CN102078411B - Preparation method of spreading hedyotis herb injection - Google Patents
Preparation method of spreading hedyotis herb injection Download PDFInfo
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- CN102078411B CN102078411B CN 200910238513 CN200910238513A CN102078411B CN 102078411 B CN102078411 B CN 102078411B CN 200910238513 CN200910238513 CN 200910238513 CN 200910238513 A CN200910238513 A CN 200910238513A CN 102078411 B CN102078411 B CN 102078411B
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Abstract
The invention discloses a preparation method of a spreading hedyotis herb injection, and the method belongs to the field of traditional Chinese medicine and comprises the following steps: performing heating reflux extraction on spreading hedyotis herb with 60% ethanol, and filtering, thus getting an ethanol extract solution and filter residues; extracting the filter residues with water, and filtering, thus getting a water extract solution; merging the ethanol extract solution with the water extract solution, regulating the pH to 12 by using lime water, refrigerating, filtering, regulating thepH value of a filtrate to 3 by using a 50% sulfuric acid solution, standing, filtering, regulating the filtrate to be neutral by further using a 40% sodium hydroxide solution, adding the ethanol, refrigerating, filtering, adding an appropriate amount of activated carbon into the filtrate, stirring, filtering, regulating the pH value of the filtrate to 6.5-7.0 by using the 40% sodium hydroxide solution, adding polysorbate and sodium bisulfite, stirring, and filtering; and adding the water for injection, filling, sealing, and sterilizing, thus getting the spreading hedyotis herb injections.
Description
Technical field
The present invention relates to the preparation method of BAIHUASHESHECAO ZHUSHEYE.
Background technology
Herba Hedyotidis Diffusae (Oldenlandia diffusa (Willd) Roxb) beginning is stated from " Guangxi Chinese medicinal herbal ", is the whole herb with root of Maguireothamnus speciosus Herba Hedyotidis Diffusae.Be distributed widely in the Yangtze river basin and on the south, ground such as main product Fujian, Guangdong, Guangxi, its bitter in the mouth, sweet, cold is gone into the heart, liver, spleen three warps, and heat-clearing and toxic substances removing is arranged, blood circulation promoting and blood stasis dispelling, effects such as anti-inflammatory analgetic.Modern pharmacological research shows that Herba Hedyotidis Diffusae has effects such as anti-inflammation, heat-clearing and toxic substances removing, blood circulation promoting and blood stasis dispelling, relieving stranguria by diuresis and antitumor, can be used for treating gastric cancer, the esophageal carcinoma, rectal cancer, malignant lymphoma, pulmonary carcinoma, hepatocarcinoma, cervical cancer, ovarian cancer, bladder cancer etc., clinical practice is extensive.Flavonoid in the Herba Hedyotidis Diffusae, triterpene mixed acid, Coumarins and polysaccharide are its anticancer main effective ingredient.
Solvent extraction method is according to the dissolution properties of various compositions in solvent in the Chinese herbal medicine, select for use the active component dissolubility big, to not needing the little solvent of stripping composition dissolubility, and the method that effective ingredient is dissolved out in the medical material tissue.When solvent is added in the herbal raw material (needing suitably to pulverize), solvent is owing to diffusion, osmosis penetrate in the cell by cell wall gradually, dissolved solable matter, and cause concentration difference inside and outside the cell, so intracellular concentrated solution is constantly to external diffusion, solvent constantly enters in the medical material histiocyte again, so repeatedly come and go, when solution concentration reaches dynamic equilibrium inside and outside cell, this saturated solution is leached, continue repeatedly to add novel solvent, just can be bordering on complete stripping or the stripping of big portion to desirable ingredients.
Summary of the invention
The invention provides a kind of preparation method of BAIHUASHESHECAO ZHUSHEYE, purpose provides the high BAIHUASHESHECAO ZHUSHEYE of a kind of general flavone content.
