CN102293805A - Total phenolic acid of ixeris sonchifolia (Bunge) hance, and preparation method - Google Patents
Total phenolic acid of ixeris sonchifolia (Bunge) hance, and preparation method Download PDFInfo
- Publication number
- CN102293805A CN102293805A CN 201110001528 CN201110001528A CN102293805A CN 102293805 A CN102293805 A CN 102293805A CN 201110001528 CN201110001528 CN 201110001528 CN 201110001528 A CN201110001528 A CN 201110001528A CN 102293805 A CN102293805 A CN 102293805A
- Authority
- CN
- China
- Prior art keywords
- phenolic acid
- total phenolic
- herba ixeritis
- ethanol
- ixeritis sonchifoliae
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Landscapes
- Medicines Containing Plant Substances (AREA)
- Acyclic And Carbocyclic Compounds In Medicinal Compositions (AREA)
Abstract
The invention relates to a preparation method for the total phenolic acid of ixeris sonchifolia (Bunge) hance. The preparation method comprises the following steps: crushing the medicinal material of the ixeris sonchifolia (Bunge) hance; adding 0.1-0.5% of a sodium bicarbonate solution adopted as a solvent to carry out percolation; collecting the percolation solution, wherein the volume of the percolation solution is 5-15 times the total volume of the ixeris sonchifolia (Bunge) hance and the sodium bicarbonate solution; adopting dilute sulfuric acid to adjust a pH value to 2-3; carrying out filtration and precipitation to provide a spare use; carrying out an elution treatment for the resulting filtrate through a polyamide column, firstly adopting the water to remove impurities, followed by adopting 90% ethanol to carry out the elution and collecting the ethanol eluent to provide a spare use, wherein the volume of the water is 1-5 times the total volume of the polyamide column, the volume of the collected ethanol eluent is 5-15 times the total volume of the polyamide column; adopting the 90% ethanol to carry out extraction for the precipitation for three times, wherein the volume of the 90% ethanol is 2-10 times the volume of the precipitation; then carrying out filtering, mixing the resulting filtrate and the collected ethanol eluent; recovering the ethanol at a temperature of 40-70 DEG C; carrying out vacuum concentration; adding a 4% sodium hydroxide solution to dissolve, then carrying out steps of filtering and drying to obtain the total phenolic acid of the ixeris sonchifolia (Bunge) hance. In the prior art, the phenolic acid compounds are easy to be deposed and deteriorated during the preparation process and the storage process. With the total phenolic acid injection of the ixeris sonchifolia (Bunge) hance provided by the present invention, the disadvantages in the prior art are overcome, the stabilities of the active ingredients are ensured, such that the quality and the efficacy of the total phenolic acid injection of the ixeris sonchifolia (Bunge) hance are ensured.
Description
Technical field
The present invention relates to total phenolic acid of a kind of Herba Ixeritis Sonchifoliae and preparation method thereof, the invention still further relates to the freeze-dried powder that contains the total phenolic acid of this Herba Ixeritis Sonchifoliae and preparation method thereof and method of quality control, belong to pharmaceutical field.
Background technology
Herba Ixeritis Sonchifoliae, be commonly called as Herba Ixeritis Sonchifoliae, magnitude all over the sky, 2 years living dry aerial parts for Compositae gutweed Lepidium Herba Ixeritis Sonchifoliae [Ixeris sonchifolia (Bge) Hance] have heat-clearing and toxic substances removing, the effect of blood-activating analgetic, clinical practice is comparatively extensive with KUDIEZI ZHUSHEYE.KUDIEZI ZHUSHEYE is made by the Herba Ixeritis Sonchifoliae single medicinal material, and main component has flavone, phenolic acid, adenosine, aminoacid etc., is used for the treatment of ischemic cardio cerebrovascular diseases such as coronary heart disease, angina pectoris and myocardial infarction.Research to this medicine in recent years has remarkable progress, but focuses mostly in flavone compound, and the independent research of the total phenolic acid compound of another effective site is not appeared in the newspapers.
Summary of the invention
Purpose of the present invention provides the preparation method of the total phenolic acid of a kind of Herba Ixeritis Sonchifoliae.
Another object of the present invention provides the preparation method of the total phenolic acid lyophilized injectable powder of this Herba Ixeritis Sonchifoliae and the method for quality control of lyophilized injection.
