CN1660278B - Compound injection of Chinese angelica root and chuanxiong rhizome and preparation method - Google Patents
Compound injection of Chinese angelica root and chuanxiong rhizome and preparation method Download PDFInfo
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- CN1660278B CN1660278B CN 200410082967 CN200410082967A CN1660278B CN 1660278 B CN1660278 B CN 1660278B CN 200410082967 CN200410082967 CN 200410082967 CN 200410082967 A CN200410082967 A CN 200410082967A CN 1660278 B CN1660278 B CN 1660278B
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Abstract
A Chinese medicine in the form of injection is prepared from Chinese angelica root, Chuan-xiong rhizome, stabilizer, pH regulator and the water for injection through distilling to extract volatile oil, extracting water-soluble active components, separating by macroreticular adsorbent, removing tannin by polyamide, purifying, and mixing it with said volatile oil.
Description
Technical field:
The present invention relates to a kind of Chinese medicine injection and preparation method thereof, particularly, is a kind of Chinese medicine injection (comprising the used for intravenous injection freeze-dried powder)-compound Chinese angelica-root Rhizoma Chuanxiong injection that supplies intramuscular injection and preparation method thereof.
Background technology:
The powder of being made up of Radix Angelicae Sinensis and Rhizoma Chuanxiong is called foshousan, belongs to blood-activating stasis-removing kind Chinese medicine, is widely used in tcm clinical practice, and it is evident in efficacy, but clinical practice has only powder and decocting decoction, so far the injection of none set pattern lattice.All contain water solublity effective site and volatile oil in Radix Angelicae Sinensis and the Rhizoma Chuanxiong, wherein volatile oil is one of main active site of two flavor Chinese medicines, but extremely unstable, is difficult to make certain dosage form for clinical use.Use in the preparation of Radix Angelicae Sinensis and Rhizoma Chuanxiong medical material preparation all not moisture simultaneously dissolubility effective site and volatile oil at present.The FUFANG DANGGUI ZHUSHEYE of recording in " national standard for traditional Chinese medicines compilation " is made with extra care and is formed by Radix Angelicae Sinensis, Rhizoma Chuanxiong and Flos Carthami three flavor Chinese crude drugs, wherein Radix Angelicae Sinensis and Rhizoma Chuanxiong two medical materials is adopted decocting technology, does not contain volatile oil.
Summary of the invention:
The object of the present invention is to provide a kind of compound Chinese angelica-root Rhizoma Chuanxiong injection, both contained water solublity effective site, contain volatile oil again, and solve the unsettled difficult problem of effective site among this side, filled up the blank of this side's injection type, safe in utilization, reliably, evident in efficacy, and its preparation method is provided.
Compound Chinese angelica-root Rhizoma Chuanxiong injection provided by the invention, contained main component are the effective part groups that Radix Angelicae Sinensis and Rhizoma Chuanxiong extract, and its packing of product is the ampoule of 1～10ml; It makes intermediate by Radix Angelicae Sinensis Rhizoma Chuanxiong decoction pieces through the extraction separation purification, and it is formulated to add pharmaceutical carriers such as solubilizing agent, cosolvent, pH regulator agent, stabilizing agent and water for injection again in intermediate.
Compound Chinese angelica-root Rhizoma Chuanxiong injection provided by the invention, it basic composition is: Radix Angelicae Sinensis 50～1000g/L injection, Rhizoma Chuanxiong 50～1000g/L injection, solubilizing agent 0～50g/L injection, cosolvent 0～700g/L injection, stabilizing agent 2～12g/L injection, all the other are pH regulator agent and water for injection.Wherein Radix Angelicae Sinensis content is 50～1000g/L injection, and Rhizoma Chuanxiong content is 50～1000g/L injection, and Radix Angelicae Sinensis and Rhizoma Chuanxiong content sum are 100～1000g/L injection.Radix Angelicae Sinensis and Rhizoma Chuanxiong volatile oil extract and comprise the water distil process, and water solublity effective site is extracted and comprised that in water decoction-alcohol sedimentation, alcohol extracting-water precipitating, macroporous absorption, polyamide absorption and the organic solvent extracting taking technique one or more combine.
