CN1296089C - Zedoary injection preparation and its preparing method - Google Patents
Zedoary injection preparation and its preparing method Download PDFInfo
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- CN1296089C CN1296089C CNB2004100711796A CN200410071179A CN1296089C CN 1296089 C CN1296089 C CN 1296089C CN B2004100711796 A CNB2004100711796 A CN B2004100711796A CN 200410071179 A CN200410071179 A CN 200410071179A CN 1296089 C CN1296089 C CN 1296089C
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- rhizoma curcumae
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- 238000002347 injection Methods 0.000 title claims abstract description 41
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- 235000003405 Curcuma zedoaria Nutrition 0.000 title claims abstract description 13
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Abstract
The present invention discloses a zedoary injection preparation and a preparing method thereof. The present invention is characterized in that a low-temperature saturation method is used for the inclusion of the effective sites of zedoary by 2-hydroxypropyl beta-cyclodextrin so that the inclusion ratio of the effective sites of the zedoary reaches more than 90%, and the encapsulation ratio reaches more than 80%; pharmaceutic auxiliary materials are added to an obtained inclusion compound of the effective sites of the zedoary so as to prepare a water needle preparation, a transfusion preparation, a powder needle preparation and a freeze dried powder needle preparation. The results of pharmacological experiments indicate that the zedoray injection preparation of the present invention has preferable pharmacological action.
Description
Affiliated technical field
The invention belongs to technical field of traditional Chinese medicine pharmacy, be specifically related to a kind of Zedoary injection preparation and preparation method thereof.
Background technology
(be called for short HP-β-CD) is the hydroxyalkylation derivant of a class beta-schardinger dextrin-to the 2-HP-.Beta-schardinger dextrin-(has the hydrogen atom of 3 hydroxyls among C-2, C-3 and the C-6 (CHCHOHCH) to be replaced by hydroxypropyl in each glucose residue of β-CD), replace the back and generate 2-HP-β-CD, 3-HP-β-CD, 2,3-DHP-β-CD, 2,6-DHP-β-CD, 2,3, homologues such as 6-THP-β-CD.If controlled condition also can generate the product based on 2-HP-β-CD.2-HP-β-CD be research at present at most, work do the safety aspect data of fullest, collection the most comprehensive, to medicament solubilization with improve the best CD derivant of stabilizing effect.A lot of character of 2-HP-β-CD change, and mainly show as the following aspects: (1) 2-HP-β-CD is the amorphism powder, and β-CD solid is a crystalline powder; (2) dissolution properties changes, and the dissolubility of 2-HP-β-CD in water be greater than 50%, and dissolves in alcoholic solution, and β-CD water solublity is poor, and (25 ℃) dissolubility in water has only 1.85% under the room temperature, and is crystallizable in alcoholic solution; (3) 2-HP-β-CD nephrotoxicity is low, can be used for the parenterai administration approach, and β-CD parenterai administration has nephrotoxicity, so can only be oral and can not be used for the prescription of parenterai administration; (4) 2-HP-β-CD is not by gastric acid and α-Dian Fenmeishuixie, participate in the organism intracellular metabolite hardly, do not accumulate yet, basically all excrete with stool after oral with complete morphology, parenterai administration discharges (5) β-CD with complete morphology with urine basically and medicine formation complex has slow releasing function to medicine, and 2-HP-β-CD and medicine form complex and medicine is had shortly release effect, and medicine is discharged rapidly in vivo; (6) β-CD has haemolysis, and parenterai administration also has certain zest, and 2-HP-β-CD surface activity is low, does not have hemolytic and zest basically.
Cyclodextrin is to investigate the fabricating technology parameter to the bag of medicine and rate and inclusion rate, inclusion rate is defined as inclusion rate=(weight of clathrate/(weight of the weight of 2-HP-β-CD+adding medicine)) * 100%), the inclusion rate is defined as inclusion rate=(drug weight of the weight/adding of the medicine of the recovery * blank response rate) * 100%.At present, β-CD has only about 60% the bag and the rate of liposoluble class medicine, because liposoluble class medicine is in Chinese medicine extraction difficulty especially, bag and rate are low can to make the fat-soluble medicine of the highly difficult extraction of a large amount of processes be not fully utilized, to natural resources of Chinese medicinal materials is huge waste, reduces the pharmacological effect of Chinese medicine preparation; The inclusion rate is also not being well solved in the preparation technical process at present, and is lower by the fat-soluble medicine release of β-CDBao He, causes the concentration of fat-soluble medicine low, and pharmacological action can not be given full play to.
