CN1296036C - Compound light-yellow sophora root freeze-drying injection and preparation thereof - Google Patents
Compound light-yellow sophora root freeze-drying injection and preparation thereof Download PDFInfo
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- CN1296036C CN1296036C CNB2005100048961A CN200510004896A CN1296036C CN 1296036 C CN1296036 C CN 1296036C CN B2005100048961 A CNB2005100048961 A CN B2005100048961A CN 200510004896 A CN200510004896 A CN 200510004896A CN 1296036 C CN1296036 C CN 1296036C
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Abstract
The present invention discloses a compound kuh-seng freeze-drying injection and a preparation method thereof, which is characterized in that the freeze-drying injection is made of 5 to 7 wt parts of active parts made of kuh seng and white China roots through extraction and purification and 3.4 to 15 wt parts of pharmaceutic adjuvant; the total alkali content of the kuh seng of the active parts is from 50 to 70 %. Pharmacological experiments show that the compound kuh-seng freeze-drying injection has the advantages of good stability, high safety and strong 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 light-yellow sophora root freeze-drying injection and preparation method thereof.
Technical background
FUFANG KUSHEN ZHUSHEYE is made up of Radix Sophorae Flavescentis, Smilax lanceaefolia Roxb. Var.opaca A.DC. two flavor Chinese medicines, and the main chemical compositions of this injection is oxymatrine, matrine, sophocarpine, Radix Sophorae Flavescentis flavone, Rhizoma Smilacis Glabrae saponin etc.Has clearing away heat-damp and promoting diuresis, removing pathogenic heat from blood and toxic substance from the body, the function of removing obstruction for relieving pain.FUFANG KUSHEN ZHUSHEYE has functions such as hemostasis, pain relieving, anticancer diffusion, can also improve hemopoietic function simultaneously, increase the immunity of organisms effect, for the tumor patient rehabilitation provides reliable means, has effectively improved patient's life quality.The history that Western medicine rules all the land has been broken in the development of this medicine aspect potent pain relieving.FUFANG KUSHEN ZHUSHEYE not only to cancerous pain, carcino-matous hemorrhage, to improve patient's life quality effective, the effect that the tumor body is dwindled.Studies have shown that the alkaloid of sophora flavescens ait that FUFANG KUSHEN ZHUSHEYE contains has significant inside and outside antitumor action, its anti-inflammatory and analgesic effect is also very sure.Smilax lanceaefolia Roxb. Var.opaca A.DC. derives from Liliaceae Xiao Chinaroot Greenbier Rhizome platymiscium short column Xiao's Chinaroot Greenbier Rhizome and magnificent Xiao's Chinaroot Greenbier Rhizome, has removing damp-heat, the function of detoxifcation.
FUFANG KUSHEN ZHUSHEYE has the slight stimulation except the part use in clinical practice, the report that also has other untoward reaction to take place, the main adverse reactions symptom has dizziness, constipation, feels sick, allergy etc., anaphylactic type and delayed type two classes are arranged, and also occurs shiver with cold, hyperpyrexia infusion reaction.Symptom such as there is report injection matrine to instil too fastly also can to produce dizziness, feel sick, therefore think that the untoward reaction of FUFANG KUSHEN ZHUSHEYE also mainly is because Radix Sophorae Flavescentis wherein causes, main cause is complicated component, purity not enough and some impurity of existence or the influence of microgranule composition of Chinese medicine extract.Matrine and oxymatrine that the while FUFANG KUSHEN ZHUSHEYE contains are also not really stable, and twenty percent branch takes place to transform mutually in the long term store process, and these have also influenced the quality control and the clinical practice of FUFANG KUSHEN ZHUSHEYE.
Patent (ZL97112532) " FUFANG KUSHEN ZHUSHEYE " discloses a kind of FUFANG KUSHEN ZHUSHEYE and preparation method thereof.
In the data-searching without any the report of compound light-yellow sophora root freeze-drying injection.
Summary of the invention
For these reasons, in order to overcome above-mentioned deficiency, research worker of the present invention is through further investigation, extraction and purification process to the Radix Sophorae Flavescentis Smilax lanceaefolia Roxb. Var.opaca A.DC. improves, by extracting purification, obtain Radix Sophorae Flavescentis, Smilax lanceaefolia Roxb. Var.opaca A.DC. effective site, Radix Sophorae Flavescentis, Smilax lanceaefolia Roxb. Var.opaca A.DC. effective site are mixed with pharmaceutic adjuvant, are prepared into lyophilized injectable powder.
The object of the present invention is to provide a kind of active constituent content height, eutherapeutic compound light-yellow sophora root freeze-drying injection.
The present invention also aims to provide the preparation method of this lyophilized injectable powder.
The present invention is achieved through the following technical solutions.
One. process recipes:
(1) raw material medicines in portions by weight consists of: Radix Sophorae Flavescentis 1-1.2 part, Smilax lanceaefolia Roxb. Var.opaca A.DC. 0.5-0.6 part.
