CN102895311B - Preparation method of illicium henryi injecta - Google Patents
Preparation method of illicium henryi injecta Download PDFInfo
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- CN102895311B CN102895311B CN201210458686.XA CN201210458686A CN102895311B CN 102895311 B CN102895311 B CN 102895311B CN 201210458686 A CN201210458686 A CN 201210458686A CN 102895311 B CN102895311 B CN 102895311B
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Abstract
The invention discloses a preparation method of illicium henryi injecta, comprising the following steps of: collecting volatile oil extracting solution (solution A) from velamen or bark coarse powder of illicium henryi by a steam distillation method to be stored; filtering the residual liquid medicine after distilling, and concentrating to be taken as a concentrated water solution (solution B) to be stored; and carrying out reflux extraction on the dregs of a decoction with ethanol to obtain ethanol extract solution (solution C), and merging the solution A, the solution B and the solution C to prepare the injecta. The injecta prepared by the method disclosed by the invention has the effects of removing tumescence, dissipating stasis, and promoting blood circulation to arrest pain, and can be used for treating the lumbar muscle strain, the joint or muscle and ligament pain, the rheumatalgia and the like.
Description
Technical field
The invention belongs to the field of Chinese medicines, be specifically related to a kind of preparation method of Injection liquid of red fennel.
Background technology
The skin of the root that Radix Illicii Lanceolati chain timbers the orchid family Illicium plant Folium illicii Lanceolati (Lllicium lanceolatum A.C Smith) is dry or stem, has effect of detumescence dissipating blood stasis, promoting blood circulation and stopping pain, for traumatic injury, and the treatment of rheumatism atrophic arthritis.At present except idol among the people has powder, outside the oral or above-mentioned disease of external curing of medicated wine, existing Zhejiang Tai Kang Pharmaceutical Group Co., Ltd produces Injection liquid of red fennel without competition, former technique is ethanol extract from water precipitation, there is the problem (particularly volatile oil part) that effective site is cannotd be used up complete, therefore the preparation technology of this Injection liquid of red fennel needs improvement badly.
Summary of the invention
The object of the invention is to overcome the preparation method that above-mentioned weak point provides a kind of Injection liquid of red fennel.
The object of the invention is to realize in the following manner:
A preparation method for Injection liquid of red fennel, the method comprises the following steps: adopt vapor distillation to extract the root bark of Radix Illicii Lanceolati or peel of stem coarse powder and obtain volatile oil is drawn liquid, separately deposit; Filter residue medicinal liquid, be concentrated into 1 ~ 2 times amount of medical material, be concentrated aqueous liquid, separately deposit; Be that 90% ~ 95% alcohol heating reflux extraction obtains alcohol extract by the medicinal residues concentration filtered out, volatile oil is drawn liquid, Aqueous extracts, alcohol extract three part merged, makes injection.
It is as follows that described vapor distillation extracts the step obtaining volatile oil is drawn liquid: the water soaking of bark of Radix Illicii Lanceolati or peel of stem coarse powder medical material 10 ~ 15 times amount 4 ~ 8 hours, and vapor distillation extracts volatile oil, collects the volatile oil is drawn liquid of medical material 5 ~ 6 times amount.
Above-mentioned alcohol heating reflux extracts and is specially medicinal residues concentration is that 90% ~ 95% alcohol heating reflux extracts 2 ~ 3 times, and each is the ethanol of 90% ~ 95% by the concentration of medical material 2 ~ 3 times amount, 1 hour each extraction time, merges ethanol extract.
