owing to oxidation; Only chlorogenic acid contents is measured in the injection quality standard, can not be reflected the another kind of active component content of flavonoids of Flos Chrysanthemi Indici situation; Injection is owing to adopted two step alcohol deposition methods in the injection preparation technology simultaneously, and loss of effective components is big in the precipitate with ethanol process; Injection is to the stability requirement height, carry, store, broken easily when transporting, also result in hand cramps.
Patent (CN1014611B) discloses a kind of preparation method of Flos Chrysanthemi Indici concrete, and extractum mainly contains the oils composition; Patent (application number 01100043) discloses a kind of nanometer wild chrysanthemum preparation medicine and preparation method thereof, it is characterized in that with nanometer Flos Chrysanthemi Indici prepared slices of Chinese crude drugs useful in preparing drug formulations.。
In data-searching, do not find the report of other relevant Wild chrysanthemum flower freeze-dried powder injection.
Summary of the invention
The objective of the invention is to disclose a kind of active component, good effect, steady quality, convenient Flos Chrysanthemi Indici freeze-dried powder that uses of being rich in.
Another object of the present invention provides the preparation method of above-mentioned freeze-dried powder.
The present invention is achieved through the following technical solutions.
One, preparation method
(1) prescription of crude drug is: Flos Chrysanthemi Indici.
(2) get the 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 5 hours, and cold preservation is spent the night, filter, 60 ℃ of dryings obtain clathrate.
(3) the water liquid that extracts behind the volatile oil filters, and medicinal residues add the water extraction 2 times that 6-8 doubly measures, each 1 hour again; Merge decoction liquor twice, leave standstill, filter, merging is carried the filtrate behind the oil and is decocted filtrate, is concentrated into the extractum that relative density is 1.20-1.24, adding ethanol makes the alcohol amount of containing reach 60%-70%, left standstill 12 hours, and filtered, decompression filtrate recycling ethanol is to there not being the alcohol flavor, 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, after column volume 40%-50% ethanol elution is doubly measured with 2-4 by elder generation, reuse 3-5 times of column volume 60%-80% ethanol water eluting, merge ethanol elution, concentrating under reduced pressure, drying, 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 5.5-7.0 to ormal weight, filtering with microporous membrane, fill, lyophilization, promptly.
In the preparation of Wild chrysanthemum flower freeze-dried powder injection, adopt steam distillation to extract volatile oil in 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.Contain a large amount of effective ingredient flavone compound and chlorogenic acid in the Flos Chrysanthemi Indici water extract, we adopt classical decoction and alcohol sedimentation technique after removing partial impurities, with macroporous adsorbent resin chlorogenic acid and total flavones have been carried out separation and purification again, use earlier the 40%-50% ethanol elution during eluting, make chlorogenic acid and part flavone by eluting, reuse 60-80% ethanol elution makes most of flavones ingredient by eluting.The content of main effective ingredient total flavone valid target is greater than 50% in the Flos Chrysanthemi Indici extract after purified, and chlorogenic acid content is greater than 0.6%.Simultaneously, labile element chlorogenic acid after the lyophilizing in the preparation and volatile oil are 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.
During the macroporous resin eluting, the concentration of alcohol of eluting macroporous adsorbent resin preferably is preferably 44-46% for the first time among the above preparation technology.The concentration of alcohol of eluting macroporous adsorbent resin is preferably 68-72% for the second time.