(2) getting Radix Sophorae Flavescentis pulverizes, cross the 20-40 mesh sieve, in the percolator of packing into after the 0.1% hydrochloric acid solution moistening expansion, after adding 0.1% soak with hydrochloric acid 4h, percolator is linked to each other with storng-acid cation exchange resin, carry out percolation, percolate is crossed resin column, exchanger resin is used in the ethanol and adds the ammonia alcohol gradation backflow eluting of ammonia to pH value 9-10, and the ammonia alcohol eluen reclaims ethanol and concentrates, concentrated solution 1.Radix Sophorae Flavescentis medicinal residues and Smilax lanceaefolia Roxb. Var.opaca A.DC. decoct with water secondary, and each 1-3 hour, merge decoction liquor, be concentrated into 1.5g crude drug/ml; Add ethanol and make and contain alcohol amount and reach 65%, leave standstill, filter, decompression recycling ethanol also is concentrated into 2g crude drug/ml, adds ethanol again and makes that to contain the alcohol amount be 90%, and standing over night filters, decompression recycling ethanol, concentrated solution 2.Merge concentrated solution 1 and 2, vacuum drying gets Radix Sophorae Flavescentis, Smilax lanceaefolia Roxb. Var.opaca A.DC. effective site.
(3) the prescription weight portion of preparation of the present invention consists of:
Radix Sophorae Flavescentis, Smilax lanceaefolia Roxb. Var.opaca A.DC. effective site 5-7 part, pharmaceutic adjuvant 3.4-15 part.
(4) getting above-mentioned Radix Sophorae Flavescentis, Smilax lanceaefolia Roxb. Var.opaca A.DC. effective site and pharmaceutic adjuvant mixes, add the dissolving of injection water, activated carbon adsorption filters, and filtrate filters with the ultrafilter membrane of molecular cut off 10000-30000, add the injection water to ormal weight, regulate pH value to 5.5-7.0, filtering with microporous membrane, fill, lyophilization, promptly.
Radix Sophorae Flavescentis of the present invention takes the sour water percolation to extract, cation exchange resin, ammonia alcohol eluting carry out purification, Radix Sophorae Flavescentis medicinal residues and Smilax lanceaefolia Roxb. Var.opaca A.DC. water extract-alcohol precipitation are made with extra care, merge said extracted liquid, drying, obtain Radix Sophorae Flavescentis, Smilax lanceaefolia Roxb. Var.opaca A.DC. effective site, make to adopt the Radix Sophorae Flavescentis of the present invention's preparation, the Radix Sophorae Flavescentis total alkaloids content in the Smilax lanceaefolia Roxb. Var.opaca A.DC. effective site reach 50%-70%, significantly improved effective ingredient purity.Ultrafiltration technology is a kind of new isolation technics, can hold back the macromole impurity of removing in the extracting solution by molecular selectivity, the present invention handles medicinal liquid with the ultrafilter membrane ultrafiltration of molecular cut off 10000-30000, can effectively remove the contained matter of mixing of medicinal liquid, protein, resin, macromole impurity such as starch, also has simultaneously the effect of certain removal pyrogen, because compound light-yellow sophora root freeze-dried powder of the present invention adopts the lyophilization production technology, medicine is at vacuum dehydrating at lower temperature, make medicine be difficult for oxidation, avoided the mutual conversion of matrine and oxymatrine and decomposed because of hyperpyrexia, the manufactured goods water content is low, helps long term store.
Pharmaceutic adjuvant of the present invention is the acceptable compound of pharmaceutics, can be in mannitol or lactose or glucose or dextran or the glucosan one or both.The consumption of described compound is: Radix Sophorae Flavescentis, Smilax lanceaefolia Roxb. Var.opaca A.DC. effective site: the filler weight ratio is 1: 0.5-3.0, preferred 1: 0.5-2.0.Said diluted acid is 0.1% hydrochloric acid or 1% acetic acid.
The lyophilized powder effective ingredient purity height that the present invention makes, has dissolubility, stability preferably, the present invention compares with FUFANG KUSHEN ZHUSHEYE and has reduced the consumption of Radix Sophorae Flavescentis, and the aftermentioned pharmacological evaluation shows that compound light-yellow sophora root freeze-drying injection of the present invention has better pharmacological action.
Two. the check and analysis of effective site
1. the mensuration of Radix Sophorae Flavescentis total alkaloids:
1.1 experiment medicine: Radix Sophorae Flavescentis of the present invention, Smilax lanceaefolia Roxb. Var.opaca A.DC. effective site (Tianzhijiao Medication Development Co., Ltd., Guangdong's laboratory provides, by preparation method preparation of the present invention); FUFANG KUSHEN ZHUSHEYE extract (by the preparation of FUFANG KUSHEN ZHUSHEYE preparation method).
