CN1682957A - Freeze-dried preparation containing honeysuckle flower and astragalus root and its preparing method - Google Patents
Freeze-dried preparation containing honeysuckle flower and astragalus root and its preparing method Download PDFInfo
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Abstract
The freeze dried preparation is obtained with honeysuckle and skullcap root and through proper extraction process and freeze drying process. It has high and stable performance, fast acting, high effect, easy preparation, transportation and storing, and easy use, and is favorable to produce in large scale.
Description
Technical field
The present invention belongs to field of pharmaceutical preparations, specifically, relates to a kind of lyophilized formulations that contains Flos Lonicerae and Radix Scutellariae and preparation method thereof.
Background technology
Flos Lonicerae and Radix Scutellariae have the effect of heat clearing away, detoxifcation and sore-throat relieving, are used for the treatment of wind-heat invading the lung and upper respiratory tract infection and cause diseases such as heating, cough, pharyngalgia, and curative effect is preferably arranged, and clinical demand is big.Though existing YINHUANG ZHUSHEYE, oral liquid, tablets and other formulations are asked the city.CN1398626 and CN1424084 have also announced silver yellow injectable powder and preparation method.And that market presses for preparation method is simple, and cost is low, and performance is good, the pharmaceutical preparation that contains Flos Lonicerae and Radix Scutellariae easy to use.
Summary of the invention
In order to overcome the deficiency of prior art, the object of the present invention is to provide a kind of pharmaceutical preparation that contains Flos Lonicerae and Radix Scutellariae, its performance is good and stable, instant effect, effect is strong, is easy to preparation, transports and stores, and is easy to use.
Another object of the present invention is to provide a kind of above-mentioned method that contains the pharmaceutical preparation of Flos Lonicerae and Radix Scutellariae for preparing, and method is simple for this, and the cycle is short, helps large-scale production.
The appropriate formulation that performance is good, rapid-action, effect is strong in order to seek for the inventor, stable performance, convenient transportation store, having done a large amount of deep researchs explores, find by using suitable extracting method, measures such as employing freeze drying process prepare lyophilized formulations, can solve problems such as stability of formulation and transportation storage effectively, the injection instant effect, good drug efficacy.
The invention provides a kind of pharmaceutical preparation that contains Flos Lonicerae and Radix Scutellariae, it is got by following method preparation:
(1) extract Flos Lonicerae:
(a) Flos Lonicerae is extracted 1～3 time with 8～12 times of water (not comprising the water yield that bole self absorbs), decocts 0.5～1.5 hour, and extracting solution concentrates, and adds ethanol precipitation, filters, and removes ethanol in the filtrate; Add entry, or
(b) Flos Lonicerae is extracted 1～3 time with 6～10 times of ethanol (not comprising the amount of alcohol that bole self absorbs), decocts 0.5～1.5 hour, and extracting solution reclaims ethanol, concentrate,
(c),, reclaim ethyl acetate or n-butyl alcohol with 1～2 times of ethyl acetate or n-butanol extraction 4～6 times with (a) or (b) step gains, add entry, regulating its pH is 3.0～7.0, preferred 5.0, filters, its pH of re-adjustment is 6.0～8.0, preferred 7.0, cold preservation is spent the night, and promptly gets Flos Lonicerae extract, contain crude drug amount 4g/ml～20g/ml, or contain chlorogenic acid 25mg/ml～100mg/ml;
(2) extract Radix Scutellariae: Radix Scutellariae did not decoct with water 1～3 time with 6～10 times (not comprising the water yield that bole self absorbs), decocted 1～2 hour, filtered, filtrate concentrates, and transfers 1.5～2.5,70～90 ℃ of insulations of its pH value 0.5～1.5 hour, left standstill 18～28 hours, and filtered, precipitation is dissolved with 2～4 times of water gagings, transfer its pH value to 6.0～8.0, preferred 7.0, filter the filtrate ethanol precipitation, filter, transfer filtrate pH value to 1～3, preferred 1.5,70～90 ℃ of insulations 0.5～1.5 hour, left standstill 18～28 hours, filter, precipitation is earlier with Diluted Alcohol washing, the dense washing with alcohol of reuse, the precipitation vacuum drying gets Radix Scutellariae extract;
(3) make it contain crude drug amount 4g/ml～20g/ml with water dissolution (2) step gains; Merge with (1) step gains, regulating its pH value is 4.5～8.0, more preferably between 5.0～6.5; Activated carbon decolorizing is removed pyrogen, 0.22 μ m filtering with microporous membrane, lyophilization.