Rhizoma Curcumae is a zingiberaceous plant Rhizoma Curcumae Curcuma aerugionosa Roxb. rhizome, have circulation of qi promoting removing blood stasis, the effect of removing food stagnancy analgesic, modern pharmacological research shows, extract the effective site obtain and has anticancer, antiviral, pain relieving, effect such as antipruritic from Rhizoma Curcumae, injection, suppository, the ointment made with Rhizoma Curcumae effective site have been widely used in clinical; The effective site of Rhizoma Curcumae is liposoluble constituent, is insoluble in water, the Zedoary injection preparation of listing, main some surfactant hydrotropies that adopt, as tween etc., but these cosolvents have hemolytic side effect, in clinical practice, have very big restriction, also there is potential danger in the patient; Number of patent application is 02109680 patent, adopt paddling process or polishing or sonic oscillation method, with HP-Rhizoma Curcumae effective site is carried out enclose, mention inclusion rate in the patent under identical enclose condition, it is the difference of the consumption of HP-, the inclusion rate that makes crosses 95% from 62%, and its credibility is worth suspecting, and this patent is not done any experiment and elaboration to the inclusion rate of HP-.
Summary of the invention
For these reasons, the present invention adopts the low temperature saturation to the fat-soluble effective site of the Rhizoma Curcumae of extraction purification, carry out enclose with 2-HP-β-CD, make the inclusion rate of Rhizoma Curcumae effective site reach more than 90%, the inclusion rate reaches more than 80%, the Rhizoma Curcumae effective site clathrate that obtains mixes with pharmaceutic adjuvant, be prepared into hydro-acupuncture preparation, infusion preparation injectable powder, lyophilized injectable powder, The pharmacological results shows that Zedoary injection preparation of the present invention has better pharmacological action.The present invention is achieved through the following technical solutions.
One. process recipes
(1) get Rhizoma Curcumae, pulverize, put into volatile oil extractor, it is complete to extract volatile oil, and volatile oil is standby; Residue behind the extraction volatile oil is measured 80% ethanol extractions twice with 6 times, 2 hours for the first time, the 2nd time 1 hour, filter merge extractive liquid,, decompression filtrate recycling ethanol, and to be concentrated into relative density be extractum about 1.10-1.20 (50 ℃), and extractum merges ethyl acetate extraction liquid with equivalent ethyl acetate extraction 6 times, the reclaim under reduced pressure ethyl acetate is to most, and concentrate drying is standby;
(2) get Rhizoma Curcumae volatile oil and ethanol extraction, it is complete to add dissolve with ethanol, simultaneously according to Rhizoma Curcumae volatile oil and ethanol extraction: the ratio of 2-hydroxypropyl=1: 20-60, the 2-hydroxypropyl is made saturated solution with distilled water, put into 30 ℃-40 ℃ water-bath, temperature is controlled in strictness well, by the time 2-hydroxypropyl saturated aqueous solution reaches bath temperature, stir, slowly drip and dissolve Rhizoma Curcumae volatile oil and ethanol extraction completely, continue to stir 12-24 hour, placed 12-24 hour at refrigerator, 30 ℃ of-40 ℃ of dryings obtain Rhizoma Curcumae effective site clathrate;
(3) Rhizoma Curcumae effective site is mixed with pharmaceutic adjuvant, be prepared into hydro-acupuncture preparation or infusion preparation or injectable powder or lyophilized injectable powder.
Two. check and analysis
The content of gas chromatography determination curcumenol
Experimental apparatus: day island proper Tianjin GC-9A type gas chromatograph; The C-R3A microprocessor.
Experimental drug: curcumenol reference substance (Nat'l Pharmaceutical ﹠ Biological Products Control Institute provides)
Oleum Curcumae injection (Qingan County, Heilungkiang Pharmacy stock Co., Ltd provides)
According to number of patent application is the Rhizoma Curcumae injection (Qianluchun Science and Technology Co., Ltd., Beijing's laboratory provides) that 02109680 patent is prepared
Zedoary injection preparation of the present invention (Qianluchun Science and Technology Co., Ltd., Beijing's laboratory provides)
Chromatographic condition: 3.2mm*2m glass packed column; Carrier chromosorb WAW60-80 order; Fixative OV-17;
Detector: FID; 155 ℃ of column temperatures; Injection port and detected temperatures: 220 ℃; N
2Be carrier gas 50ml/min, Air500ml/min;
Experimental technique: it is an amount of that precision takes by weighing reference substance, add dehydrated alcohol and be mixed with 5mg/ml, precision is measured reference substance solution 1.25,2.5,5.0,10.0,20.0ml places the 50ml volumetric flask respectively, be diluted to scale with dehydrated alcohol, shake up every kind of concentration sample introduction 2 microlitres, continuous sample introduction 3 times, obtaining regression equation is Y=994.2+5314.8X, r=0.996.