The volatile oil that the water distillating method extracts, its quality can meet the injection related request, but water solublity effective site contains a large amount of ash after extracting, and must separation and purification.Use macroporous adsorbent, purpose is water solublity drug effect position is separated with non-drug effect position.The present invention uses nonpolar macroporous adsorbent, comprises among D101, X-5, HP series, CAD series, XAD series, LD series, H107, AB-8, the NKA-9 one or more.The pH of feed liquid and concentration during absorption, the kind of eluant and concentration directly influence the content and the quality of effective site in the eluent.The absorption pH value is between pH2.0～pH6.0, and feed concentration is between 0.5ml/g decoction pieces～15ml/g decoction pieces, and eluant is Different concentrations of alcohol or aqueous propanol solution, and concentration is 50%～100%.Polyamide is used for removing a spot of tannin, its model comprises one or more among polyamide series, polyamide 103,650#, 651#, 900GC, 930GC, 930GLC, PS-1 and the PS-2, solvent for use is the aqueous solution of ethanol or acetone during polyamide absorption, and concentration range is a certain concentration in 30%～100%.Solvent extraction is further purified the drug effect position, extraction conditions such as solvent species and pH value is the Quality Control key factor, solvent species comprises it being in ethers (as ether), esters (as ethyl acetate), the halogenated alkane (as dichloromethane, chloroform) one or more, and pH value is an a certain value between pH2.0～pH6.0.
The use of pharmaceutical carrier is to dissolve intermediate, guarantees that it is stable, and makes corresponding dosage for clinical use.Pharmaceutical carriers such as solubilizing agent, cosolvent, pH regulator agent, stabilizing agent and water for injection can be used one or more, and stabilizing agent is a key of guaranteeing content and drug effect, must use all the other pharmaceutical carriers even can.Stabilizing agent comprises one or more in sodium sulfite, sodium sulfite, sodium pyrosulfite, vitamin C, sodium thiosulfate, cysteine, methionine, thiacetic acid., thioglycerol, enuatrol or various low-molecular-weight alcohol or the sugar.Solubilizing agent solubilized volatile oil comprises in tween series, span series, the rare fatty acid ester series of polyoxy second, the rare fat lipidol of polyoxy second ether series and the poloxamer series one or more.Cosolvent comprises one or more in lower alcohols such as ethanol, propylene glycol and the glycerol etc., the injection pH value is influential to stability, the pH regulator agent comprises acids such as hydrochloric acid, acetic acid, phosphoric acid, or among the bases such as sodium hydroxide, sodium bicarbonate, sodium hydroxide one or more.
Compound Chinese angelica-root Rhizoma Chuanxiong injection preparation method provided by the invention comprises following step: (1) first water distillation preparation Radix Angelicae Sinensis Rhizoma Chuanxiong volatile oil; (2) extract water solublity effective site with water decoction-alcohol sedimentation in conjunction with alcohol extraction process, and adopt macroporous adsorbent separation, polyamide to remove tannin, the organic solvent extraction purification gets water solublity effective site refined liquid, with water solublity effective site refined liquid and volatile oil merge intermediate; (3) be mixed with clear and bright solution by adding cosolvent, solubilizing agent, stabilizing agent, pH regulator agent and water for injection etc.; (4) with sodium hydroxide or sodium carbonate or sodium bicarbonate or hydrochloric acid accent pH to 5.0～7.0, filter, benefit adds to the full amount of water for injection, measure the qualified back of content with being packaged in behind the microporous filter membrane fine straining in the suitable ampoule, after sterilization, lamp inspection, the quality inspection of routine are qualified, obtain compound recipe again when the Rhizoma Chuanxiong injection finished product.Its packing is undertaken by the injection relevant requirements.