Described pH value can transfer the conventional substances of pH to regulate with this area, for example hydrochloric acid or sodium hydroxide solution.
Can before ethyl acetate or n-butanol extraction, treat that with the concentrated hydrochloric acid accent pH of extract is 1.5～2.5 in described (1) step.
The material that also can further comprise one or more in the acceptable adjuvant on the conventional pharmaceutical such as stabilizing agent, analgesics and buffer agent in the pharmaceutical preparation that contains Flos Lonicerae and Radix Scutellariae of the present invention.
The invention provides a kind of pharmaceutical preparation that contains Flos Lonicerae and Radix Scutellariae, it is got by following method preparation:
(1) extract Flos Lonicerae:
(a) Flos Lonicerae is extracted 1～3 time with 8～12 times of water (not comprising the water yield that bole self absorbs), decocted 0.5～1.5 hour, extracting solution is concentrated into and contains crude drug amount 1: 0.8～1: 2,20～50 ℃ add concentration is 60～80% ethanol precipitations, cold preservation is spent the night, and filters, and removes ethanol in the filtrate, add entry to containing crude drug amount 1: 0.8～1: 2.0, or
(b) Flos Lonicerae is extracted 1～3 time with 6～10 times of ethanol (do not comprise bole self absorb amount of alcohol), decocts 0.5～1.5 hour, and extracting solution recovery ethanol is concentrated into and contains crude drug amount 1: 0.8～1: 2.0,
(c) with (a) or (b) step gains, transferring pH with hydrochloric acid is 1.5～2.5, with 1～2 times of ethyl acetate or n-butanol extraction 4～6 times, reclaim ethyl acetate or n-butyl alcohol, add an amount of water for injection, regulate pH3.0～7.0 with sodium hydroxide solution, preferred 5.0, filter, regulate pH value to 6.0～8.0, preferred 7.0 with sodium hydroxide solution, cold preservation is spent the night, 0.22 the filtering with microporous membrane of μ m promptly gets Flos Lonicerae extract, contains crude drug amount 4g/ml～20g/ml;
(2) extract Radix Scutellariae:
Radix Scutellariae did not decoct with water 1～3 time with 6～10 times (not comprising the water yield that bole self absorbs), decocted 1～2 hour, and filtered merging filtrate, be concentrated into and contain crude drug 0.2～0.8g/ml, concentrated solution left standstill 18～28 hours with 1.5～2.5,70～90 ℃ of insulations of hydrochloric acid adjust pH 0.5-1.5 hour, filter, precipitation is with 2～4 times of water gaging dissolvings, with sodium hydroxide solution adjust pH to 6.0～8.0, preferred 7.0, filter, filtrate adds 0.5～1.5 times of ethanol precipitation, filters, and filtrate is used hydrochloric acid adjust pH to 1.0～3.0, preferred 1.5,80 ℃ are incubated 0.5 hour, leave standstill 24 hours, filter, precipitation is earlier with the washing of 1～3 times of amount Diluted Alcohol, 2～4 times of dense washing with alcohol of amount of reuse, the precipitation vacuum drying gets Radix Scutellariae extract;
(3) with water dissolution (2) step gains, contain crude drug amount 4g/ml～20g/ml; , merge with (1) step gains, regulating its pH value is 4.5～8.0, more preferably between 5.0～6.5;
Add 0.05%～5% in gained solution, preferred 0.1%～2% active carbon stirred 10～30 minutes filtering decarbonization, 0.22 μ m filtering with microporous membrane down at 25 ℃～60 ℃; Treat that with filtering it is-30 ℃～-40 ℃ freeze drying box pre-freeze 2～4 hours that freeze-drying solution is put into temperature, under-10 ℃～-20 ℃ evacuation, sublimation drying 9～12 hours, 0 ℃～10 ℃ dry 3～5 hours again.