1.2 experimental technique: it is an amount of that precision takes by weighing above sample, the accurate test sample 2ml that draws puts in the small beaker, put in the water-bath heating and be concentrated into about 2.sml, put and be chilled to room temperature, drip ammonia solution and make and be alkaline, quantitatively move in the separatory funnel, gradation adds that atmosphere is imitative 20,20,20,10ml extracts, and carries to the greatest extent to alkaloid. and merge extractive liquid, is put to steam in the water-bath near and is done, and adds the neutral second liquor-saturated (C.I. 13020. indication) of 3ml, evaporate to dryness, the residue 5ml that adds diethyl ether makes dissolving.Precision adds sulphuric acid liquid (0.01mol/L) 10ml, shakes up, and puts in the water-bath heating and residue is dissolved fully and eliminates ether, puts cold.Add 2 of the cold water 15ml that newly boiled and C.I. 13020. indicator solutions, with caustic lye of soda (0.02mol/L) titration to yellow, promptly; The sulphuric acid liquid (0.01mol/L) of every 1ml is equivalent to the matrine (C15H24N20) of 4.967mg, and the result proofreaies and correct with blank assay.The results are shown in Table 1.
Table 1 effective site total alkaloids percentage composition
| Group | FUFANG KUSHEN ZHUSHEYE extract (%) | Radix Sophorae Flavescentis of the present invention, Smilax lanceaefolia Roxb. Var.opaca A.DC. effective site (%) |
| 1 2 3 | 32.6 33.4 32.5 | 53.3 57.2 66.0 |
Conclusion: test us by above-mentioned check and analysis and can learn that the effective ingredient percentage composition obviously improves in the effective site of the present invention, prove absolutely that technology of the present invention increases significantly than former technology.
Three. oxymatrine and content of matrine are measured in the preparation
Instrument and reagent: Waters high liquid chromatography instrument, 2487 UV-detector, Millinium32 chromatographic work station; FUFANG KUSHEN ZHUSHEYE (Shanxi Jin Jing Pharmaceutical Co., Ltd), compound light-yellow sophora root lyophilized powder of the present invention (Tianzhijiao Medication Development Co., Ltd., Guangdong's laboratory provides, by preparation method preparation of the present invention); Oxymatrine reference substance, matrine reference substance are all available from Nat'l Pharmaceutical ﹠ Biological Products Control Institute.
Experimental technique: reference literature method (Zhang Lei etc., ion pair RP-HPLC measures oxymatrine and matrine content in the FUFANG KUSHEN ZHUSHEYE simultaneously. Chinese patent medicine: 26 (11), 2004:876) oxymatrine in the above-mentioned sample and matrine are measured, be the results are shown in Table 2.
Table 2 oxymatrine and content of matrine (mg/ props up)
| Group | The FUFANG KUSHEN ZHUSHEYE extract | Radix Sophorae Flavescentis of the present invention, Smilax lanceaefolia Roxb. Var.opaca A.DC. effective site | ||
| Oxymatrine | Matrine | Oxymatrine | Matrine | |
| 1 2 3 | 19.5 18.6 19.7 | 3.64 3.57 3.65 | 16.9 16.7 16.0 | 3.17 3.14 3.10 |
Lower by oxymatrine and matrine content in the above experimental result preparation of the present invention as can be known than FUFANG KUSHEN ZHUSHEYE, the present invention is owing to reduced the crude drug consumption, thereby effective ingredient reduces, the aftermentioned pharmacological evaluation shows that the present invention has better pharmacological action, simultaneously owing to reduced the consumption of Radix Sophorae Flavescentis, its untoward reaction is reduced, and safety is more secure, illustrates that preparation technology of the present invention is more scientific and reasonable.
Four. pharmacology embodiment
Reagent and animal: compound light-yellow sophora root freeze-drying injection of the present invention (providing by Tianzhijiao Medication Development Co., Ltd., Guangdong's laboratory) by preparation method preparation of the present invention; FUFANG KUSHEN ZHUSHEYE (Shanxi Jin Jing Pharmaceutical Co., Ltd), normal saline is provided by Tianzhijiao Medication Development Co., Ltd., Guangdong's laboratory.Healthy mice, body weight 20 ± 2g, male and female half and half (providing) by the Guangzhou Experimental Animal Center; Tumor strain: mice S
180(Guangzhou Experimental Animal Center).
1. antitumor action
1.1 to mice S
180The tumor growth inhibitory action
Get and inoculate the mice S180 that goes down to posterity, in homogenizer, add normal saline, make mice S180 tumor homogenate, again with normal saline dilution in 1: 3, it is subcutaneous to get oxter, a 0.2ml injection mice left side then, weighed in 24 hours, administration group mice tail every day intravenously administrable once, dosage is FUFANG KUSHEN ZHUSHEYE group 8g crude drug/kg, compound light-yellow sophora root freeze-drying injection group 7.2g crude drug/kg of the present invention, the administration volume only is all 0.2ml/, and matched group gives the equivalent normal saline, totally 7 days.Next day is put to death mice in drug withdrawal, and the subcutaneous tumors piece is peeled off in the also carefulness of weighing, and takes by weighing tumor in the EM50 electronic balance and weighs, and calculate tumour inhibiting rate, sees Table 3.