Sample is complete with ethanol extraction, and precision is measured 2ml and is put the 50ml volumetric flask,, shake up to scale with ethanol dilution, and every kind of concentration sample introduction 2 microlitres, continuous sample introduction 3 times calculates, and obtains the results are shown in Table 1:
Table 1 is respectively organized preparation curcumenol content relatively
| Group | The each consumption of curcumenol content mg/ |
| Commercially available Oleum Curcumae injection number of patent application is 02109680 Rhizoma Curcumae injection curcuma zedoary liquid drugs injection of the present invention curcuma zedoary infusion solution of the present invention curcuma zedoary powder-injection of the present invention curcuma zedoary freeze drying powder injection of the present invention | 7.412 9.501 14.793 14.801 14.797 14.795 |
Conclusion: by above-mentioned analyzing and testing experiment, active constituent content of the present invention all increases, and proves absolutely that technology of the present invention has practical significance.
Three. the mensuration of bag and rate and inclusion rate:
The experiment medicine: technology of the present invention is carried out the clathrate (Qianluchun Science and Technology Co., Ltd., Beijing's laboratory provides) of the Rhizoma Curcumae effective site of enclose
According to number of patent application is the Rhizoma Curcumae clathrate (Qianluchun Science and Technology Co., Ltd., Beijing's laboratory provides) that 02109680 patent is prepared
Experimental technique: get clathrate and put in the round-bottomed flask, add distilled water 150ml and a little zeolite distillation 4h, extract volatile oil, measure the volatile oil volume behind the 30min to be cooled with volatile oil determination apparatus, carry out three experiments (annotate: after measured, 1ml mixed volatilization oil weighs 0.9218g)
The blank response rate of inclusion rate=(the volatile oil volume * blank response rate of the volatile oil volume/adding of recovery) * 100%[(1) respectively is 91.2% (2) to be 91.0%]
Inclusion rate=(weight of clathrate/(weight of the weight of cyclodextrin+adding volatile oil)) * 100%.Calculate according to formula, see Table 2
The comparison of table 2 clathrate bag and rate and inclusion rate
| Medicine | Fat-soluble medicine or volatilization oil mass (V/ml) | Cyclodextrin consumption (mg) | Clathrate amount (mg) | Bag and rate (%) | Reclaim volatilization oil mass (V/ml) | Inclusion rate (%) |
| Clathrate number of patent application of the present invention is 02109680 clathrate | 1.000 1.000 | 30.055 30.008 | 28.499 27.332 | 92.0 88.4 | 0.8265 0.7746 | 82.7 77.5 |
Conclusion: the inclusion rate and the inclusion rate of the clathrate by above-mentioned experiment prepared of the present invention all are significantly improved, and prove absolutely that technology of the present invention has practical significance.