The technical scheme that adopts is:
The preparation method of the total phenolic acid of a kind of Herba Ixeritis Sonchifoliae comprises following processing step:
1, the sodium bicarbonate solution that adds 0.1%-0.5% after the Herba Ixeritis Sonchifoliae pulverizing medicinal materials is carried out percolation as solvent, collect the percolate that 10-15 doubly measures, regulate pH value to 2-3, filter, precipitate standby with dilute sulfuric acid;
2, the filtrate that step 1 is obtained, is continued and used 90% ethanol elution earlier with 1-5 times of water gaging flush away impurity by polyamide column, collects 5-15 and doubly measures ethanol elution, and is standby;
3, the precipitation that step 1 is obtained is doubly measured 90% ethanol extraction 3 times with 2-10, filters, and filtrate and step 2 gained ethanol liquid merge, and 40-70 ℃ is reclaimed ethanol, and concentrating under reduced pressure adds 4% sodium hydroxide solution and makes dissolving, filters, and drying promptly gets the total phenolic acid of Herba Ixeritis Sonchifoliae.
The present invention adopts the weak base percolation just to carry, cross the polyamide column remove impurity, the method that the high concentration ethanol essence is carried, promptly adopt the low concentration weak base composition that acidity is stronger such as phenolic acid, tannin etc. to extract selectively, in the research, the sodium carbonate of variable concentrations and sodium bicarbonate are compared respectively as extracting solvent, and the result shows, and is most effective and impurities is minimum as solvent extraction with the sodium bicarbonate of 0.2%-0.5%; In order to keep the stable of Herba Ixeritis Sonchifoliae phenolic acid compound, avoid liposoluble ingredient that oxidative degradation at high temperature takes place, adopt percolation to extract; Because alkaline extraction may be brought tannin class impurity into, and tannin adsorptivity on polyamide column is very strong, need so polyamide column is carried out eluting, just when effective ingredient is eluted, tannin to be removed with 90% ethanol with highly basic ability flush away; Adopt high concentration alcohol that free total phenols acid treating is come out at last.The content height of the total phenolic acid of Herba Ixeritis Sonchifoliae in the final extract of this law gained, impurity is few, and its total phenolic content is more than 80%, and physiologically active is strong, and technical process is simple, safety is controlled, lays a good foundation for the total phenolic acid of gained Herba Ixeritis Sonchifoliae is applied to various preparations.
The total phenolic acid of the Herba Ixeritis Sonchifoliae that utilizes the inventive method to obtain can be used for preparing said preparation on any pharmaceutics.For example, be used for to make corresponding tablet, forms such as granule or capsule when oral; Can also make the forms such as solution of injectable powder, injection.
The invention still further relates to the preparation method of the total phenolic acid injectable powder of Herba Ixeritis Sonchifoliae; its technical essential is to get the total phenolic acid of Herba Ixeritis Sonchifoliae, adds an amount of water for injection and makes dissolving, regulates pH value to 7.0 with 10% sodium hydroxide solution; add proppant mannitol; addition is 1:0.1-1 in weight ratio Herba Ixeritis Sonchifoliae total phenols acid ratio mannitol, adds protective agent sodium thiosulfate again, and addition is 0.1-1% by weight percentage; and proper amount of water for injection; add the 5g active carbon in every 1000ml solution, regulate pH value to 7.0, being heated to boils and keep little boiled 15 minutes; cooling; filter, sterilization filters; fill; lyophilization, gland, promptly.
The total phenolic acid injectable powder of Herba Ixeritis Sonchifoliae that makes with the inventive method has overcome phenolic acid compound and easily decomposed rotten defective in preparation and storage process, guarantee the stability of effective ingredient, thereby guaranteed the quality and the curative effect of the total phenolic acid injectable powder of Herba Ixeritis Sonchifoliae.
The specific embodiment
Embodiment one
The preparation method of the total phenolic acid of a kind of Herba Ixeritis Sonchifoliae comprises following processing step:
1, the Herba Ixeritis Sonchifoliae pulverizing medicinal materials is become add 0.5% sodium bicarbonate solution behind the long segment of 10cm and carry out percolation, collect the percolate of 10 times of amounts, regulate pH value to 2.0, filter, precipitate standby with dilute sulfuric acid as solvent;
2, the filtrate that step 1 is obtained, is continued and used 90% ethanol elution earlier with 5 times of water gaging flush away impurity by polyamide column, collects 8 times of amount ethanol elution, and is standby;
3, the precipitation that step 1 is obtained is measured 90% ethanol extractions 3 times with 5 times, filters, and filtrate and step 2 gained ethanol liquid merge, and 50 ℃ are reclaimed ethanol, and concentrating under reduced pressure adds 4% sodium hydroxide solution and makes dissolving, filters, and drying promptly gets the total phenolic acid 108g of Herba Ixeritis Sonchifoliae.