The preparation method of a kind of BAIHUASHESHECAO ZHUSHEYE provided by the present invention, the alcohol heating reflux with 60% extracts Herba Hedyotidis Diffusae, filters, obtain ethanol extract and filtering residue, described filtering residue water extraction filters, obtain aqueous extract, described ethanol extract and described aqueous extract are merged, transfer pH to 12 with lime water, cold preservation filters, and it is 3 that filtrate is regulated pH value with 50% sulfuric acid solution, leave standstill, filter, filtrate reuse 40% sodium hydroxide solution transfers to neutrality, add ethanol, cold preservation filters, and filtrate adds proper amount of active carbon, stir, filter, it is 6.5～7.0 that filtrate is regulated pH value with 40% sodium hydroxide solution, adds Polysorbate and sodium sulfite, stir, filter, add the injection water, embedding, sterilization obtains BAIHUASHESHECAO ZHUSHEYE.
Wherein, described alcohol heating reflux carries out three times, and each extraction time was respectively 2,1 and 1 hours.
Described water extraction 2 times, each time of extracting is 2 and 1 hours.
It is 1.23-1.25 that described ethanol extract is concentrated into relative density.
Solution concentration to relative density after described ethanol extract and described aqueous extract merge is 1.20-1.25.
The total flavones of effective ingredient exceeds one times than the effective ingredient in the BAIHUASHESHECAO ZHUSHEYE of percolation extraction in the BAIHUASHESHECAO ZHUSHEYE of the present invention.
The specific embodiment
Embodiment 1, BAIHUASHESHECAO ZHUSHEYE
That gets 1000g is viridian Guangxi Herba Hedyotidis Diffusae herb through drying in the shade, put in the extraction pot, extract 3 times with 60% alcohol heating reflux, each extraction time was respectively 2,1,1 hours, and it is standby that merge extractive liquid,, filtration, filtrate are concentrated into relative density 1.23-1.25.Medicinal residues are put in another extraction pot with the water extraction of 5 times of Herba Hedyotidis Diffusae herb quality 2 times again, and each time of extracting is 2 and 1 hours, merge extractive liquid,, filter, be concentrated into relative density 1.20-1.25 after, two concentrated solutions are merged, transfer pH to 12 with lime water, cold preservation 12 hours filters, it is 3 that filtrate is regulated pH value with 50% sulfuric acid solution, leaves standstill 12 hours, filters, filtrate reuse 40% sodium hydroxide solution transfers to neutrality, adds ethanol 2000ml, cold preservation 24 hours, filter, filtrate decompression is concentrated into 250ml, adds water to 500ml, adds proper amount of active carbon, stir evenly, filter, it is 6.5～7.0 that filtrate is regulated pH value with 40% sodium hydroxide solution, adds the 10g polyoxyethylene sorbitan monoleate, the 1g sodium sulfite, fully stir evenly, filter, add the injection water to 1000ml, embedding, sterilization namely gets BAIHUASHESHECAO ZHUSHEYE.
BAIHUASHESHECAO ZHUSHEYE is the clear liquid of pale brown color.
Get BAIHUASHESHECAO ZHUSHEYE 30ml, be added on the polyamide column (50 orders, 2g, the internal diameter 12～15mm that have handled well, wet method dress post) on, uses the 50ml water elution, discard water liquid, use 70% ethanol elution, when yellow colour band flows out, begin to collect eluent 5ml, as need testing solution.Get need testing solution number droplet, put on filter paper, dry, Dropwise 5 % aluminum chloride alcoholic solution dries, and puts under the ultra-violet lamp (365nm) and observes, and shows yellow-green fluorescence.
Precision takes by weighing at the control substance of Rutin 10mg of 120 ℃ of drying under reduced pressure to constant weight, puts in the 50ml measuring bottle, adds an amount of 70% ethanol, put that slight fever makes dissolving in the water-bath, put coldly, add 70% ethanol to scale, shake up, namely get (containing anhydrous rutin 0.2mg among every 1ml) reference substance solution.