The invention provides the method that a kind of preparation contains the lyophilized formulations of Flos Lonicerae and Radix Scutellariae, comprising:
(1) extract Flos Lonicerae:
(a) Flos Lonicerae is extracted 1～3 time with 8～12 times of water (not comprising the water yield that bole self absorbs), decocts 0.5～1.5 hour, and extracting solution concentrates, and adds ethanol precipitation, filters, and removes ethanol in the filtrate; Add entry, or
(b) Flos Lonicerae is extracted 1～3 time with 6～10 times of ethanol (not comprising the amount of alcohol that bole self absorbs), decocts 0.5～1.5 hour, and extracting solution reclaims ethanol, concentrate,
(c),, reclaim ethyl acetate or n-butyl alcohol with 1～2 times of ethyl acetate or n-butanol extraction 4～6 times with (a) or (b) step gains, add entry,, regulating its pH is 3.0～7.0, preferred 5.0, filter, its pH of re-adjustment is 6.0～8.0, preferred 7.0, cold preservation is spent the night, promptly get Flos Lonicerae extract, contain crude drug amount 4g/ml～20g/ml, or contain chlorogenic acid 25mg/ml～100mg/ml;
(2) extract Radix Scutellariae: Radix Scutellariae did not decoct with water 1～3 time with 6～10 times (not comprising the water yield that bole self absorbs), decocted 1～2 hour, filtered, filtrate concentrates, and transfers 1.5～2.5,70～90 ℃ of insulations of its pH value 0.5～1.5 hour, left standstill 18～28 hours, and filtered, precipitation is dissolved with 2～4 times of water gagings, transfer its pH value to 6.0～8.0, preferred 7.0, filter the filtrate ethanol precipitation, filter, transfer filtrate pH value to 1～3, preferred 1.5,70～90 ℃ of insulations 0.5～1.5 hour, left standstill 18～28 hours, filter, precipitation is earlier with Diluted Alcohol washing, the dense washing with alcohol of reuse, the precipitation vacuum drying gets Radix Scutellariae extract;
(3) make it contain crude drug amount 4g/ml～20g/ml with water dissolution (2) step gains; Merge with (1) step gains, regulating its pH value is 4.5～8.0, more preferably between 5.0～6.5; Activated carbon decolorizing is removed pyrogen, 0.22 μ m filtering with microporous membrane, lyophilization.
In described (3) step, acceptable adjuvant on the conventional pharmaceutical can be added, for example: stabilizing agent, analgesics and/or buffer agent etc. in gained solution.
The lyophilization step in described (3) step can be conventional or known freeze drying process step.Described freeze drying process carries out under aseptic condition, can adjust lyophilization cycle according to conventional or known method according to the demand of clinical preparation and concrete production equipment.