Table 3 is respectively organized preparation to mice S
180The tumor growth inhibitory action
| Group | Tumor body weight (mg) | Tumour inhibiting rate (%) |
| Normal saline FUFANG KUSHEN ZHUSHEYE compound light-yellow sophora root freeze-drying injection of the present invention | 1.5014 1.0018 0.8281 | 32.3** 44.8** Δ |
Annotate: compare * * P＜0.01 with the normal saline group, compare with FUFANG KUSHEN ZHUSHEYE
ΔP＜0.05＜
The result shows that compound light-yellow sophora root freeze-drying injection of the present invention can significantly suppress tumor growth, has than the better pharmacological action of FUFANG KUSHEN ZHUSHEYE.
1.2 influence to tumor-bearing mice mortality rate and time-to-live
Get and inoculate the mice S180 that goes down to posterity, in homogenizer, add normal saline, make mice S180 tumor homogenate, again with normal saline 1: 3 dilution, getting 0.2ml then, to inject oxter, a mice left side subcutaneous, a week behind inoculated tumour, promptly the 8th day begins by 1.1 method administrations, allow its natural death, treat the whole death of control animals after, mortality rate relatively, and the time-to-live difference of 90 days each treated animals of comparison, if administration group and matched group, 20 of every group of mices the results are shown in Table 4.
Table 4 pair is respectively organized the influence of mouse death rate and time-to-live
| Group | Death toll (%) | Mortality rate (%) | Mean survival time (my god) | Increase in life span (%) |
| Normal saline FUFANG KUSHEN ZHUSHEYE compound light-yellow sophora root freeze-drying injection of the present invention | 20 14 9 | 100 70* 45* Δ | 31.5±1.9 58.6±4.0 66.0±12.4 | 86.0** 109.5** Δ |
Annotate: compare * * P＜0.01 with the normal saline group, compare with FUFANG KUSHEN ZHUSHEYE
ΔP＜0.05
The result shows that compound light-yellow sophora root freeze-drying injection of the present invention can significantly reduce the tumor-bearing mice mortality rate, prolongs the tumor-bearing mice time-to-live, relatively acts on more remarkable with FUFANG KUSHEN ZHUSHEYE.
2. analgesic test
2.1 the mice hot plate is caused the influence of pain effect
Get 30 of body weight 20 ± 2g mices, male and female half and half, be divided into 3 groups at random, every group 10, it is the normal saline group, the FUFANG KUSHEN ZHUSHEYE group, compound light-yellow sophora root freeze-drying injection group of the present invention, dosage is FUFANG KUSHEN ZHUSHEYE group 8g crude drug/kg, compound light-yellow sophora root lyophilized powder 7.2g crude drug/kg of the present invention, the administration volume only is all 0.2ml/ mutually, and the blank group gives the equivalent normal saline, 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 5 to the response time of hot plate pain after the observation administration.
2.2 the influence of the writhing response that Dichlorodiphenyl Acetate causes
Get body weight 20 ± 2g mice, male and female half and half, grouping and medication are with 2.1, 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 5.
Table 5 analgesic test result (X ± SD)
| Group | Pain threshold (s) | |
| The hot plate pain response time (s) | Turn round the body number of times | |
| Normal saline FUFANG KUSHEN ZHUSHEYE compound light-yellow sophora root freeze-drying injection of the present invention | 11.5±4.0 17.3±4.3 * 19.2±3.6 ** | 29.0±5.0 19.0±4.5 * 14.1±2.1 ** |
Annotate: compare with the normal saline group:
*P＜0.05
*P＜0.01
Result of the test shows that compound light-yellow sophora root freeze-drying injection of the present invention has analgesic activity preferably, and wherein the analgesic activity of lyophilized injectable powder of the present invention is more more remarkable than the effect of FUFANG KUSHEN ZHUSHEYE.
3. anastalsis
3.1 influence to the mice bleeding time
Get body weight 20 ± 2g mice, male and female half and half, grouping and medication are with 2.1, successive administration 3 days, 30min cuts off the most advanced and sophisticated 3mm of mouse tail place after the last administration, treats that blood flows out voluntarily to pick up counting, inhale to dehematize with filter paper every 30s and drip 1 time, till blood flow stops (filter paper suction depletion of blood) voluntarily, calculate the bleeding time, the results are shown in Table 6.