Described volatile oil is drawn liquid, Aqueous extracts, alcohol extract three part merges the step making injection: in ethanol extract, add concentrated aqueous liquid, stir, leave standstill cold preservation more than 24 hours, filter, filtrate recycling ethanol is to obtaining concentrated solution without alcohol taste, the concentration adding concentrated solution 2 ~ 3 times amount is again the ethanol of 95%, staticly settle, filter, filtrate recycling ethanol is extremely without alcohol taste, the medicinal liquid reclaimed after ethanol adds the water for injection of medical material 4 ~ 6 times amount, and add activated carbon decolorizing, cold preservation more than 24 hours, filter, filtrate adjusts pH to 7.0 ~ 7.5, add volatile oil is drawn liquid, obtain oil-water mixture, again with the tween 80 stirring and dissolving of mixed liquor weight 2%, leave standstill cold preservation more than 24 hours, filter, adjust pH to 9.7 again, add to the full amount of water for injection, agitation and filtration, embedding, sterilizing, obtain.Adopt in said method concentration be 10% NaOH solution adjust pH.
Beneficial effect of the present invention compared with the prior art: preparation method of the present invention for first to use extraction by steam distillation volatile oil part, then is carried combined techniques by water extraction-ol and extracted all the other effective sites, adds volatile oil part and makes injection.The inventive method makes full use of each effective site of medical material, and the injection prepared has detumescence dissipating blood stasis, and effect of promoting blood circulation and stopping pain, is used for the treatment of lumbar muscle strain, and the grieved and rheumatalgia of joint or muscle ligament etc. has significant curative effect and safety, curative effect are lasting.
Detailed description of the invention
Below by specific embodiment, the present invention is further described; it should be pointed out that for the person of ordinary skill of the art, under the premise without departing from the principles of the invention; can also make some modification and improvement, these also should be considered as belonging to protection scope of the present invention.
Embodiment 1
Radix Illicii Lanceolati peel of stem 50g is processed into coarse powder, adds the water soaking 8 hours of medical material 10 times amount, vapor distillation, collects volatile oil is drawn liquid 300mL, separately deposits; By the residue medical filtration after volatile matter distillation oil, be concentrated into 1 times amount of 50mL(and medical material) be concentrated aqueous liquid, separately deposit.Medicinal residues concentration after filtration be 95% alcohol heating reflux extract 2 times, each ethanol consumption is 100mL, 1 hour each extraction time, merge ethanol extract, add concentrated aqueous liquid to stir, leave standstill cold preservation 24 hours, filter, filtrate recycling ethanol is to obtaining concentrated solution without alcohol taste, add the alcohol settling more than 24 hours that concentrated solution 2 times amount concentration is 95% again, filter, filtrate recycling ethanol is extremely without alcohol taste, the medicinal liquid reclaimed after ethanol injects uses water 300mL, and add 5g activated carbon decolorizing, cold preservation, filter, filtrate concentration is NaOH solution tune pH to 7.0 ~ 7.5 of 10%, add aforementioned volatile oil is drawn liquid, obtain oil-water mixture, with the tween 80 stirring and dissolving of mixed liquor weight 2%, leave standstill cold preservation 24 hours, filter, pH to 9.7 is adjusted again by the NaOH solution that concentration is 10%, inject water to 1000mL, agitation and filtration, embedding, sterilizing, obtain.
Embodiment 2
Radix Illicii Lanceolati peel of stem 50g is processed into coarse powder, adds the water soaking 4 hours of medical material 15 times amount, vapor distillation, collects volatile oil is drawn liquid 300mL, separately deposits.Residue medical filtration after volatile matter distillation oil, is concentrated into 2 times amount of 100mL(and medical material) be concentrated aqueous liquid, separately deposit.Medicinal residues concentration after filtration be 90% alcohol heating reflux extract 3 times, each ethanol consumption is 150mL, 1 hour each extraction time, merge ethanol extract, add concentrated aqueous liquid to stir, leave standstill cold preservation more than 24 hours, filter, filtrate recycling ethanol is to obtaining concentrated solution without alcohol taste, add the alcohol settling more than 24 hours that concentrated solution 3 times amount concentration is 95% again, filter, filtrate recycling ethanol is extremely without alcohol taste, the medicinal liquid reclaimed after ethanol injects uses water 300mL, and add 8g activated carbon decolorizing, cold preservation is filtered, filtrate concentration is that 10%NaOH solution adjusts pH to 7.0 ~ 7.5, add aforementioned volatile oil is drawn liquid, obtain oil-water mixture, with the tween 80 stirring and dissolving of mixed liquor weight 2%, leave standstill cold preservation 24 hours, filter, again with concentration be 10%NaOH solution adjust pH to 9.7, inject water to 1000mL, agitation and filtration, embedding, sterilizing, obtain.