Four. pharmacology embodiment
Embodiment 1
To mice S
180The tumor growth inhibitory action
Laboratory animal: healthy mice, body weight 16-20g, male and female half and half.(Beijing University of Chinese Medicine provides) tumor strain: mice S
180(Beijing University of Chinese Medicine provides)
Experiment medicine: normal saline (Qianluchun Science and Technology Co., Ltd., Beijing's laboratory provides)
Oleum Curcumae injection (Qingan County, Heilungkiang Pharmacy stock Co., Ltd provides)
According to number of patent application is the Rhizoma Curcumae injection (Qianluchun Science and Technology Co., Ltd., Beijing's laboratory provides) that 02109680 patent is prepared
Zedoary injection preparation of the present invention (Qianluchun Science and Technology Co., Ltd., Beijing's laboratory provides)
Experimental technique: get and inoculate the mice S that goes down to posterity
180, in homogenizer, add normal saline, make mice S
180The tumor homogenate, again with normal saline 1: 3 dilution, getting 0.2ml then, to inject oxter, a mice left side subcutaneous, weighed in 24 hours, mice tail every day intravenously administrable once, administration volume identical (0.5ml/ is only), 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 % |
| The commercially available Oleum Curcumae injection of physiological saline is the Rhizoma Curcumae injection liquid drugs injection of the present invention infusion solution of the present invention powder-injection of the present invention freeze drying powder injection of the present invention that 02109680 patent is prepared according to number of patent application | 1.4965 1.0289 0.9765 0.8893 0.8796 0.8826 0.8791 | 100 31.2** 33.7** 40.6**# 41.2**# 41.0**# 41.3**# |
Annotate: compare * * P＜0.01 with the normal saline group, compare #P＜0.05 with positive controls
Embodiment 2
Adopt half intracorporal method to do the antivirus action test
Experiment medicine: normal saline (Qianluchun Science and Technology Co., Ltd., Beijing's laboratory provides)
Oleum Curcumae injection (Qingan County, Heilungkiang Pharmacy stock Co., Ltd provides)
According to number of patent application is the Rhizoma Curcumae injection (Qianluchun Science and Technology Co., Ltd., Beijing's laboratory provides) that 02109680 patent is prepared
Zedoary injection preparation of the present invention (Qianluchun Science and Technology Co., Ltd., Beijing's laboratory provides)
Experimental technique: half intracorporal method is adopted in experiment, normal control group and virus control group, the medicine of variable concentrations is directly acted on virus respectively, be inoculated in immediately in the chick embryo allantoic cavity,, put 37 ℃ of incubators and cultivate 48h with paraffin sealing-in kind hole, collect the urine of every embryo, with the test of 0.5% chicken erythrocyte agglutination, judge the antiviral activity of medicine, the results are shown in Table 4.Influence to Influenza B virus: inoculation method, drug dose are tested with influenza A virus.The results are shown in following table 4.
The effect of table 4 pair influenza virus relatively
| Group | Influenza A virus | Influenza B virus |
| The commercially available Oleum Curcumae injection of physiological saline is the Rhizoma Curcumae injection liquid drugs injection of the present invention infusion solution of the present invention powder-injection of the present invention freeze drying powder injection of the present invention that 02109680 patent is prepared according to number of patent application | +++ + - - - - - | +++ ++ + - - - - |
Annotate :-represent virus-free growth ,+represent a small amount of viral growth, ++ represent more viral growth, ++ a large amount of viral growth conclusions of+representative: show that by pharmacological evaluation the preparation of respectively organizing of the present invention has better pharmacological action.
Five. preparation embodiment
Embodiment 1
(1) get Rhizoma Curcumae, pulverize, put into volatile oil extractor, it is complete to extract volatile oil, and volatile oil is standby; Residue behind the extraction volatile oil is measured 80% ethanol extractions twice with 6 times, 2 hours for the first time, the 2nd time 1 hour, filter merge extractive liquid,, decompression filtrate recycling ethanol, and to be concentrated into relative density be extractum about 1.10 (50 ℃), and extractum merges ethyl acetate extraction liquid with equivalent ethyl acetate extraction 6 times, the reclaim under reduced pressure ethyl acetate is to most, and concentrate drying is standby;