The influence in table 6 pair mice bleeding time (X ± SD)
| Group | Bleeding time (s) |
| Normal saline FUFANG KUSHEN ZHUSHEYE compound light-yellow sophora root freeze-drying injection of the present invention | 12.5±3.2 8.1±1.9 * 6.0±1.2 ** |
Annotate: compare with the normal saline group:
*P＜0.05
*P＜0.01
Result of the test shows that compound light-yellow sophora root freeze-drying injection of the present invention has significant anastalsis, and its haemostatic effect is better than the FUFANG KUSHEN ZHUSHEYE group.
4. antiinflammatory action
4.1 influence to mouse ear caused by dimethylbenzene xylene inflammation
Get 30 of body weight 20 ± 2g mices, male and female half and half, grouping and medication be with 1.1, successive administration 3 days, 30min after the last administration, dimethylbenzene 0.02ml is applied to mice left side ear, mice is put to death in dislocation behind the 1h, cuts two ears, and punching is weighed, with left ear and auris dextra sheet weight difference is the swelling degree, the results are shown in Table 7.
Table 7 pair mouse ear caused by dimethylbenzene xylene inflammation influence result (X ± SD)
| Group | Swelling degree difference (mg) |
| Normal saline FUFANG KUSHEN ZHUSHEYE compound light-yellow sophora root freeze-drying injection of the present invention | 7.9±1.5 5.0±1.3 * 3.9±1.0 ** |
Annotate: compare with the normal saline group:
*P＜0.05
*P＜0.01
The result shows that compound light-yellow sophora root freeze-drying injection of the present invention has good antiinflammatory action, and its antiphlogistic effects is better than the FUFANG KUSHEN ZHUSHEYE group.
Sum up: though above The pharmacological results shows lyophilized injectable powder dosage of the present invention than FUFANG KUSHEN ZHUSHEYE still less, pharmacological action significantly is better than FUFANG KUSHEN ZHUSHEYE, illustrates that freeze-dried powder preparation preparation technology of the present invention and method are more scientific and reasonable.
Five. preparation embodiment
Embodiment 1
(1) getting Radix Sophorae Flavescentis 1200g pulverizes, cross 20 mesh sieves, in the percolator of packing into after the 0.1% hydrochloric acid solution moistening expansion, after adding 0.1% soak with hydrochloric acid 4h, percolator is linked to each other with storng-acid cation exchange resin, carry out percolation, percolate is crossed resin column, exchanger resin is used in the ethanol and adds the ammonia alcohol gradation backflow eluting of ammonia to pH value 9-10, and the ammonia alcohol eluen reclaims ethanol and concentrates, concentrated solution 1.Radix Sophorae Flavescentis medicinal residues and Smilax lanceaefolia Roxb. Var.opaca A.DC. 600g decoct with water secondary, and each 1 hour, merge decoction liquor, be concentrated into 1.5g crude drug/ml; Add ethanol and make and contain alcohol amount and reach 65%, leave standstill, filter, decompression recycling ethanol also is concentrated into 2g crude drug/ml, adds ethanol again and makes that to contain the alcohol amount be 90%, leaves standstill, filter, decompression recycling ethanol, concentrated solution 2.Merge concentrated solution 1 and 2, vacuum drying gets Radix Sophorae Flavescentis, Smilax lanceaefolia Roxb. Var.opaca A.DC. effective site 69g.
(2) prescription of preparation of the present invention is:
Radix Sophorae Flavescentis, Smilax lanceaefolia Roxb. Var.opaca A.DC. effective site 69g, mannitol 81g.
(3) getting above-mentioned Radix Sophorae Flavescentis, Smilax lanceaefolia Roxb. Var.opaca A.DC. effective site and mannitol mixes, add the dissolving of injection water, activated carbon adsorption filters, and filtrate filters with the ultrafilter membrane of molecular cut off 10000, add the injection water to ormal weight, regulate pH value to 5.5-7.0, filtering with microporous membrane, fill, lyophilization promptly gets 500 bottles of lyophilized injectable powders of the present invention.
Embodiment 2
(1) getting Radix Sophorae Flavescentis 1200g pulverizes, cross 40 mesh sieves, in the percolator of packing into after the 1% acetum moistening expansion, after adding 1% acetic acid immersion 4h, percolator is linked to each other with storng-acid cation exchange resin, carry out percolation, percolate is crossed resin column, exchanger resin is used in the ethanol and adds the ammonia alcohol gradation backflow eluting of ammonia to pH value 9-10, and the ammonia alcohol eluen reclaims ethanol and concentrates, concentrated solution 1.Radix Sophorae Flavescentis medicinal residues and Smilax lanceaefolia Roxb. Var.opaca A.DC. 600g decoct with water secondary, and each 2 hours, merge decoction liquor, be concentrated into 1.5g crude drug/ml; Add ethanol and make and contain alcohol amount and reach 65%, leave standstill, filter, decompression recycling ethanol also is concentrated into 2g crude drug/ml, adds ethanol again and makes that to contain the alcohol amount be 90%, leaves standstill, filter, decompression recycling ethanol, concentrated solution 2.Merge concentrated solution 1 and 2, vacuum drying gets Radix Sophorae Flavescentis, Smilax lanceaefolia Roxb. Var.opaca A.DC. effective site 70g.