The effect of injection of the present invention is further illustrated below by way of effect experiment:
Test example 1
Adopt the analgesic and anti-inflammatory effects of mouse tail pressure analgesic experiment, mice ear experiment and rat paw edema laboratory observation Radix Illicii Lanceolati peel of stem volatile oil is drawn position (HHX-1), water extract-alcohol precipitation position (HHX-2), the embodiment of the present invention 1 group (Injection liquid of red fennel prepared by the inventive method), the embodiment of the present invention 2 groups (Injection liquid of red fennel prepared by the inventive method), comparative example group (commercially available Zhejiang Tai Kang Pharmaceutical Group Co., Ltd produce Injection liquid of red fennel).
Radix Illicii Lanceolati peel of stem volatile oil is drawn position (HHX-1): get Radix Illicii Lanceolati peel of stem 50g and be processed into coarse powder, adds the water soaking 8 hours of medical material 10 times amount, vapor distillation, collects volatile oil is drawn liquid 300mL.
Radix Illicii Lanceolati peel of stem water extract-alcohol precipitation position (HHX-2): by according to the residue medical filtration after embodiment 1 method volatile matter distillation oil, being concentrated into 50mL is concentrated aqueous liquid, separately deposits.Medicinal residues concentration after filtration be 95% alcohol heating reflux extract 2 times, each ethanol consumption is 100mL, 1 hour each extraction time, merge ethanol extract, add concentrated aqueous liquid to stir, leave standstill cold preservation 24 hours, filter, filtrate recycling ethanol is to obtaining concentrated solution without alcohol taste, add concentrated solution 2 times amount dehydrated alcohol again and precipitate more than 24 hours, filter, filtrate recycling ethanol is extremely without alcohol taste, add water to 300mL, to obtain final product.
1 impact on mouse tail tenderness pain threshold
Choose the SPF level KM mice of body weight 18 ~ 22g, be placed in by mice in holder, afterbody and extremity are exposed to outside holder, test after animal peace and quiet.Survey pain before mouse tail apart from tail point 1/3 place as compression point labelling, when exerting pressure using mice occur struggle or shout as pain reaction index, this force value is this Mus pain threshold, and tie-in secondary is averaged and is worth in contrast.Select 80 mices altogether, be divided at random 8 groups (10/group), male and female half and half, namely blank group, YUNNAN BAIYAO group (5mL/kg), diclofenac group (50mg/kg), HHX-1 group (500mg/kg), HHX-2 group (500mg/kg), the embodiment of the present invention 1 group (500mg/kg), the embodiment of the present invention 2 groups (500mg/kg), comparative example group (500mg/kg).Medicine is applied in mouse tail pressure spot, 5mL/kg with microsyringe during administration, measures 15min, 30min pain threshold after administration, calculate the Δ threshold of pain (after the Δ threshold of pain=medicine before pain threshold-medicine pain threshold).Result shows: HHX-2 group upon administration 15min can significantly improve mouse tail Pain-threshold (P<0.05), and HHX-1 group has no significantly increases mouse tail Pain-threshold; Injection liquid of red fennel prepared by the inventive method and comparative example group Injection liquid of red fennel upon administration 15min all can significantly improve mouse tail Pain-threshold (P<0.05), but Injection liquid of red fennel analgesic effect prepared by the inventive method is better, and the present invention compares with comparative example group and has very significant difference, specifically in Table 1-1.
Table 1-1 is on the impact of mice tenderness pain threshold
Note: compare with blank group, * P < 0.05.