(2) get Rhizoma Curcumae volatile oil and ethanol extraction, it is complete to add dissolve with ethanol, simultaneously according to Rhizoma Curcumae volatile oil and ethanol extraction: the ratio of 2-hydroxypropyl=1: 20, the 2-hydroxypropyl is made saturated solution with distilled water, put into 30 ℃ water-bath, temperature is controlled in strictness well, by the time 2-hydroxypropyl saturated aqueous solution reaches bath temperature, stir, slowly drip and dissolve Rhizoma Curcumae volatile oil and ethanol extraction completely, continue to stir 12 hours, placed 12 hours at refrigerator, 30 ℃ of dryings obtain Rhizoma Curcumae effective site clathrate; (inclusion rate of Rhizoma Curcumae effective site clathrate is 92.1% after testing, and the inclusion rate is 82.7%)
(3) preparation prescription is:
Aqueous injection prescription: Rhizoma Curcumae effective site clathrate 50 grams, sodium chloride 150 grams;
Infusion solution prescription: Rhizoma Curcumae effective site clathrate 200 grams, sodium chloride 600 grams;
Injectable powder prescription: Rhizoma Curcumae effective site clathrate 50 grams, mannitol 150 grams;
Lyophilized injectable powder prescription: Rhizoma Curcumae effective site clathrate 50 grams, mannitol 150 grams;
(4) Rhizoma Curcumae effective site is mixed with pharmaceutic adjuvant, be prepared into 1000 bottles of 1000 bottles of 1000 bottles of 1000 bottles of hydro-acupuncture preparations or infusion preparations or injectable powder or lyophilized injectable powders.(effective ingredient curcumenol content is 10.0mg in the each dosage of above-mentioned after testing ejection preparation)
Embodiment 2
(1) get Rhizoma Curcumae, pulverize, put into volatile oil extractor, it is complete to extract volatile oil, and volatile oil is standby; Residue behind the extraction volatile oil is measured 80% ethanol extractions twice with 6 times, 2 hours for the first time, the 2nd time 1 hour, filter merge extractive liquid,, decompression filtrate recycling ethanol, and to be concentrated into relative density be extractum about 1.20 (50 ℃), and extractum merges ethyl acetate extraction liquid with equivalent ethyl acetate extraction 6 times, the reclaim under reduced pressure ethyl acetate is to most, and concentrate drying is standby;
(2) get Rhizoma Curcumae volatile oil and ethanol extraction, it is complete to add dissolve with ethanol, simultaneously according to Rhizoma Curcumae volatile oil and ethanol extraction: the ratio of 2-hydroxypropyl=1: 60, the 2-hydroxypropyl is made saturated solution with distilled water, put into 40 ℃ water-bath, temperature is controlled in strictness well, by the time 2-hydroxypropyl saturated aqueous solution reaches bath temperature, stir, slowly drip and dissolve Rhizoma Curcumae volatile oil and ethanol extraction completely, continue to stir 24 hours, placed 24 hours at refrigerator, 40 ℃ of dryings obtain Rhizoma Curcumae effective site clathrate; (inclusion rate of Rhizoma Curcumae effective site clathrate is 92.6% after testing, and the inclusion rate is 82.9%)
(3) preparation prescription is:
Aqueous injection prescription: Rhizoma Curcumae effective site clathrate 50 grams, glucose 150 grams;
Infusion solution prescription: Rhizoma Curcumae effective site clathrate 200 grams, sodium chloride 600 grams;
Injectable powder prescription: Rhizoma Curcumae effective site clathrate 50 grams, sucrose 150 grams;
Lyophilized injectable powder prescription: Rhizoma Curcumae effective site clathrate 50 grams, sucrose 150 grams;
(4) Rhizoma Curcumae effective site is mixed with pharmaceutic adjuvant, be prepared into 1000 bottles of 1000 bottles of 1000 bottles of 1000 bottles of hydro-acupuncture preparations or infusion preparations or injectable powder or lyophilized injectable powders.(effective ingredient curcumenol content is 15.0mg in the each dosage of above-mentioned after testing ejection preparation)
Embodiment 3
(1) get Rhizoma Curcumae, pulverize, put into volatile oil extractor, it is complete to extract volatile oil, and volatile oil is standby; Residue behind the extraction volatile oil is measured 80% ethanol extractions twice with 6 times, 2 hours for the first time, the 2nd time 1 hour, filter merge extractive liquid,, decompression filtrate recycling ethanol, and to be concentrated into relative density be extractum about 1.15 (50 ℃), and extractum merges ethyl acetate extraction liquid with equivalent ethyl acetate extraction 6 times, the reclaim under reduced pressure ethyl acetate is to most, and concentrate drying is standby;