The invention provides the method that a kind of preparation contains the medicament freeze-drying preparation of Flos Lonicerae and Radix Scutellariae, also can may further comprise the steps:
(1) extract Flos Lonicerae:
(a) Flos Lonicerae is extracted 1～3 time with 8～12 times of water (do not comprise bole self absorb the water yield), decocts 0.5～1.5 hour, and extracting solution is concentrated into and contains crude drug amount 1: 0.8～1: 2.0,20～50 ℃ add concentration is 60～80% ethanol precipitations, cold preservation is spent the night, and filters, and removes ethanol in the filtrate; Add entry, to containing crude drug amount 1: 0.8～1: 2.0, or
(b) Flos Lonicerae is extracted 1～3 time with 6～10 times of ethanol (do not comprise bole self absorb amount of alcohol), decocts 0.5～1.5 hour, and extracting solution recovery ethanol continues to be concentrated into and contains crude drug amount 1: 0.8～1: 2.0,
(c) with (a) or (b) step gains, transferring pH with hydrochloric acid is 1.5～2.5, with 1～2 times of ethyl acetate or n-butanol extraction 4～6 times, reclaim ethyl acetate or n-butyl alcohol, add an amount of water for injection, regulate pH3.0～7.0 with sodium hydroxide solution, preferred 5.0, filter, regulate pH value to 6.0～8.0, preferred 7.0 with sodium hydroxide solution, cold preservation is spent the night, 0.22 the filtering with microporous membrane of μ m promptly gets Flos Lonicerae extract, contains crude drug amount 4g/ml～20g/ml;
(2) extract Radix Scutellariae:
Radix Scutellariae did not decoct with water 1～3 time with 6～10 times (not comprising the water yield that bole self absorbs), decocted 1～2 hour, and filtered merging filtrate, be concentrated into and contain crude drug 0.2～0.8g/ml, concentrated solution left standstill 18～28 hours with 1.5～2.5,70～90 ℃ of insulations of hydrochloric acid adjust pH 0.5-1.5 hour, filter, precipitation is with 2～4 times of water gaging dissolvings, with sodium hydroxide solution adjust pH to 6.0～8.0, preferred 7.0, filter, filtrate adds 0.5～1.5 times of ethanol precipitation, filters, and filtrate is used hydrochloric acid adjust pH to 1.0～3.0, preferred 1.5,80 ℃ are incubated 0.5 hour, leave standstill 24 hours, filter, precipitation is earlier with the washing of 1～3 times of amount Diluted Alcohol, 2～4 times of dense washing with alcohol of amount of reuse, the precipitation vacuum drying gets Radix Scutellariae extract;
(3) with water dissolution (2) step gains, contain crude drug amount 4g/ml～20g/ml; Merge with (1) step gains, regulating its pH value is 4.5～8.0, more preferably between 5.0～6.5;
Add 0.05%～5% in gained solution, preferred 0.1%～2% active carbon stirred 10～30 minutes filtering decarbonization, 0.22 μ m filtering with microporous membrane down at 25 ℃～60 ℃; Treat that with filtering it is-30 ℃～-40 ℃ freeze drying box pre-freeze 2～4 hours that freeze-drying solution is put into temperature, under-10 ℃～-20 ℃ evacuation, sublimation drying 9～12 hours, 0 ℃～10 ℃ dry 3～5 hours again.
Should avoid the contact such as metal ions such as ferrum in the process of preparation preparation of the present invention, it might influence the color of preparation, and medicament contg is descended.
Lyophilized formulations of the present invention can be dissolved in water for injection or other injection to lyophilized formulations before using.Described injection can be conventional injection, as is used for the isotonic water medium of venoclysis, for example 5% glucose injection or 0.9% sodium chloride injection.
Pharmaceutical preparation provided by the invention, performance is good and stable, and dissolving is rapidly fully used easily in use.And preparation method of the present invention is simple and easy to do, and is simpler than the method for prior art, and manufacturing cycle is short, helps large-scale production.
The specific embodiment
Below will the invention will be further described by embodiment, these descriptions are not that content of the present invention is done further to limit.One skilled in the art will understand that to be equal to replacement to what technical characterictic of the present invention was done, or corresponding the improvement, still belong within protection scope of the present invention.
Embodiment 1-3
Extracting honeysuckle, add 12 respectively, 8,10 times water (does not comprise the water yield that bole self absorbs, so add 2 times of water during with bole) decoct 3 times, reflux half respectively, one, one and a half hours, merge extractive liquid,, being evaporated to extracting solution crude drug content was respectively 1: 1.5,1: 1,1: 2, add 60% while hot, 70% or 80% ethanol precipitation, cold preservation is spent the night, filter, with filtrate revolving steam do not have an alcohol flavor till, adding suitable quantity of water is that the crude drug amount is 1: 1.5 in the solution, 1: 1,1: 2, transfer pH1.5 with concentrated hydrochloric acid, 2.0,2.5, with 1.5,2,1 times ethyl acetate extraction 4,5,6 times, reclaim ethyl acetate till do not have an ethyl acetate, add water for injection, the water for injection addition so that in the gained solution crude drug content be that 5-20g/ml is advisable, sodium hydroxide solution is regulated pH5.0, filters, regulate ph7.0 with sodium hydroxide solution, after cold preservation is spent the night, cross the microporous filter membrane of 0.22 μ m, promptly.