Precision is measured reference substance solution 0.0,1.0,2.0,3.0,4.0,5.0 and 6.0ml, puts respectively in the 25ml measuring bottle, respectively adds 70% ethanol to 6ml, add 5% sodium nitrite solution 1ml, shake up, placed 6 minutes, add 10% aluminum nitrate solution 1ml, shake up, placed 6 minutes, hydro-oxidation sodium test solution 10ml adds ethanol again to scale, shakes up, placed 15 minutes, and according to spectrophotography, measured trap at the wavelength place of 507nm, be that vertical coordinate, concentration are abscissa with the trap, the drawing standard curve.
Precision is measured BAIHUASHESHECAO ZHUSHEYE 10ml, is added on the polyamide column (50 orders, the 2g that have handled well, internal diameter 12～15mm, wet method dress post) on, use the 50ml water elution, discard eluent, use 70% ethanol elution, collect the about 25ml of eluent, put in the 25ml measuring bottle, add 70% ethanol dilution to scale, shake up, precision is measured 5ml respectively, puts first, in two 25ml measuring bottles of second, add 5% sodium nitrite solution 1ml in the first bottle, shake up, placed 6 minutes, and added 10% aluminum nitrate solution 1ml, shake up, placed 6 minutes, in first, each hydro-oxidation sodium test solution 10ml in two bottles of the second adds ethanol dilution again to scale, shakes up, placed 15 minutes, according to spectrophotography, be blank with the second bottle, measure trap at the wavelength place of 507nm, read the amount of rutin the BAIHUASHESHECAO ZHUSHEYE from standard curve, calculate.
The amount that contains total flavones in every milliliter of rutin in 8 parts of BAIHUASHESHECAO ZHUSHEYE is respectively 0.59,0.56,0.61,0.58,0.52,0.50,0.54 and 0.62mg.
Comparative Examples,
Get Herba Hedyotidis Diffusae 1000g, be ground into coarse powder, make solvent with 80% ethanol, flooded 24 hours, percolation slowly, the liquid of filtering is concentrated into about 250ml, regulate pH value to 12 with lime cream, cold preservation 12 hours filters, it is 3 that filtrate is regulated pH value with 50% sulfuric acid solution, leaves standstill 12 hours, filters, filtrate reuse 40% sodium hydroxide solution transfers to neutrality, adds ethanol 2000ml, cold preservation 24 hours, filter, filtrate decompression is concentrated into 250ml, adds water to 500ml, adds proper amount of active carbon, stir evenly, filter, it is 6.5～7.0 that filtrate is regulated pH value with 40% sodium hydroxide solution, adds the 10g polyoxyethylene sorbitan monoleate, the 1g sodium sulfite, fully stir evenly, filter, add the injection water to 1000ml, embedding, sterilization namely gets BAIHUASHESHECAO ZHUSHEYE.
BAIHUASHESHECAO ZHUSHEYE is the clear liquid of pale brown color.
Get BAIHUASHESHECAO ZHUSHEYE 30ml, be added on the polyamide column (50 orders, 2g, the internal diameter 12～15mm that have handled well, wet method dress post) on, uses the 50ml water elution, discard water liquid, use 70% ethanol elution, when yellow colour band flows out, begin to collect eluent 5ml, as need testing solution.Get need testing solution number droplet, put on filter paper, dry, Dropwise 5 % aluminum chloride alcoholic solution dries, and puts under the ultra-violet lamp (365nm) and observes, and shows yellow-green fluorescence.
Precision takes by weighing at the control substance of Rutin 10mg of 120 ℃ of drying under reduced pressure to constant weight, puts in the 50ml measuring bottle, adds an amount of 70% ethanol, put that slight fever makes dissolving in the water-bath, put coldly, add 70% ethanol to scale, shake up, namely get (containing anhydrous rutin 0.2mg among every 1ml) reference substance solution.
Precision is measured reference substance solution 0.0,1.0,2.0,3.0,4.0,5.0 and 6.0ml, puts respectively in the 25ml measuring bottle, respectively adds 70% ethanol to 6ml, add 5% sodium nitrite solution 1ml, shake up, placed 6 minutes, add 10% aluminum nitrate solution 1ml, shake up, placed 6 minutes, hydro-oxidation sodium test solution 10ml adds ethanol again to scale, shakes up, placed 15 minutes, and according to spectrophotography, measured trap at the wavelength place of 507nm, be that vertical coordinate, concentration are abscissa with the trap, the drawing standard curve.