Compound Chinese angelica-root Rhizoma Chuanxiong injection of the present invention can be by following index test:
The name of an article: compound Chinese angelica-root Rhizoma Chuanxiong injection
Character: faint yellow to yellow clear liquid
Differentiate: show positive reaction
PH value: 5.0～7.0
Other: meet requirement under the injection item
Sterility test: qualified
Pyrogen testing: qualified
The specific embodiment:
Embodiment 1: preparation compound Chinese angelica-root Rhizoma Chuanxiong injection: carry out according to the following steps:
(1) preparation volatile oil: Radix Angelicae Sinensis Rhizoma Chuanxiong decoction pieces was pulverized 20 mesh sieves, respectively get flour 100g, add injection water 1600ml, soaking 4h, is solvent with volatile oil extractor with petroleum ether (30～60 ℃), behind the water distillation 6h, collect volatile oil, 60 ℃ volatilize petroleum ether, get faint yellow volatile oil, and 4 ℃ of freezer storages are standby.
(2) preparation water solublity effective site: connect above-mentioned (1) step, will distill the back residual liquid and filter, get filtrate A, medicinal residues add 1600ml 70% ethanol again, filter behind the reflux, extract, 1.5h, get alcohol extract B, merge A and B, filter, 65 ℃ of vacuum concentration of filtrate are put 6h for 4 ℃～10 ℃ to 2000ml, filter clear and bright filtrate, pH4.0～4.5 are transferred in 1N acid, wait to adsorb; Get the D101 macroporous adsorbent (30～60 order) that 150ml handles well, be contained in the glass column (H/D～6: 1), after the absorption of 150ml/h flow velocity upper prop, wash saturated resin with the 300ml/h flow velocity with 600ml water, reuse 85% ethanol carries out eluting with 60～75ml/h flow velocity, gets eluent 250ml; Get chromatographic grade polyamide (30～60 order) 30ml of processing, add in the eluent, filter behind the magnetic agitation 12h, 65 ℃ of vacuum concentration of filtrate behind the 200ml water dissolution residue, are put 6h to 20ml for 4 ℃～10 ℃, filter clear and bright filtrate, 1N hydrochloric acid is transferred pH3.0, the 400ml ether divides 4 extractions; Combining extraction liquid, the evaporate to dryness ether gets water solublity effective site.
(3) preparation compound Chinese angelica-root Rhizoma Chuanxiong injection: (1) step gained volatile oil is added in (2) step gained water solublity effective site, get the compound recipe intermediate, add the 40ml propylene glycol, 6.0g tween 80, the 1.0g enuatrol stirs, 2N NaOH transfers pH6.5～7.0, and water for injection is fixed to 200ml.Detection level when qualified, filters through 0.4 μ m filter membrane, fill in suitable brown ampoule, 100 ℃ of sterilization 1h, cooling back lamp inspection obtains compound Chinese angelica-root Rhizoma Chuanxiong injection finished product after qualified.
Embodiment 2: preparation compound Chinese angelica-root Rhizoma Chuanxiong injection: carry out according to the following steps:
(1) preparation volatile oil: press (1) step preparation volatile oil among the embodiment 1.
(2) preparation water solublity effective site: connect above-mentioned (1) step, to distill the back residual liquid and filter, medicinal residues add 1600ml water again, behind the decoction 0.5h that refluxes, filter, merge decocting filtrate twice, 65 ℃～80 ℃ vacuum concentration are to 1200ml, and adding 95% ethanol is 60% to containing the alcohol amount, put 6h for 4 ℃～10 ℃, filter, 65 ℃ of vacuum concentration of filtrate filter to 800ml, 65 ℃～80 ℃ vacuum concentration of filtrate are to 200ml, filter, adding 95% ethanol is that 85%, 4 ℃～10 ℃ refrigerators are put 6h to containing the alcohol amount, filter, 65 ℃ of vacuum concentration of filtrate are to 50ml, and 1N hydrochloric acid is transferred pH3.0, and the 200ml ether divides 4 extractions; Combining extraction liquid, the evaporate to dryness ether gets water solublity effective site.
(3) preparation compound Chinese angelica-root Rhizoma Chuanxiong injection: with (3) step among the embodiment 1.
Embodiment 3: preparation compound Chinese angelica-root Rhizoma Chuanxiong injection: carry out according to the following steps: its each all same embodiment (1) only will replace propylene glycol to make with glycerol in the step (3).
Embodiment 4: preparation compound Chinese angelica-root Rhizoma Chuanxiong injection: all same embodiment of its each step (1) only will replace propylene glycol to make with ethanol in the step (3).