Embodiment 4-6
Extract Flos Lonicerae according to the method for implementing 1-3, only be to use 70% ethanol to replace water, use 10,8,6 ethanol respectively as extractant.After extracting solution reclaimed ethanol, being concentrated into the crude drug amount was 1: 1.5,1: 1,1: 2.Again according to steps such as the method for embodiment 1-3 extract, Flos Lonicerae extractive solution.
Embodiment 7-9
Get Radix Scutellariae, add 6 respectively, 8,10 times water (not comprising the water yield that bole self absorbs, so add 2 times of water during with bole) decocts with water 1,2,3 times, decoct 1 at every turn, 1.5,2 hours, filter, merging filtrate is concentrated into and contains crude drug 0.2,0.5, (0.8g/ml 85 ℃ of relative densities are 1.1), concentrated solution hydrochloric acid adjust pH to 2.0,1.5,2.5,70,80,90 ℃ of insulations 0.5,1,1.5 hour, leave standstill 18,24,28 hours, filter, precipitation is with 2,3,4 times of water gaging dissolvings, with 40% sodium hydroxide adjust pH to 7.0, filter, filtrate adds 0.5,1,1.5 ethanol precipitation filters, filtrate is used hydrochloric acid adjust pH to 1.5,80 ℃ are incubated 0.5 hour, leave standstill 24 hours, filter, precipitation is earlier with 2 times of amount 50% washing with alcohol, 3 times of amounts of reuse, 95% washing with alcohol, the precipitation vacuum drying, it is standby to get Radix Scutellariae extract.
Embodiment 10
With 30,15,50 parts of dissolvings of water for injection embodiment 7-9 gains, mix with embodiment 1,2,5 gains respectively, transfer pH6.5-8.0, consumption according to 1,0.6,2% (g/ml) adds active carbon, 25,30,55 ℃ were stirred 30,20,10 minutes down, decarbonization filtering, gained filtrate is with 0.22 μ m microporous filter membrane fine straining degerming.
Under aseptic condition gained solution is placed aseptic cillin bottle, put in the freezer dryer according to the method lyophilization of embodiment 12 after about respectively 22,25,30 hours, sterile sealing promptly gets lyophilized formulations A, B, the C that contains Flos Lonicerae and Radix Scutellariae of the present invention.
Embodiment 11
With 30 parts of dissolvings of water for injection embodiment, 8 gains, mix with embodiment 3 gains respectively, transfer pH6.5-8.0, consumption according to 0.2% (g/ml) adds active carbon, 30 ℃ were stirred 30 minutes down, decarbonization filtering, and gained filtrate is with 0.22 μ m microporous filter membrane fine straining degerming.Under aseptic condition gained solution is put in the aseptic cillin bottle, put in the freezer dryer after the lyophilization, sterile sealing promptly gets lyophilized formulations D of the present invention.
Embodiment 12
With embodiment 10 gained solution lyophilizations in accordance with the following methods, prepare lyophilized formulations of the present invention:
Treat that lyophilizing solution puts into-30 ℃ ,-35 ℃ ,-40 ℃ freeze drying box and carried out pre-freeze 3,4,2 hours; Vacuum in the freeze drying box is risen to below the 13.33Pa (0.1mmHg post), be incubated 5,4,6 hours down, be incubated 4,6,4 hours down at-10 ℃ at-20 ℃; 0 ℃ dry 1,2,2 hour down, 10 ℃ of dryings 2,3,2 hours.
Embodiment 13
The solubility property of the preparation of the present invention that embodiment 10,11 is made is investigated.Preparation A of the present invention, B, C, D all can dissolve after adding water for injection well, and the clarity of gained solution is all qualified.