Compare with comparative example group, △ P < 0.05.
2 impacts on mice ear
Get SPF level male KM mice, body weight 18 ~ 22g, be divided at random 8 groups (10/group), namely blank group, YUNNAN BAIYAO group (5mL/kg), diclofenac group (50mg/kg), HHX-1 group (500mg/kg), HHX-2 group (500mg/kg), the embodiment of the present invention 1 group (500mg/kg), the embodiment of the present invention 2 groups (500mg/kg), comparative example group (500mg/kg).Medicine is applied in mice left and right auricle, 5mL/kg with microsyringe during administration.After auricle administration 30min, utilize microsyringe to drip in auris dextra both sides respectively by 0.05mL dimethylbenzene, ensure drip position consistency, left ear compares.After 3h, mice is taken off cervical vertebra to put to death, cut two ears along auricle baseline, lay circular auricle at the same position of left and right ear respectively with the card punch of diameter 9mm, weigh, ask the difference of left and right auricle weight as swelling, compare group difference with blank group.Result shows: compare with blank group, HHX-1 and HHX-2 group all can alleviate dimethylbenzene induced mice ear thickness (P<0.05); Injection liquid of red fennel prepared by the inventive method extremely significantly can alleviate dimethylbenzene induced mice ear thickness (P<0.01), and the present invention compares with comparative example group and has very significant difference, more remarkable than comparative example group Injection liquid of red fennel antiphlogistic effects, specifically in Table 1-2.
Table 1-2 is on the impact of mice ear
Note: compare with blank group, * P < 0.05, * * P < 0.01.
Compare with comparative example group, △ P < 0.05.
3 impacts on rat carrageenan pedal swelling
Get SPF level male rat, body weight 180 ~ 220g, be divided at random 8 groups (10/group), namely blank group, YUNNAN BAIYAO group (1mL/kg), diclofenac group (10mg/kg), HHX-1 group (100mg/kg), HHX-2 group (100mg/kg), the embodiment of the present invention 1 group (100mg/kg), the embodiment of the present invention 2 groups (100mg/kg), comparative example group (100mg/kg).In right back ankle joint labelling, sufficient sole of the foot capacity measurer is utilized first to survey the normal right back sufficient sole of the foot volume of rat.Microsyringe is utilized medicine to be applied in right back sufficient sole of the foot portion, 1mL/kg.After toes administration 30min, every right back sufficient plantar subcutaneous injection 1% carrageenin 0.1mL of Mus, and in giving after carrageenin 30,60,120,240,360min surveys Rat Right metapedes sole of the foot volume (mL) again, and calculate swelling (swelling degree of the paw=to different time foot sole of the foot volume after carrageenin-to before carrageenin with parapodum sole of the foot volume).Result shows: compare with blank group, and HHX-1 group 30min after administration significantly can alleviate rat paw edema degree (P<0.05), and HHX-2 group rat paw edema degree has no and obviously alleviates; Injection liquid of red fennel prepared by the inventive method significantly can alleviate rat paw edema degree (P<0.05), and the present invention compares with comparative example group and has very significant difference, than comparative example group Injection liquid of red fennel Be very effective, specifically in Table 1-3.
Table 1-3 is on the impact of rat carrageenan pedal swelling
Note: compare with blank group, * P < 0.05.
Compare with comparative example group, △ P < 0.05.
Analgesic and anti-inflammatory effects result of study shows: HHX-1 and HHX-2 group all can alleviate dimethylbenzene induced mice ear thickness, and HHX-1 group 30min after administration can significantly alleviate rat paw edema degree, and HHX-2 group has no obviously alleviating of rat paw edema degree; But HHX-2 group upon administration 15min can significantly improve mouse tail Pain-threshold.Result prompting Radix Illicii Lanceolati peel of stem volatile oil is drawn position is better than water extract-alcohol precipitation position for the inhibitory action of inflammation, but the analgesic activity at water extract-alcohol precipitation position is better than volatile oil is drawn position; The Injection liquid of red fennel adopting the Injection liquid of red fennel prepared of the inventive method to prepare than existing technique and the antalgic and inflammation relieving effect potentiation of HHX-1 and HHX-2 position remarkable.