Precision is measured BAIHUASHESHECAO ZHUSHEYE 10ml, is added on the polyamide column (50 orders, the 2g that have handled well, internal diameter 12～15mm, wet method dress post) on, use the 50ml water elution, discard eluent, use 70% ethanol elution, collect the about 25ml of eluent, put in the 25ml measuring bottle, add 70% ethanol dilution to scale, shake up, precision is measured 5ml respectively, puts first, in two 25ml measuring bottles of second, add 5% sodium nitrite solution 1ml in the first bottle, shake up, placed 6 minutes, and added 10% aluminum nitrate solution 1ml, shake up, placed 6 minutes, in first, each hydro-oxidation sodium test solution 10ml in two bottles of the second adds ethanol dilution again to scale, shakes up, placed 15 minutes, according to spectrophotography, be blank with the second bottle, measure trap at the wavelength place of 507nm, read the amount of rutin the BAIHUASHESHECAO ZHUSHEYE from standard curve, calculate.
The amount that contains total flavones in every milliliter of rutin in 8 parts of BAIHUASHESHECAO ZHUSHEYE is respectively 0.28,0.25,0.29,0.27,0.24,0.23,0.25 and 0.29mg.
Claims (3)
1. the preparation method of a BAIHUASHESHECAO ZHUSHEYE is characterized in that: the alcohol heating reflux extraction Herba Hedyotidis Diffusae with 60%, filtration, obtain ethanol extract and filtering residue, described filtering residue water extraction filters, obtain aqueous extract, described ethanol extract and described aqueous extract are merged, transfer pH to 12 with lime water, cold preservation filters, and it is 3 that filtrate is regulated pH value with 50% sulfuric acid solution, leave standstill, filter, filtrate reuse 40% sodium hydroxide solution transfers to neutrality, add ethanol, cold preservation filters, and filtrate adds proper amount of active carbon, stir, filter, it is 6.5～7.0 that filtrate is regulated pH value with 40% sodium hydroxide solution, adds Polysorbate and sodium sulfite, stir, filter, add the injection water, embedding, sterilization obtains BAIHUASHESHECAO ZHUSHEYE;
Wherein, described alcohol heating reflux extracts three times, and each extraction time was respectively 2,1 and 1 hours;
Described water extraction 2 times, each time of extracting is 2 and 1 hours.
2. the preparation method of BAIHUASHESHECAO ZHUSHEYE according to claim 1, it is characterized in that: it is 1.23-1.25 that described ethanol extract is concentrated into relative density.
3. the preparation method of BAIHUASHESHECAO ZHUSHEYE according to claim 2 is characterized in that: solution concentration to the relative density after described ethanol extract and described aqueous extract merge is 1.20-1.25.
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| CN103948717B (en) * | 2014-04-29 | 2016-06-01 | 江西天施康中药股份有限公司 | A kind of Herba Hedyotidis Diffusae injection and its preparation method |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1709355A (en) * | 2005-06-02 | 2005-12-21 | 王衡新 | Oldenlandia diffusa roxb injection agent, and its preparing method and quality control method |
| CN1799585A (en) * | 2005-09-13 | 2006-07-12 | 余世春 | Intravenous administered formulation of spreading hedyotis herb and its preparation method |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1709355A (en) * | 2005-06-02 | 2005-12-21 | 王衡新 | Oldenlandia diffusa roxb injection agent, and its preparing method and quality control method |
| CN1799585A (en) * | 2005-09-13 | 2006-07-12 | 余世春 | Intravenous administered formulation of spreading hedyotis herb and its preparation method |
Non-Patent Citations (2)
| Title |
|---|
| 梁仕声等.絮凝法制作白花蛇舌草注射液.《中国中药杂志》.2000,第25卷(第12期),756,757. |
| 絮凝法制作白花蛇舌草注射液;梁仕声等;《中国中药杂志》;20001231;第25卷(第12期);第756-757页，尤其是第757页4.1节 * |
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