Two, assay analysis
1, content of total flavone is measured in the wild chrysanthemum preparation
1.1 instrument and reagent day island proper Tianjin UV-3000A ultraviolet spectrophotometer.Flos Chrysanthemi indici injection (Sanjiu Pharmaceutical Industry Co., Ltd., Ya'an City); Wild chrysanthemum flower freeze-dried powder injection of the present invention (Qianluchun Science and Technology Co., Ltd., Beijing'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 content 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
Content (mg/ props up)
Lot number Flos Chrysanthemi indici injection Wild chrysanthemum flower freeze-dried powder injection of the present invention
1 36.0 46.2
2 35.8 44.0
3 33.0 48.4
2, the assay of chlorogenic acid in the wild chrysanthemum preparation
Content assaying method with reference to chlorogenic acid in Flos Chrysanthemi indici injection (WS-110419 (ZD-1041)-2002) quality standard is measured, and the results are shown in Table 2
Determination of chlorogenic acid in table 2 preparation
Content (mg/ props up)
Lot number Flos Chrysanthemi indici injection Wild chrysanthemum flower freeze-dried powder injection of the present invention
1 0.24 0.56
2 0.22 0.57
3 0.21 0.51
Above assay presentation of results, total flavones in the Wild chrysanthemum flower freeze-dried powder injection of the present invention and chlorogenic acid content are apparently higher than total flavones and the chlorogenic acid content of Flos Chrysanthemi indici injection (WS-11041 (ZD-1041)-2002).Illustrate that preparation method of the present invention is more reasonable, science has more practicality more.
3, total flavones and chlorogenic acid contents are measured in the extract
Determining instrument, reagent and method are the same.Flos Chrysanthemi Indici extract of the present invention is by preparation method gained of the present invention; Flos Chrysanthemi indici injection extract (according to the method for making gained in (WS-11041 (ZD-1041)-2002)); The results are shown in Table 3 and table 4.
Total flavones in table 3 extract (in anhydrous rutin) assay
Content (%)
Batch
Flos Chrysanthemi indici injection extract Flos Chrysanthemi Indici extract of the present invention
1 36.5 57.8
2 35.8 55.0
3 33.9 60.5
Determination of chlorogenic acid in table 4 extract
Content (%)
Batch
Flos Chrysanthemi indici injection extract Flos Chrysanthemi Indici extract of the present invention
1 0.24 0.71
2 0.22 0.71
3 0.22 0.64
Above assay presentation of results, effective ingredient total flavones in the extract that preparation method of the present invention obtains and chlorogenic acid content total flavones and the chlorogenic acid content in the Flos Chrysanthemi indici injection extract (according to the method for making gained in (WS-11041 (ZD-1041)-2002)).Illustrate that preparation method of the present invention is more reasonable, science has more practicality more.
Four, pharmacology embodiment
Reagent; Normal saline (Qianluchun Science and Technology Co., Ltd., Beijing's laboratory provides)
Flos Chrysanthemi indici injection (Sanjiu Pharmaceutical Industry Co., Ltd., Ya'an City)
Wild chrysanthemum flower freeze-dried powder injection of the present invention (Qianluchun Science and Technology Co., Ltd., Beijing's laboratory provides).
Animal: Kunming mouse, body weight 18-22g, 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.
Virocyte: anti-/ 359/95 (H3N2) of the influenza virus A3/ Chinese draws from national influenza center.
1. bacteriostatic test
Experimental technique: 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 Flos Chrysanthemi Indici lyophilized powder solution and injection, cultivated 24 hours for 37 ℃, observe the inhibition zone size, the results are shown in Table 5.
Table 5 bacteriostatic experiment result
Flos Chrysanthemi indici injection Flos Chrysanthemi Indici lyophilized powder of the present invention
Antibacterial (mm) (mm)
Streptococcus pneumoniae (10
10Individual/ml) 9 15
Escherichia coli (10
5Individual/ml) 7 13
Staphylococcus aureus (10
5Individual/ml) 7 14
Pseudomonas aeruginosa (10
5Individual/ml) 7 13
Shigella flexneri (10
5Individual/ml) 8 15
Wild chrysanthemum flower freeze-dried powder injection of the present invention and Flos Chrysanthemi indici injection all can form the inhibition zone of certain diameter to above antibacterial, show stronger bacteriostasis, but the bacteriostasis of Wild chrysanthemum flower freeze-dried powder injection of the present invention is obviously strong than Flos Chrysanthemi indici injection, illustrates: the pharmacological action of Wild chrysanthemum flower freeze-dried powder injection of the present invention is better than Flos Chrysanthemi indici injection.