Claims (2)
1. a preparation method for Injection liquid of red fennel, is characterized in that the method comprises the following steps: adopt vapor distillation to extract the root bark of Radix Illicii Lanceolati or peel of stem coarse powder and obtain volatile oil is drawn liquid, separately deposit, filter residue medicinal liquid, be concentrated into 1 ~ 2 times amount of medical material, be concentrated aqueous liquid, separately deposit, be that 90% ~ 95% alcohol heating reflux extraction obtains alcohol extract by the medicinal residues concentration filtered out, volatile oil is drawn liquid, Aqueous extracts, alcohol extract three part merged, makes injection, described volatile oil is drawn liquid, Aqueous extracts, alcohol extract three part merges the step making injection: in ethanol extract, add concentrated aqueous liquid, stir, leave standstill cold preservation more than 24 hours, filter, filtrate recycling ethanol is to obtaining concentrated solution without alcohol taste, the concentration adding concentrated solution 2 ~ 3 times amount is again the ethanol of 95%, staticly settle, filter, filtrate recycling ethanol is extremely without alcohol taste, the medicinal liquid reclaimed after ethanol adds the water for injection of medical material 4 ~ 6 times amount, and add activated carbon decolorizing, cold preservation more than 24 hours, filter, filtrate adjusts pH to 7.0 ~ 7.5, add volatile oil is drawn liquid, obtain oil-water mixture, again with the tween 80 stirring and dissolving of mixed liquor weight 2%, leave standstill cold preservation more than 24 hours, filter, adjust pH to 9.7 again, add to the full amount of water for injection, agitation and filtration, embedding, sterilizing, obtain,
it is as follows that described vapor distillation extracts the step obtaining volatile oil is drawn liquid: the water soaking of bark of Radix Illicii Lanceolati or peel of stem coarse powder medical material 10 ~ 15 times amount 4 ~ 8 hours, and vapor distillation extracts volatile oil, collects the volatile oil is drawn liquid of medical material 5 ~ 6 times amount;
Described to obtain ethanol extract concrete steps as follows: heating and refluxing extraction 2 ~ 3 times, each is the ethanol of 90% ~ 95% with the concentration of medical material 2 ~ 3 times amount, 1 hour each extraction time, merging ethanol extract.
2. preparation method according to claim 1, it is characterized in that by concentration be 10% NaOH solution adjust pH.
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| CN104586937A (en) * | 2013-11-01 | 2015-05-06 | 浙江泰康药业集团有限公司 | Preparation method of illicium plants injection |
| CN106265923A (en) * | 2015-06-07 | 2017-01-04 | 浙江泰康药业集团有限公司 | A kind of method improving clarity of injection |
| CN105851068A (en) * | 2016-04-01 | 2016-08-17 | 江南大学 | Method for preparing antibacterial agent and bacterial quorum sensing inhibitor by using fennel |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1634412A (en) * | 2004-10-29 | 2005-07-06 | 张平 | Lanceleaf anisetree freeze dried and preparation method thereof |
| CN102688294A (en) * | 2012-06-13 | 2012-09-26 | 浙江农林大学 | Illicium henryi-contained anti-virus ointment for external use and preparation method and application thereof |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1634412A (en) * | 2004-10-29 | 2005-07-06 | 张平 | Lanceleaf anisetree freeze dried and preparation method thereof |
| CN102688294A (en) * | 2012-06-13 | 2012-09-26 | 浙江农林大学 | Illicium henryi-contained anti-virus ointment for external use and preparation method and application thereof |
Non-Patent Citations (1)
| Title |
|---|
| 红茴香药学研究概况;陈烨丹等;《安徽农业科学》;20110731;第39卷(第14期);第8376-8377页 * |
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