Embodiment 5: preparation compound Chinese angelica-root Rhizoma Chuanxiong injection: all same embodiment of its each step (1) does not only make not adding propylene glycol in the step (3).
Embodiment 6: preparation compound Chinese angelica-root Rhizoma Chuanxiong injection: all same embodiment of its each step (1), only will not add tween 80 in the step (3), and replace propylene glycol to make with glycerol and ethanol mixing cosolvent.
Embodiment 7: preparation compound Chinese angelica-root Rhizoma Chuanxiong injection: all same embodiment of its each step (1), only will not add tween 80 in the step (3), and replace propylene glycol to make with ethanol and mixed with propylene glycol cosolvent.
Embodiment 8: preparation compound Chinese angelica-root Rhizoma Chuanxiong injection: all same embodiment of its each step (1), only will not add tween 80 in the step (3), and replace propylene glycol to make with ethanol.
Embodiment 9: preparation compound Chinese angelica-root Rhizoma Chuanxiong injection: all same embodiment of its each step (1), only with in the step (3) with NaHCO
3Replace NaOH to make.
Claims (7)
1. compound Chinese angelica-root Rhizoma Chuanxiong injection, it is characterized in that: this injection is prepared from according to the following steps:
(1) preparation volatile oil: Radix Angelicae Sinensis Rhizoma Chuanxiong decoction pieces was pulverized 20 mesh sieves, respectively get flour 100g, add injection water 1600ml, soaking 4h, is that 30～60 ℃ of petroleum ether are solvent with volatile oil extractor with boiling range, behind the water distillation 6h, collect volatile oil, 60 ℃ volatilize petroleum ether, get faint yellow volatile oil, and 4 ℃ of freezer storages are standby;
(2) preparation water solublity effective site: connect above-mentioned (1) step, will distill the back residual liquid and filter, get filtrate A, medicinal residues add 1600ml 70% ethanol again, filter behind the reflux, extract, 1.5h, get alcohol extract B, merge A and B, filter, 65 ℃ of vacuum concentration of filtrate are put 6h for 4 ℃～10 ℃ to 2000ml, filter clear and bright filtrate, pH4.0～4.5 are transferred in 1N acid, wait to adsorb; Get 30～60 order D101 macroporous adsorbents that 150ml handles well, be contained in the glass column H/D～6: 1, after the absorption of 150ml/h flow velocity upper prop, with 300ml/h flow velocity washing saturated resin, reuse 85% ethanol carries out eluting with 60～75ml/h flow velocity, gets eluent 250ml with 600ml water; Get 30～60 order chromatographic grade kymene 0ml that handle well, add in the eluent, filter behind the magnetic agitation 12h, 65 ℃ of vacuum concentration of filtrate behind the 200ml water dissolution residue, are put 6h to 20ml for 4 ℃～10 ℃, filter clear and bright filtrate, 1N hydrochloric acid is transferred pH3.0, the 400ml ether divides 4 extractions; Combining extraction liquid, the evaporate to dryness ether gets water solublity effective site;
(3) preparation compound Chinese angelica-root Rhizoma Chuanxiong injection: (1) step gained volatile oil is added in (2) step gained water solublity effective site, get the compound recipe intermediate, add the 40ml propylene glycol, 6.0g tween 80, the 1.0g enuatrol stirs, 2N NaOH transfers pH6.5～7.0, and water for injection is fixed to 200ml, detection level, when qualified, filter through 0.4 μ m filter membrane, fill in suitable brown ampoule, 100 ℃ of sterilization 1h, cooling back lamp inspection obtains compound Chinese angelica-root Rhizoma Chuanxiong injection finished product after qualified.