2. to the influence of mortality rate due to the white mice intranasal vaccination influenza virus A3 strain
Experimental technique: get 50 of white mice, random packet, 10 every group, press 60g/kg dosage lumbar injection Flos Chrysanthemi Indici lyophilized powder, every day 1 time, 7d continuously, simultaneously do parallel control with normal saline, Flos Chrysanthemi indici injection, 2h after administration in the 7th day with influenza virus A3 strain intranasal vaccination 0.2ml/ only, is an index with the mice dying, observe 48h, write down each treated animal death toll, the same procedure triplicate the results are shown in Table 6
The influence of table 6 popularity cold virus A3 strain intranasal vaccination mouse death rate
Group death toll/total mortality rate P value
23/30 76.7 ＜0.01
Normal saline
5/30 16.7 ＜0.05
Flos Chrysanthemi indici injection 0,/30 0
Flos Chrysanthemi Indici lyophilized powder of the present invention
Wild chrysanthemum flower freeze-dried powder injection of the present invention and Flos Chrysanthemi indici injection all can significantly reduce influenza virus A3 strain intranasal vaccination induced mice mortality rate, be remarkable anti-virus ability, but the antivirus action of Wild chrysanthemum flower freeze-dried powder injection of the present invention is obviously strong than Flos Chrysanthemi indici injection, illustrates: the pharmacological action of Wild chrysanthemum flower freeze-dried powder injection of the present invention is better than Flos Chrysanthemi indici injection.
Six, preparation embodiment
Embodiment 1:
(1) prescription of crude drug is: Flos Chrysanthemi Indici 1000g.
(2) get the 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 5 hours, and cold preservation is spent the night, filter, 60 ℃ of dryings obtain clathrate.
(3) the water liquid that extracts behind the volatile oil filters, and medicinal residues add the water extraction 2 times of 7 times of amounts, each 1 hour again; Merge decoction liquor twice, leave standstill, filter, merge and carry the filtrate behind the oil and decoct filtrate, be concentrated into relative density and be 1.22 extractum, adding ethanol makes and contains alcohol amount and reach 65%, left standstill 12 hours, and filtered, decompression filtrate recycling ethanol is to there not being the alcohol flavor, thin up is to solution: medical material is 1: 1, medicinal liquid is crossed the AB-8 macroporous adsorptive resins of having handled well, behind the water elution with 4 times of column volumes, earlier with behind 3 times of amount column volume 45% ethanol elutions, 4 times of column volumes of reuse, 70% ethanol water eluting, merge ethanol elution, concentrating under reduced pressure, drying, pulverize, obtain extract.
(4) get above-mentioned clathrate, extract and add the dissolving of injection water, filter, add mannitol and glucosan, add the injection water, regulate pH value to 5.5-7.0 to ormal weight, filtering with microporous membrane, fill, lyophilization promptly gets 500.
One time 1-2 props up, 2 times on the one.
Embodiment 2:
(1) prescription of crude drug is: Flos Chrysanthemi Indici 800g.
(2) get the 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 5 hours, and cold preservation is spent the night, filter, 60 ℃ of dryings obtain clathrate.
(3) the water liquid that extracts behind the volatile oil filters, and medicinal residues add the water extraction 2 times of 6 times of amounts, each 1 hour again; Merge decoction liquor twice, leave standstill, filter, merge and carry the filtrate behind the oil and decoct filtrate, be concentrated into relative density and be 1.20 extractum, adding ethanol makes and contains alcohol amount and reach 60%, left standstill 12 hours, and filtered, decompression filtrate recycling ethanol is to there not being the alcohol flavor, thin up is to solution: medical material is 1: 1, medicinal liquid is crossed the D101 macroporous adsorptive resins of having handled well, behind the water elution with 3 times of column volumes, earlier with behind 2 times of amount column volume 40% ethanol elutions, 3 times of column volumes of reuse, 60% ethanol water eluting, merge ethanol elution, concentrating under reduced pressure, drying, pulverize, obtain extract.
(4) get above-mentioned clathrate, extract and add the dissolving of injection water, filter, add polyvinylpyrrolidone, add the injection water, regulate pH value to 5.5-7.0 to ormal weight, filtering with microporous membrane, fill, lyophilization promptly gets 500.