(2) prescription of preparation of the present invention is:
Radix Sophorae Flavescentis, Smilax lanceaefolia Roxb. Var.opaca A.DC. effective site 70g, mannitol 80g.
(3) getting above-mentioned Radix Sophorae Flavescentis, Smilax lanceaefolia Roxb. Var.opaca A.DC. effective site and mannitol mixes, add the dissolving of injection water, activated carbon adsorption filters, and filtrate filters with molecular cut off 30000 ultrafilter membranes, add the injection water to ormal weight, regulate pH value to 5.5-7.0, filtering with microporous membrane, fill, lyophilization promptly gets 500 bottles of lyophilized injectable powders of the present invention.
Embodiment 3
(1) getting Radix Sophorae Flavescentis 1200g pulverizes, cross 30 mesh sieves, in the percolator of packing into after the 0.1% hydrochloric acid solution moistening expansion, after adding 0.1% soak with hydrochloric acid 4h, percolator is linked to each other with storng-acid cation exchange resin, carry out percolation, percolate is crossed resin column, exchanger resin is used in the ethanol and adds the ammonia alcohol gradation backflow eluting of ammonia to pH value 9-10, and the ammonia alcohol eluen reclaims ethanol and concentrates, concentrated solution 1.Radix Sophorae Flavescentis medicinal residues and Smilax lanceaefolia Roxb. Var.opaca A.DC. 600g decoct with water secondary, and each 3 hours, merge decoction liquor, be concentrated into 1.5g crude drug/ml; Add ethanol and make and contain alcohol amount and reach 65%, leave standstill, filter, decompression recycling ethanol also is concentrated into 2g crude drug/ml, adds ethanol again and makes that to contain the alcohol amount be 90%, leaves standstill, filter, decompression recycling ethanol, concentrated solution 2.Merge concentrated solution 1 and 2, vacuum drying gets Radix Sophorae Flavescentis, Smilax lanceaefolia Roxb. Var.opaca A.DC. effective site 67g.
(2) prescription of preparation of the present invention is:
Radix Sophorae Flavescentis, Smilax lanceaefolia Roxb. Var.opaca A.DC. effective site 67g, lactose 133g.
(3) getting above-mentioned Radix Sophorae Flavescentis, Smilax lanceaefolia Roxb. Var.opaca A.DC. effective site and lactose mixes, add the dissolving of injection water, activated carbon adsorption filters, and filtrate filters with molecular cut off 2000 ultrafilter membranes, add the injection water to ormal weight, regulate pH value to 5.5-7.0, filtering with microporous membrane, fill, lyophilization promptly gets 500 bottles of lyophilized injectable powders of the present invention.
Embodiment 4
(1) getting Radix Sophorae Flavescentis 1200g pulverizes, cross 20 mesh sieves, in the percolator of packing into after the 1% acetum moistening expansion, after adding 1% acetic acid immersion 4h, percolator is linked to each other with storng-acid cation exchange resin, carry out percolation, percolate is crossed resin column, exchanger resin is used in the ethanol and adds the ammonia alcohol gradation backflow eluting of ammonia to pH value 9-10, and the ammonia alcohol eluen reclaims ethanol and concentrates, concentrated solution 1.Radix Sophorae Flavescentis medicinal residues and Smilax lanceaefolia Roxb. Var.opaca A.DC. 600g decoct with water secondary, and each 1.5 hours, merge decoction liquor, be concentrated into 1.5g crude drug/ml; Add ethanol and make and contain alcohol amount and reach 65%, leave standstill, filter, decompression recycling ethanol also is concentrated into 2g crude drug/ml, adds ethanol again and makes that to contain the alcohol amount be 90%, leaves standstill, filter, decompression recycling ethanol, concentrated solution 2.Merge concentrated solution 1 and 2, vacuum drying gets Radix Sophorae Flavescentis, Smilax lanceaefolia Roxb. Var.opaca A.DC. effective site 67g.
(2) prescription of preparation of the present invention is:
Radix Sophorae Flavescentis, Smilax lanceaefolia Roxb. Var.opaca A.DC. effective site 67g, glucose 133g.
(3) getting above-mentioned Radix Sophorae Flavescentis, Smilax lanceaefolia Roxb. Var.opaca A.DC. effective site and glucose mixes, add the dissolving of injection water, activated carbon adsorption filters, and filtrate filters with the ultrafilter membrane of molecular cut off 10000, add the injection water to ormal weight, regulate pH value to 5.5-7.0, filtering with microporous membrane, fill, lyophilization promptly gets 500 bottles of lyophilized injectable powders of the present invention.