(2) get Rhizoma Curcumae volatile oil and ethanol extraction, it is complete to add dissolve with ethanol, simultaneously according to Rhizoma Curcumae volatile oil and ethanol extraction: the ratio of 2-hydroxypropyl=1: 30, the 2-hydroxypropyl is made saturated solution with distilled water, put into 32 ℃ water-bath, temperature is controlled in strictness well, by the time 2-hydroxypropyl saturated aqueous solution reaches bath temperature, stir, slowly drip and dissolve Rhizoma Curcumae volatile oil and ethanol extraction completely, continue to stir 14 hours, placed 16 hours at refrigerator, 32 ℃ of dryings obtain Rhizoma Curcumae effective site clathrate; (inclusion rate of Rhizoma Curcumae effective site clathrate is 93.2% after testing, and the inclusion rate is 83.5%)
(3) preparation prescription is:
Aqueous injection prescription: Rhizoma Curcumae effective site clathrate 50 grams, glucose 150 grams;
Infusion solution prescription: Rhizoma Curcumae effective site clathrate 200 grams, sodium chloride 600 grams;
Injectable powder prescription: Rhizoma Curcumae effective site clathrate 50 grams, lactose 150 grams;
Lyophilized injectable powder prescription: Rhizoma Curcumae effective site clathrate 50 grams, lactose 150 grams;
(4) Rhizoma Curcumae effective site is mixed with pharmaceutic adjuvant, be prepared into 1000 bottles of 1000 bottles of 1000 bottles of 1000 bottles of hydro-acupuncture preparations or infusion preparations or injectable powder or lyophilized injectable powders.(effective ingredient curcumenol content is 11.3mg in the each dosage of above-mentioned after testing ejection preparation)
Embodiment 4
(1) get Rhizoma Curcumae, pulverize, put into volatile oil extractor, it is complete to extract volatile oil, and volatile oil is standby; Residue behind the extraction volatile oil is measured 80% ethanol extractions twice with 6 times, 2 hours for the first time, the 2nd time 1 hour, filter merge extractive liquid,, decompression filtrate recycling ethanol, and to be concentrated into relative density be extractum about 1.14 (50 ℃), and extractum merges ethyl acetate extraction liquid with equivalent ethyl acetate extraction 6 times, the reclaim under reduced pressure ethyl acetate is to most, and concentrate drying is standby;
(2) get Rhizoma Curcumae volatile oil and ethanol extraction, it is complete to add dissolve with ethanol, simultaneously according to Rhizoma Curcumae volatile oil and ethanol extraction: the ratio of 2-hydroxypropyl=1: 40, the 2-hydroxypropyl is made saturated solution with distilled water, put into 35 ℃ water-bath, temperature is controlled in strictness well, by the time 2-hydroxypropyl saturated aqueous solution reaches bath temperature, stir, slowly drip and dissolve Rhizoma Curcumae volatile oil and ethanol extraction completely, continue to stir 15 hours, placed 15 hours at refrigerator, 35 ℃ of dryings obtain Rhizoma Curcumae effective site clathrate; (inclusion rate of Rhizoma Curcumae effective site clathrate is 91.8% after testing, and the inclusion rate is 82.0%)
(3) preparation prescription is:
Aqueous injection prescription: Rhizoma Curcumae effective site clathrate 50 grams, sodium chloride 150 grams;
Infusion solution prescription: Rhizoma Curcumae effective site clathrate 200 grams, sodium chloride 600 grams;
The injectable powder prescription: Rhizoma Curcumae effective site clathrate 50 grams, mannitol, sucrose is totally 150 grams;
The lyophilized injectable powder prescription: Rhizoma Curcumae effective site clathrate 50 grams, mannitol, lactose be totally 150 grams;
(4) Rhizoma Curcumae effective site is mixed with pharmaceutic adjuvant, be prepared into 1000 bottles of 1000 bottles of 1000 bottles of 1000 bottles of hydro-acupuncture preparations or infusion preparations or injectable powder or lyophilized injectable powders.(effective ingredient curcumenol content is 13.2mg in the each dosage of above-mentioned after testing ejection preparation)
Embodiment 5
(1) get Rhizoma Curcumae, pulverize, put into volatile oil extractor, it is complete to extract volatile oil, and volatile oil is standby; Residue behind the extraction volatile oil is measured 80% ethanol extractions twice with 6 times, 2 hours for the first time, the 2nd time 1 hour, filter merge extractive liquid,, decompression filtrate recycling ethanol, and to be concentrated into relative density be extractum about 1.15 (50 ℃), and extractum merges ethyl acetate extraction liquid with equivalent ethyl acetate extraction 6 times, the reclaim under reduced pressure ethyl acetate is to most, and concentrate drying is standby;