One time 1-2 props up, 2 times on the one.
Embodiment 3:
(1) prescription of crude drug is: Flos Chrysanthemi Indici 1200g.
(2) get the 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 5 hours, and cold preservation is spent the night, filter, 60 ℃ of dryings obtain clathrate.
(3) the water liquid that extracts behind the volatile oil filters, and medicinal residues add the water extraction 2 times of 8 times of amounts, each 1 hour again; Merge decoction liquor twice, leave standstill, filter, merge and carry the filtrate behind the oil and decoct filtrate, be concentrated into relative density and be 1.24 extractum, adding ethanol makes and contains alcohol amount and reach 70%, left standstill 12 hours, and filtered, decompression filtrate recycling ethanol is to there not being the alcohol flavor, thin up is to solution: medical material is 1: 1, medicinal liquid is crossed the D101 macroporous adsorptive resins of having handled well, behind the water elution with 5 times of column volumes, earlier with behind 4 times of amount column volume 50% ethanol elutions, 5 times of column volumes of reuse, 80% ethanol water eluting, merge ethanol elution, concentrating under reduced pressure, drying, pulverize, obtain extract.
(4) get above-mentioned clathrate, extract and add the dissolving of injection water, filter, add glucosan, polyvinylpyrrolidone and glucose, add the injection water, regulate pH value to 5.5-7.0 to ormal weight, filtering with microporous membrane, fill, lyophilization promptly gets 500.
One time 1-2 props up, 2 times on the one.
Embodiment 4:
(1) prescription of crude drug is: Flos Chrysanthemi Indici 900g.
(2) get the 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 5 hours, and cold preservation is spent the night, filter, 60 ℃ of dryings obtain clathrate.
(3) the water liquid that extracts behind the volatile oil filters, and medicinal residues add the water extraction 2 times of 8 times of amounts, each 1 hour again; Merge decoction liquor twice, leave standstill, filter, merge and carry the filtrate behind the oil and decoct filtrate, be concentrated into relative density and be 1.24 extractum, adding ethanol makes and contains alcohol amount and reach 65%, left standstill 12 hours, and filtered, decompression filtrate recycling ethanol is to there not being the alcohol flavor, thin up is to solution: medical material is 1: 1, medicinal liquid is crossed the AB-8 macroporous adsorptive resins of having handled well, behind the water elution with 4 times of column volumes, earlier with behind 3 times of amount column volume 45% ethanol elutions, 5 times of column volumes of reuse, 65% ethanol water eluting, merge ethanol elution, concentrating under reduced pressure, drying, pulverize, obtain extract.
(4) get above-mentioned clathrate, extract and add the dissolving of injection water, filter, add dextrorotation fructose and lactose, add the injection water, regulate pH value to 5.5-7.0 to ormal weight, fill, lyophilization promptly gets 500.
One time 1-2 props up, 2 times on the one.
Embodiment 5:
(1) prescription of crude drug is: Flos Chrysanthemi Indici 1100g.
(2) get the 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 5 hours, and cold preservation is spent the night, filter, 60 ℃ of dryings obtain clathrate.
(3) the water liquid that extracts behind the volatile oil filters, and medicinal residues add the water extraction 2 times of 6 times of amounts, each 1 hour again; Merge decoction liquor twice, leave standstill, filter, merging is carried the filtrate behind the oil and is decocted filtrate, be concentrated into relative density and be 1.23 extractum, add ethanol and make and contain alcohol amount and reach 65%, left standstill 12 hours, filter, merging is carried the filtrate behind the oil and is decocted filtrate, decompression recycling ethanol is not to there being the alcohol flavor, and thin up is to solution: medical material is 1: 1, and medicinal liquid is crossed the AB-8 macroporous adsorptive resins of having handled well, behind the water elution with 3 times of column volumes, with behind 3 times of amount column volume 45% ethanol elutions, 4 times of column volumes of reuse, 70% ethanol water eluting merges ethanol elution earlier, concentrating under reduced pressure, drying is pulverized, and obtains extract.