Embodiment 5
(1) getting Radix Sophorae Flavescentis 1200g pulverizes, cross 30 mesh sieves, in the percolator of packing into after the 0.1% hydrochloric acid solution moistening expansion, after adding 0.1% soak with hydrochloric acid 4h, percolator is linked to each other with storng-acid cation exchange resin, carry out percolation, percolate is crossed resin column, exchanger resin is used in the ethanol and adds the ammonia alcohol gradation backflow eluting of ammonia to pH value 9-10, and the ammonia alcohol eluen reclaims ethanol and concentrates, concentrated solution 1.Radix Sophorae Flavescentis medicinal residues and Smilax lanceaefolia Roxb. Var.opaca A.DC. 600g decoct with water secondary, and each 2.5 hours, merge decoction liquor, be concentrated into 1.5g crude drug/ml; Add ethanol and make and contain alcohol amount and reach 65%, leave standstill, filter, decompression recycling ethanol also is concentrated into 2g crude drug/ml, adds ethanol again and makes that to contain the alcohol amount be 90%, leaves standstill, filter, decompression recycling ethanol, concentrated solution 2.Merge concentrated solution 1 and 2, vacuum drying gets Radix Sophorae Flavescentis Smilax lanceaefolia Roxb. Var.opaca A.DC. effective site 66g.
(2) prescription of preparation of the present invention is:
Radix Sophorae Flavescentis, Smilax lanceaefolia Roxb. Var.opaca A.DC. effective site 66g, dextran 34g.
(3) getting above-mentioned Radix Sophorae Flavescentis, Smilax lanceaefolia Roxb. Var.opaca A.DC. effective site and dextran mixes, add the dissolving of injection water, activated carbon adsorption filters, and filtrate filters with the ultrafilter membrane of molecular cut off 30000, add the injection water to ormal weight, regulate pH value to 5.5-7.0, filtering with microporous membrane, fill, lyophilization promptly gets 500 bottles of lyophilized injectable powders of the present invention.
Embodiment 6
(1) getting Radix Sophorae Flavescentis 1200g pulverizes, cross 30 mesh sieves, in the percolator of packing into after the 0.1% hydrochloric acid solution moistening expansion, after adding 0.1% soak with hydrochloric acid 4h, percolator is linked to each other with storng-acid cation exchange resin, carry out percolation, percolate is crossed resin column, exchanger resin is used in the ethanol and adds the ammonia alcohol gradation backflow eluting of ammonia to pH value 9-10, and the ammonia alcohol eluen reclaims ethanol and concentrates, concentrated solution 1.Radix Sophorae Flavescentis medicinal residues and Smilax lanceaefolia Roxb. Var.opaca A.DC. 600g decoct with water secondary, and each 1 hour, merge decoction liquor, be concentrated into 1.5g crude drug/ml; Add ethanol and make and contain alcohol amount and reach 65%, leave standstill, filter, decompression recycling ethanol also is concentrated into 2g crude drug/ml, adds ethanol again and makes that to contain the alcohol amount be 90%, leaves standstill, filter, decompression recycling ethanol, concentrated solution 2.Merge concentrated solution 1 and 2, vacuum drying gets Radix Sophorae Flavescentis, Smilax lanceaefolia Roxb. Var.opaca A.DC. effective site 66g.
(2) prescription of preparation of the present invention is:
Radix Sophorae Flavescentis, Smilax lanceaefolia Roxb. Var.opaca A.DC. effective site 66g, Dextran 8 4g.
(3) getting above-mentioned Radix Sophorae Flavescentis, Smilax lanceaefolia Roxb. Var.opaca A.DC. effective site and glucosan mixes, add the dissolving of injection water, activated carbon adsorption filters, and filtrate filters with the ultrafilter membrane of molecular cut off 30000, add the injection water to ormal weight, regulate pH value to 5.5-7.0, filtering with microporous membrane, fill, lyophilization promptly gets 500 bottles of lyophilized injectable powders of the present invention.
Embodiment 7
(1) getting Radix Sophorae Flavescentis 1000g pulverizes, cross 30 mesh sieves, in the percolator of packing into after the 1% acetum moistening expansion, after adding 1% acetic acid immersion 4h, percolator is linked to each other with storng-acid cation exchange resin, carry out percolation, percolate is crossed resin column, exchanger resin is used in the ethanol and adds the ammonia alcohol gradation backflow eluting of ammonia to pH value 9-10, and the ammonia alcohol eluen reclaims ethanol and concentrates, concentrated solution 1.Radix Sophorae Flavescentis medicinal residues and Smilax lanceaefolia Roxb. Var.opaca A.DC. 500g decoct with water secondary, and each 1 hour, merge decoction liquor, be concentrated into 1.5g crude drug/ml; Add ethanol and make and contain alcohol amount and reach 65%, leave standstill, filter, decompression recycling ethanol also is concentrated into 2g crude drug/ml, adds ethanol again and makes that to contain the alcohol amount be 90%, leaves standstill, filter, decompression recycling ethanol, concentrated solution 2.Merge concentrated solution 1 and 2, vacuum drying gets Radix Sophorae Flavescentis, Smilax lanceaefolia Roxb. Var.opaca A.DC. effective site 50g.