Embodiment 14-15
A, B, C, D preparation to the present invention's preparation have carried out pharmacology and effect experiment, and the result shows that preparation performance of the present invention is good, easy to use.
Claims (9)
1, a kind of pharmaceutical preparation that contains Flos Lonicerae and Radix Scutellariae, it is got by following method preparation:.
(1) extract Flos Lonicerae:
(a) Flos Lonicerae is extracted 1～3 time with 8～12 times of water (not comprising the water yield that bole self absorbs), and extracting solution concentrates, and adds ethanol precipitation, filters, and removes ethanol in the filtrate; Add entry, or
(b) Flos Lonicerae is extracted 1～3 time with 6～10 times of ethanol (not comprising the amount of alcohol that bole self absorbs), and extracting solution reclaims ethanol, concentrate,
(c),, reclaim ethyl acetate or n-butyl alcohol with ethyl acetate or n-butanol extraction with (a) or (b) step gains, add entry, filter, regulating its pH is 6.0～8.0, promptly get Flos Lonicerae extract, contain crude drug amount 4g/ml～20g/ml, or contain chlorogenic acid 25mg/ml～100mg/ml;
(2) extract Radix Scutellariae: Radix Scutellariae did not decoct with water 1～3 time with 6～10 times (not comprising the water yield that bole self absorbs), filtered, and filtrate concentrates, leave standstill, filter, precipitation is dissolved with 2～4 times of water gagings, transfer gained solution pH value to 6.0～8.0, filter the filtrate ethanol precipitation, filter, transfer filtrate pH value to 1～3, leave standstill, filter, precipitation is used washing with alcohol, and drying gets Radix Scutellariae extract;
(3) make it contain crude drug amount 4g/ml～20g/ml with water dissolution (2) step gains; Merge with (1) step gains, regulating its pH value is 4.5～8.0, and activated carbon decolorizing is removed pyrogen, filters lyophilization.
2, preparation according to claim 1 is characterized in that can treating that with the concentrated hydrochloric acid accent pH of extract is 1.5～2.5 before ethyl acetate or n-butanol extraction in described (1) step.
3, preparation according to claim 1 is characterized in that also comprising the material of one or more in the acceptable adjuvant on the conventional pharmaceutical such as stabilizing agent, analgesics and buffer agent.
4, a kind of pharmaceutical preparation that contains Flos Lonicerae and Radix Scutellariae, it is got by following method preparation:
(1) extract Flos Lonicerae:
(a) Flos Lonicerae is extracted 1～3 time with 8～12 times of water (not comprising the water yield that bole self absorbs), decocted 0.5～1.5 hour, extracting solution is concentrated into and contains crude drug amount 1: 0.8～1: 2,20～50 ℃ add concentration is 60～80% ethanol precipitations, cold preservation is spent the night, and filters, and removes ethanol in the filtrate, add entry to containing crude drug amount 1: 0.8～1: 2.0
(b) Flos Lonicerae is extracted 1～3 time with 6～10 times of ethanol (do not comprise bole self absorb amount of alcohol), decocts 0.5～1.5 hour, and extracting solution recovery ethanol is concentrated into and contains crude drug amount 1: 0.8～1: 2.0,
(c) with (a) or (b) step gains, transferring pH with hydrochloric acid is 1.5～2.5, with 1～2 times of ethyl acetate or n-butanol extraction 4～6 times, and recovery ethyl acetate or n-butyl alcohol, add an amount of water for injection, regulate pH3.0～7.0 for the first time with sodium hydroxide solution, filter, regulate pH value to 6.0～8.0 for the second time with sodium hydroxide solution, cold preservation is spent the night, 0.22 the filtering with microporous membrane of μ m promptly gets Flos Lonicerae extract, contains crude drug amount 4g/ml～20g/ml;