(4) get above-mentioned clathrate, extract and add the dissolving of injection water, filter, add glucose and fructose, add the injection water, regulate pH value to 5.5-7.0 to ormal weight, filtering with microporous membrane, fill, lyophilization promptly gets 500.
One time 1-2 props up, 2 times on the one.
Claims (7)
1, a kind of Wild chrysanthemum flower freeze-dried powder injection is characterized in that it is to be prepared from by Flos Chrysanthemi Indici volatile oil HP-beta-CD inclusion, Flos Chrysanthemi Indici extract and pharmaceutic adjuvant; Its feature is that also the effective site content of total flavone is more than or equal to 50% in the Flos Chrysanthemi Indici extract, and chlorogenic acid content is more than or equal to 0.6%.
2, lyophilized injectable powder according to claim 1 is characterized in that pharmaceutic adjuvant is a kind of, two or more the mixture in mannitol, glucosan, polyvinylpyrrolidone, glucose, fructose, dextrorotation fructose and the lactose.
3, a kind of preparation method of Wild chrysanthemum flower freeze-dried powder injection, its feature may further comprise the steps:
(1) prescription of crude drug is: Flos Chrysanthemi Indici.
(2) get the 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 5 hours, and cold preservation is spent the night, filter, 60 ℃ of dryings obtain clathrate.
(3) the water liquid that extracts behind the volatile oil filters, and medicinal residues add the water extraction 2 times that 6-8 doubly measures, each 1 hour again; Merge decoction liquor twice, leave standstill, filter, merging is carried the filtrate behind the oil and is decocted filtrate, is concentrated into the extractum that relative density is 1.20-1.24, adding ethanol makes the alcohol amount of containing reach 60%-70%, left standstill 12 hours, and filtered, decompression filtrate recycling ethanol is to there not being the alcohol flavor, 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, after column volume 40%-50% ethanol elution is doubly measured with 2-4 by elder generation, reuse 3-5 times of column volume 60%-80% ethanol water eluting, merge ethanol elution, concentrating under reduced pressure, drying, 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 5.5-7.0 to ormal weight, filtering with microporous membrane, fill, lyophilization, promptly.
4, preparation method according to claim 3 is characterized in that, macroporous adsorbent resin is nonpolar or low pole.
5, preparation method according to claim 3 is characterized in that, macroporous adsorbent resin is preferably AB-8 or D101 type.
6, preparation method according to claim 3 is characterized in that, the concentration of alcohol of eluting macroporous adsorbent resin is 44-46% for the first time.
7, preparation method according to claim 3 is characterized in that, the concentration of alcohol of eluting macroporous adsorbent resin is 68-72% for the second time.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1899339B (en) * | 2006-07-24 | 2011-11-09 | 成都三明药物研究所 | Medicinal composition for treating acute and chronic conjunctivitis for eye and its preparing method |
| CN103142674A (en) * | 2013-01-30 | 2013-06-12 | 时维静 | Preparation method for Chuzhou chrysanthemum extract powder |
| CN103142674B (en) * | 2013-01-30 | 2014-02-12 | 时维静 | Preparation method for Chuzhou chrysanthemum extract powder |
| CN103976453A (en) * | 2014-05-16 | 2014-08-13 | 南京中医药大学 | Chuzhou chrysanthemum extract, solid beverage, lozenges and food additive as well as preparation method of Chuzhou chrysanthemum extract |
| CN103976453B (en) * | 2014-05-16 | 2015-12-30 | 南京中医药大学 | Chu chrysanthemum extract, solid beverage, lozenge and food additives and preparation method thereof |
| CN104490973A (en) * | 2014-12-02 | 2015-04-08 | 江西钟山药业有限责任公司 | Method for preparing tradtional Chinese medicine wild chrysanthemum injection |
| CN107929105A (en) * | 2017-12-27 | 2018-04-20 | 广州潮徽生物科技有限公司 | Removing miliaria and relieving itching balm that a kind of infant is applicable in and preparation method and application |
| CN107929105B (en) * | 2017-12-27 | 2021-05-04 | 广州潮徽生物科技有限公司 | Prickly heat removing and itching relieving balm suitable for infants and preparation method and application thereof |
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