2. compound Chinese angelica-root Rhizoma Chuanxiong injection as claimed in claim 1 is characterized in that: in step (2) above-mentioned for connecing (1) step, will distill the back residual liquid and filter, medicinal residues add 1600ml water again, reflux behind the decoction 0.5h, filter, merge decocting filtrate twice, 65 ℃～80 ℃ vacuum concentration are to 1200ml, add 95% ethanol and be 60%, 4 ℃～10 ℃ to the alcohol amount of containing and put 6h, filter, 65 ℃ of vacuum concentration of filtrate are to 800ml, filter, 65 ℃～80 ℃ vacuum concentration of filtrate filter to 200ml, adding 95% ethanol is 85% to containing the alcohol amount, 4 ℃～10 ℃ refrigerators are put 6h, filter, and 65 ℃ of vacuum concentration of filtrate are to 50ml, 1N hydrochloric acid is transferred pH3.0, and the 200ml ether divides 4 extractions; Combining extraction liquid, the evaporate to dryness ether gets water solublity effective site.
3. compound Chinese angelica-root Rhizoma Chuanxiong injection as claimed in claim 1 is characterized in that: substitute propylene glycol with glycerol in the step (3).
4. compound Chinese angelica-root Rhizoma Chuanxiong injection as claimed in claim 1 is characterized in that: substitute propylene glycol with ethanol in the step (3).
5. compound Chinese angelica-root Rhizoma Chuanxiong injection as claimed in claim 1 is characterized in that: step does not add propylene glycol in (3).
6. compound Chinese angelica-root Rhizoma Chuanxiong injection as claimed in claim 1 is characterized in that: step does not add tween 80 in (3), replaces propylene glycol with ethanol.
7. compound Chinese angelica-root Rhizoma Chuanxiong injection as claimed in claim 1 is characterized in that: in the step (3) with NaHCO
3Replace NaOH.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410082967 CN1660278B (en) | 2004-12-14 | 2004-12-14 | Compound injection of Chinese angelica root and chuanxiong rhizome and preparation method |
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| CN 200410082967 CN1660278B (en) | 2004-12-14 | 2004-12-14 | Compound injection of Chinese angelica root and chuanxiong rhizome and preparation method |
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| CN1660278A CN1660278A (en) | 2005-08-31 |
| CN1660278B true CN1660278B (en) | 2011-05-25 |
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| CN 200410082967 Expired - Fee Related CN1660278B (en) | 2004-12-14 | 2004-12-14 | Compound injection of Chinese angelica root and chuanxiong rhizome and preparation method |
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Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1813833B (en) * | 2005-12-11 | 2012-02-22 | 沈阳药科大学 | Medicinal composition of chinese angelica and ligusticum wallichii and its preparing method |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1197654A (en) * | 1997-04-25 | 1998-11-04 | 中国人民解放军第八十八医院 | Cardio- and cerebro-angiopathy curing drop pellet and its preparation |
| CN1376504A (en) * | 2002-04-10 | 2002-10-30 | 武汉大学 | Intravenous injection of Chinese angelica root and its preparing process |
| CN1478501A (en) * | 2002-08-28 | 2004-03-03 | 山东凤凰制药有限公司 | Chinese medicinal composition for treating coronary heart disease and angina pectoris and its preparation process |
| CN1502353A (en) * | 2002-11-20 | 2004-06-09 | 北京瑞康医药技术有限公司 | Compound chuanxiong and angelica total extract and preparation, use thereof |
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2004
- 2004-12-14 CN CN 200410082967 patent/CN1660278B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1197654A (en) * | 1997-04-25 | 1998-11-04 | 中国人民解放军第八十八医院 | Cardio- and cerebro-angiopathy curing drop pellet and its preparation |
| CN1376504A (en) * | 2002-04-10 | 2002-10-30 | 武汉大学 | Intravenous injection of Chinese angelica root and its preparing process |
| CN1478501A (en) * | 2002-08-28 | 2004-03-03 | 山东凤凰制药有限公司 | Chinese medicinal composition for treating coronary heart disease and angina pectoris and its preparation process |
| CN1502353A (en) * | 2002-11-20 | 2004-06-09 | 北京瑞康医药技术有限公司 | Compound chuanxiong and angelica total extract and preparation, use thereof |
Non-Patent Citations (2)
| Title |
|---|
| 陈金秀.复方当归注射液的制备、质量控制及临床疗效.河南医药信息10 19.2002,10(19),39. |
| 陈金秀.复方当归注射液的制备、质量控制及临床疗效.河南医药信息10 19.2002,10(19),39. * |
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