(2) extract Radix Scutellariae:
Radix Scutellariae did not decoct with water 1～3 time with 6～10 times (not comprising the water yield that bole self absorbs), decocted 1～2 hour, filtered, merging filtrate, be concentrated into and contain crude drug 0.2～0.8g/ml, transfer 1.5～2.5,70～90 ℃ of insulations of concentrated solution pH value 0.5-1.5 hour with hydrochloric acid, left standstill 18～28 hours, filter, precipitation transfers gained solution pH value to 6.0～8.0 to filter with 2～4 times of water gaging dissolvings with sodium hydroxide solution, filtrate adds 0.5～1.5 times of ethanol precipitation, filter, transfer filtrate pH value to 1.0～3.0,80 ℃ insulation 0.5 hour with hydrochloric acid, left standstill 24 hours, filter, precipitation is earlier with Diluted Alcohol washing, the dense washing with alcohol of reuse, the precipitation vacuum drying gets Radix Scutellariae extract;
(3) with water dissolution (2) step gains, contain crude drug amount 4g/ml～20g/ml, merge with (1) step gains, regulating its pH value is 4.5～8.0; Activated carbon decolorizing is removed pyrogen, 0.22 μ m filtering with microporous membrane; Treat that with filtering it is-30 ℃～-40 ℃ freeze drying box pre-freeze 2～4 hours that freeze-drying solution is put into temperature, under-10 ℃～-20 ℃ evacuation, sublimation drying 9～12 hours, 0 ℃～10 ℃ dry 3～5 hours again.
5, according to claim 1 or 4 described preparations, it is characterized in that (1) step the (c) step is 5.0 with regulating pH the described first time, after the filtration, adjust pH is 7.0 for the second time; In (2) step, described accent gained solution pH value 7.0, described accent filtrate pH value is 1.5; Regulating pH value in (3) step is 5.0～6.5.
6, a kind of preparation contains the method for the lyophilized formulations of Flos Lonicerae and Radix Scutellariae, comprising:
(1) extract Flos Lonicerae:
(a) Flos Lonicerae is extracted 1～3 time with 8～12 times of water (not comprising the water yield that bole self absorbs), and extracting solution concentrates, and adds ethanol precipitation, filters, and removes ethanol in the filtrate; Add entry, or
(b) Flos Lonicerae is extracted 1～3 time with 6～10 times of ethanol (not comprising the amount of alcohol that bole self absorbs), and extracting solution reclaims ethanol, concentrate,
(c),, reclaim ethyl acetate or n-butyl alcohol with ethyl acetate or n-butanol extraction with (a) or (b) step gains, add entry, filter, regulating its pH is 6.0～8.0, promptly get Flos Lonicerae extract, contain crude drug amount 4g/ml～20g/ml, or contain chlorogenic acid 25mg/ml～100mg/ml;
(2) extract Radix Scutellariae: Radix Scutellariae did not decoct with water 1～3 time with 6～10 times (not comprising the water yield that bole self absorbs), filtered, and filtrate concentrates, leave standstill, filter, precipitation is dissolved with 2～4 times of water gagings, transfer gained solution pH value to 6.0～8.0, filter the filtrate ethanol precipitation, filter, transfer filtrate pH value to 1～3, leave standstill, filter, precipitation is used washing with alcohol, and drying gets Radix Scutellariae extract;
(3) with water dissolution (2) step gains, contain crude drug amount 4g/ml～20g/ml; Merge with (1) step gains, regulating its pH value is 4.5～8.0; Activated carbon decolorizing is removed pyrogen, filters lyophilization.
7, the method for lyophilized formulations according to claim 6 is characterized in that treating that with the concentrated hydrochloric acid accent pH of extract is 1.5～2.5 in described (1) step before ethyl acetate or n-butanol extraction.