(2) get Rhizoma Curcumae volatile oil and ethanol extraction, it is complete to add dissolve with ethanol, simultaneously according to Rhizoma Curcumae volatile oil and ethanol extraction: the ratio of 2-hydroxypropyl=1: 45, the 2-hydroxypropyl is made saturated solution with distilled water, put into 36 ℃ water-bath, temperature is controlled in strictness well, by the time 2-hydroxypropyl saturated aqueous solution reaches bath temperature, stir, slowly drip and dissolve Rhizoma Curcumae volatile oil and ethanol extraction completely, continue to stir 18 hours, placed 22 hours at refrigerator, 38 ℃ of dryings obtain Rhizoma Curcumae effective site clathrate; (inclusion rate of Rhizoma Curcumae effective site clathrate is 92.2% after testing, and the inclusion rate is 82.7%)
(3) preparation prescription is:
Aqueous injection prescription: Rhizoma Curcumae effective site clathrate 50 grams, glucose 150 grams;
Infusion solution prescription: Rhizoma Curcumae effective site clathrate 200 grams, sodium chloride 600 grams;
The injectable powder prescription: Rhizoma Curcumae effective site clathrate 50 grams, mannitol, sucrose, lactose be totally 150 grams;
The lyophilized injectable powder prescription: Rhizoma Curcumae effective site clathrate 50 grams, sucrose, lactose be totally 150 grams;
(4) Rhizoma Curcumae effective site is mixed with pharmaceutic adjuvant, be prepared into 1000 bottles of 1000 bottles of 1000 bottles of 1000 bottles of hydro-acupuncture preparations or infusion preparations or injectable powder or lyophilized injectable powders.(effective ingredient curcumenol content is 13.8mg in the each dosage of above-mentioned after testing ejection preparation)
Embodiment 6
(1) get Rhizoma Curcumae, pulverize, put into volatile oil extractor, it is complete to extract volatile oil, and volatile oil is standby; Residue behind the extraction volatile oil is measured 80% ethanol extractions twice with 6 times, 2 hours for the first time, the 2nd time 1 hour, filter merge extractive liquid,, decompression filtrate recycling ethanol, and to be concentrated into relative density be extractum about 1.19 (50 ℃), and extractum merges ethyl acetate extraction liquid with equivalent ethyl acetate extraction 6 times, the reclaim under reduced pressure ethyl acetate is to most, and concentrate drying is standby;
(2) get Rhizoma Curcumae volatile oil and ethanol extraction, it is complete to add dissolve with ethanol, simultaneously according to Rhizoma Curcumae volatile oil and ethanol extraction: the ratio of 2-hydroxypropyl=1: 50, the 2-hydroxypropyl is made saturated solution with distilled water, put into 39 ℃ water-bath, temperature is controlled in strictness well, by the time 2-hydroxypropyl saturated aqueous solution reaches bath temperature, stir, slowly drip and dissolve Rhizoma Curcumae volatile oil and ethanol extraction completely, continue to stir 22 hours, placed 18 hours at refrigerator, 38 ℃ of dryings obtain Rhizoma Curcumae effective site clathrate; (inclusion rate of Rhizoma Curcumae effective site clathrate is 92.9% after testing, and the inclusion rate is 81.7%)
(3) preparation prescription is:
Aqueous injection prescription: Rhizoma Curcumae effective site clathrate 50 grams, sodium chloride 150 grams;
Infusion solution prescription: Rhizoma Curcumae effective site clathrate 200 grams, glucose 600 grams;
The injectable powder prescription: Rhizoma Curcumae effective site clathrate 50 grams, mannitol, lactose be totally 150 grams;
The lyophilized injectable powder prescription: Rhizoma Curcumae effective site clathrate 50 grams, mannitol, sucrose is totally 150 grams;
(4) Rhizoma Curcumae effective site is mixed with pharmaceutic adjuvant, be prepared into 1000 bottles of 1000 bottles of 1000 bottles of 1000 bottles of hydro-acupuncture preparations or infusion preparations or injectable powder or lyophilized injectable powders.(effective ingredient curcumenol content is 14.8mg in the each dosage of above-mentioned after testing ejection preparation)
Embodiment 7
(1) get Rhizoma Curcumae, pulverize, put into volatile oil extractor, it is complete to extract volatile oil, and volatile oil is standby; Residue behind the extraction volatile oil is measured 80% ethanol extractions twice with 6 times, 2 hours for the first time, the 2nd time 1 hour, filter merge extractive liquid,, decompression filtrate recycling ethanol, and to be concentrated into relative density be extractum about 1.17 (50 ℃), and extractum merges ethyl acetate extraction liquid with equivalent ethyl acetate extraction 6 times, the reclaim under reduced pressure ethyl acetate is to most, and concentrate drying is standby;