(2) prescription of preparation of the present invention is:
Radix Sophorae Flavescentis, Smilax lanceaefolia Roxb. Var.opaca A.DC. effective site 50g, mannitol 80g, macrodex g.
(3) get above-mentioned Radix Sophorae Flavescentis, Smilax lanceaefolia Roxb. Var.opaca A.DC. effective site and mannitol, glucosan mixing, add the dissolving of injection water, activated carbon adsorption filters, and filtrate filters with the ultrafilter membrane of molecular cut off 20000, add the injection water to ormal weight, regulate pH value to 5.5-7.0, filtering with microporous membrane, fill, lyophilization promptly gets 500 bottles of lyophilized injectable powders of the present invention.
Claims (4)
1. compound light-yellow sophora root freeze-drying injection, it is characterized in that it is to be prepared from by Radix Sophorae Flavescentis, Smilax lanceaefolia Roxb. Var.opaca A.DC. effective site 5-7 weight portion and pharmaceutic adjuvant 3.4-15 weight portion, wherein Radix Sophorae Flavescentis total alkaloids content is 50%-70% in Radix Sophorae Flavescentis, the Smilax lanceaefolia Roxb. Var.opaca A.DC. effective site, and its feature is that also its preparation method is:
(1) crude drug consists of: Radix Sophorae Flavescentis 1-1.2 part, Smilax lanceaefolia Roxb. Var.opaca A.DC. 0.5-0.6 part;
(2) getting Radix Sophorae Flavescentis pulverizes, cross the 20-40 mesh sieve, in the percolator of packing into after the 0.1% hydrochloric acid solution moistening expansion, after adding 0.1% soak with hydrochloric acid 4h, percolator is linked to each other with storng-acid cation exchange resin, carry out percolation, percolate is crossed resin column, exchanger resin is used in and adds the ammonia alcohol gradation backflow eluting of ammonia to pH value 9-10 in the ethanol, and ammonia alcohol eluen decompression recycling ethanol also concentrates, and gets concentrated solution 1; Radix Sophorae Flavescentis medicinal residues and Smilax lanceaefolia Roxb. Var.opaca A.DC. decoct with water secondary, each 1-3 hour, merge decoction liquor, be concentrated into 1.5g crude drug/ml, add ethanol and make and contain alcohol amount and reach 65%, leave standstill, filter, decompression recycling ethanol also is concentrated into 2g crude drug/ml, add ethanol again and make that to contain alcohol amount be 90%, leave standstill, filter, decompression recycling ethanol gets concentrated solution 2; Merge concentrated solution 1 and 2, vacuum drying gets Radix Sophorae Flavescentis, Smilax lanceaefolia Roxb. Var.opaca A.DC. effective site;
(3) getting above-mentioned Radix Sophorae Flavescentis, Smilax lanceaefolia Roxb. Var.opaca A.DC. effective site and pharmaceutic adjuvant mixes, add the dissolving of injection water, activated carbon adsorption filters, filtrate filters with ultrafilter membrane, add the injection water to ormal weight, regulate pH value to 5.5-7.0, filtering with microporous membrane, fill, lyophilization, that is, wherein pharmaceutic adjuvant is one or both in mannitol, lactose, the glucosan.
2. according to the compound light-yellow sophora root freeze-drying injection of claim 1, it is characterized in that Radix Sophorae Flavescentis, Smilax lanceaefolia Roxb. Var.opaca A.DC. effective site: the weight ratio of pharmaceutic adjuvant is 1: 0.5-3.0.
3. according to the compound light-yellow sophora root freeze-drying injection of claim 1, it is characterized in that Radix Sophorae Flavescentis, Smilax lanceaefolia Roxb. Var.opaca A.DC. effective site: the weight ratio of pharmaceutic adjuvant is 1: 0.5-2.0.
4. according to the compound light-yellow sophora root freeze-drying injection of claim 1, the molecular cut off that it is characterized in that used ultrafilter membrane is 10000-30000.
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| CNB2005100048961A CN1296036C (en) | 2005-02-04 | 2005-02-04 | Compound light-yellow sophora root freeze-drying injection and preparation thereof |
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| CN114832058B (en) * | 2022-04-18 | 2023-06-16 | 北京振东光明药物研究院有限公司 | Compound kuh-seng gel and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1062181C (en) * | 1997-07-16 | 2001-02-21 | 山西金晶药业有限公司 | Compound sophora flavescens injection |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1062181C (en) * | 1997-07-16 | 2001-02-21 | 山西金晶药业有限公司 | Compound sophora flavescens injection |
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