8, a kind of preparation contains the method for the medicament freeze-drying preparation of Flos Lonicerae and Radix Scutellariae, may further comprise the steps:
(1) extract Flos Lonicerae:
(d) Flos Lonicerae is extracted 1～3 time with 8～12 times of water (do not comprise bole self absorb the water yield), decocts 0.5～1.5 hour, and extracting solution is concentrated into and contains crude drug amount 1: 0.8～1: 2.0,20～50 ℃ add concentration is 60～80% ethanol precipitations, cold preservation is spent the night, and filters, and removes ethanol in the filtrate; Add entry, to containing crude drug amount 1: 0.8～1: 2.0,
(e) Flos Lonicerae is extracted 1～3 time with 6～10 times of ethanol (do not comprise bole self absorb amount of alcohol), decocts 0.5～1.5 hour, and extracting solution recovery ethanol continues to be concentrated into and contains crude drug amount 1: 0.8～1: 2.0,
(f) with (a) or (b) step gains, transferring pH with hydrochloric acid is 1.5～2.5, with 1～2 times of ethyl acetate or n-butanol extraction 4～6 times, reclaim ethyl acetate or n-butyl alcohol, add an amount of water for injection, regulating pH for the first time with sodium hydroxide solution is 3.0～7.0, filter, regulating pH for the second time with sodium hydroxide solution is 6.0～8.0, and cold preservation is spent the night, promptly get Flos Lonicerae extract, contain crude drug amount 4g/ml～20g/ml;
(2) extract Radix Scutellariae:
Radix Scutellariae did not decoct with water 1～3 time with 6～10 times (not comprising the water yield that bole self absorbs), decocted 1～2 hour, filtered, merging filtrate is concentrated into and contains crude drug 0.2～0.8g/ml, transfers concentrated solution pH value 1.5～2.5 with hydrochloric acid, 70～90 ℃ are incubated 0.5～1.5 hour, left standstill 18～28 hours, and filtered, precipitation is dissolved with 2～4 times of water gagings, transfer gained solution pH value to 6.0～8.0 with sodium hydroxide solution, filter, filtrate adds 0.5～1.5 times of ethanol precipitation, filters, transfer filtrate pH value to 1.0～3.0 with hydrochloric acid, 80 ℃ are incubated 0.5 hour, leave standstill 24 hours, filter, precipitation is washed with Diluted Alcohol earlier, the dense washing with alcohol of reuse, the precipitation vacuum drying gets Radix Scutellariae extract;
(3) with water dissolution (2) step gains, contain crude drug amount 4g/ml～20g/ml; Merge with (1) step gains, regulating its pH value is 4.5～8.0; Add 0.05%～5% in gained solution, preferred 0.1%～2% active carbon stirred 10～30 minutes filtering decarbonization, 0.22 μ m filtering with microporous membrane down at 25 ℃～60 ℃; Treat that with filtering it is-30 ℃～-40 ℃ freeze drying box pre-freeze 2～4 hours that freeze-drying solution is put into temperature, under-10 ℃～-20 ℃ evacuation, sublimation drying 9～12 hours, 0 ℃～10 ℃ dry 3～5 hours again.
9, according to the method for claim 6 or 8 described lyophilized formulations, it is characterized in that (1) step the (c) step is 5.0 with regulating pH the described first time, after the filtration, adjust pH is 7.0 for the second time; In (2) step, described accent gained solution pH value 7.0, described accent filtrate pH value is 1.5; Regulating pH value in (3) step is 5.0～6.5.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104154708A (en) * | 2014-08-25 | 2014-11-19 | 济南康众医药科技开发有限公司 | Drying method of honeysuckles |
| CN104154715A (en) * | 2014-08-25 | 2014-11-19 | 济南康众医药科技开发有限公司 | Freeze-drying method of honeysuckles |
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| CN1062142C (en) * | 1994-12-30 | 2001-02-21 | 山东北方制药厂 | Process for producing particle of honeysuckle flower and scutellaria |
| CN1398626A (en) * | 2002-08-23 | 2003-02-26 | 李大鹏 | Yinhuang powder injection for intravenous injection and its prepn process |
| CN1424084A (en) * | 2002-12-19 | 2003-06-18 | 中国人民解放军第二军医大学 | Honeysuckle flower and coptis root powder injection and its preparing method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104154708A (en) * | 2014-08-25 | 2014-11-19 | 济南康众医药科技开发有限公司 | Drying method of honeysuckles |
| CN104154715A (en) * | 2014-08-25 | 2014-11-19 | 济南康众医药科技开发有限公司 | Freeze-drying method of honeysuckles |
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