(2) get Rhizoma Curcumae volatile oil and ethanol extraction, it is complete to add dissolve with ethanol, simultaneously according to Rhizoma Curcumae volatile oil and ethanol extraction: the ratio of 2-hydroxypropyl=1: 55, the 2-hydroxypropyl is made saturated solution with distilled water, put into 34 ℃ water-bath, temperature is controlled in strictness well, by the time 2-hydroxypropyl saturated aqueous solution reaches bath temperature, stir, slowly drip and dissolve Rhizoma Curcumae volatile oil and ethanol extraction completely, continue to stir 24 hours, placed 12 hours at refrigerator, 32 ℃ of dryings obtain Rhizoma Curcumae effective site clathrate; (inclusion rate of Rhizoma Curcumae effective site clathrate is 92.6% after testing, and the inclusion rate is 82.6%)
(3) preparation prescription is:
Aqueous injection prescription: Rhizoma Curcumae effective site clathrate 100 grams, glucose 300 grams;
Infusion solution prescription: Rhizoma Curcumae effective site clathrate 400 grams, sodium chloride 1200 grams;
Injectable powder prescription: Rhizoma Curcumae effective site clathrate 100 grams, sucrose, lactose 300 grams;
Lyophilized injectable powder prescription: Rhizoma Curcumae effective site clathrate 100 grams, mannitol, sucrose 300 grams;
(4) Rhizoma Curcumae effective site is mixed with pharmaceutic adjuvant, be prepared into 2000 bottles of 2000 bottles of 2000 bottles of 2000 bottles of hydro-acupuncture preparations or infusion preparations or injectable powder or lyophilized injectable powders.(effective ingredient curcumenol content is 14.3mg in the each dosage of above-mentioned after testing ejection preparation)
Claims (1)
1. Zedoary injection preparation, the effective site that the ethanol extraction of residue is formed after it is characterized in that adopting the low temperature saturation with Rhizoma Curcumae volatile oil and extraction volatile oil is carried out enclose with the 2-hydroxypropyl, make that Rhizoma Curcumae effective site inclusion rate reaches more than 90%, the inclusion rate reaches more than 80%, wherein the preparation method of effective site clathrate is:
(1) get Rhizoma Curcumae, pulverize, put into volatile oil extractor, it is complete to extract volatile oil, and volatile oil is standby; Residue behind the extraction volatile oil is measured 80% ethanol extractions twice with 6 times, 2 hours for the first time, 1 hour for the second time, filter merge extractive liquid,, decompression filtrate recycling ethanol, and relative density is a extractum about 1.10-1.20 when being concentrated into 50 ℃, and extractum merges ethyl acetate extraction liquid with equivalent ethyl acetate extraction 6 times, the reclaim under reduced pressure ethyl acetate is to most, and concentrate drying is standby;
(2) get Rhizoma Curcumae volatile oil and ethanol extraction, it is complete to add dissolve with ethanol, simultaneously according to Rhizoma Curcumae volatile oil and ethanol extraction: the ratio of 2-hydroxypropyl=1: 20-60, the 2-hydroxypropyl is made saturated solution with distilled water, put into 30 ℃-40 ℃ water-bath, temperature is controlled in strictness well, by the time 2-hydroxypropyl saturated aqueous solution reaches bath temperature, stir, slowly drip and dissolve Rhizoma Curcumae volatile oil and ethanol extraction completely, continue to stir 12-24 hour, placed 12-24 hour at refrigerator, 30 ℃ of-40 ℃ of dryings obtain Rhizoma Curcumae effective site clathrate.
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| CN104324382A (en) * | 2013-07-22 | 2015-02-04 | 广州五丰动物保健品有限公司 | Zedoary turmeric oil beta-cyclodextrin clathrate and preparation method |
| CN108236699B (en) * | 2016-12-26 | 2021-11-09 | 中国人民解放军第三0二医院 | Zedoary turmeric oil inclusion compound for preventing or treating acute liver failure and preparation method thereof |
| CN110721289A (en) * | 2018-12-29 | 2020-01-24 | 南京中山制药有限公司 | Preparation method of Renzhu stomach-invigorating granules |
| CN115317452B (en) * | 2022-08-30 | 2023-07-21 | 北京康仁堂药业有限公司 | Traditional Chinese medicine formula particles containing curcuma zedoary and preparation method of traditional Chinese medicine formula particles |
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| CN1457798A (en) * | 2002-05-15 | 2003-11-26 | 董英杰 | Hydroypropyl-beta-cyclodextrin inclusion of Rhizoma Zedoariae oil and preparation and preparing method |
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