Embodiment two
The preparation method of the total phenolic acid of a kind of Herba Ixeritis Sonchifoliae comprises following processing step:
1, the Herba Ixeritis Sonchifoliae pulverizing medicinal materials is become add 0.3% sodium bicarbonate solution behind the long segment of 12cm and carry out percolation, collect the percolate of 12 times of amounts, regulate pH value to 2.5, filter, precipitate standby with dilute sulfuric acid as solvent;
2, the filtrate that step 1 is obtained, is continued and used 90% ethanol elution earlier with 8 times of water gaging flush away impurity by polyamide column, collects 10 times of amount ethanol elution, and is standby;
3, the precipitation that step 1 is obtained is measured 90% ethanol extractions 3 times with 8 times, filters, and filtrate and step 2 gained ethanol liquid merge, and 55 ℃ are reclaimed ethanol, and concentrating under reduced pressure adds 4% sodium hydroxide solution and makes dissolving, filters, and drying promptly gets the total phenolic acid 113g of Herba Ixeritis Sonchifoliae.
Embodiment three
The preparation method of the total phenolic acid of a kind of Herba Ixeritis Sonchifoliae comprises following processing step:
1, the Herba Ixeritis Sonchifoliae pulverizing medicinal materials is become add 0.2% sodium bicarbonate solution behind the long segment of 15cm and carry out percolation, collect the percolate of 15 times of amounts, regulate pH value to 3, filter, precipitate standby with dilute sulfuric acid as solvent;
2, the filtrate that step 1 is obtained, is continued and used 90% ethanol elution earlier with 10 times of water gaging flush away impurity by polyamide column, collects 15 times of amount ethanol elution, and is standby;
3, the precipitation that step 1 is obtained is measured 90% ethanol extractions 3 times with 10 times, filters, and filtrate and step 2 gained ethanol liquid merge, and 60 ℃ are reclaimed ethanol, and concentrating under reduced pressure adds 4% sodium hydroxide solution and makes dissolving, filters, and drying promptly gets the total phenolic acid 115g of Herba Ixeritis Sonchifoliae.
Embodiment four
The preparation method of the total phenolic acid of a kind of Herba Ixeritis Sonchifoliae comprises following processing step:
Get the total phenolic acid 20g of Herba Ixeritis Sonchifoliae, add an amount of water for injection and make dissolving, regulate pH value to 7.0 with 10% sodium hydroxide solution; add proppant mannitol 4g, add protective agent sodium thiosulfate 0.1g again, and proper amount of water for injection; add the 5g active carbon in every 1000ml solution, regulate pH value to 7.0, being heated to boils and keep little boiled 15 minutes; cooling filters, sterilization; filter fill, lyophilization; gland can obtain 1000 injection lyophilized powders.
The content assaying method of total phenolic acid in the Herba Ixeritis Sonchifoliae injection freeze-dried powder
The present invention adopts ultraviolet spectrophotometry that total phenolic acid is carried out assay, through methodology verify this method accurately and reliably, simple and easy to do.Be that reference substance is investigated with caffeic acid, chicoric acid and taraxacin B respectively, the maximum absorption wavelength of taraxacin B is consistent with need testing solution and content is the highest as a result, is reference substance so select taraxacin B for use.In investigating, linear relationship finds that standard curve is through initial point, so adopt the reference substance relative method as the cubage method.Concrete grammar is as follows:
The preparation of reference substance solution
Get the about 8mg of taraxacin B reference substance, the accurate title, decide, and puts in the 10ml measuring bottle, adds 50% ethanol to scale, shakes up; Precision is measured 1ml, puts the 100ml measuring bottle, adds 50% ethanol to scale, shakes up, promptly.
This product 10mg is got in the preparation of need testing solution, and accurate the title decides, and adds water 5ml and makes dissolving, the AB-8 type macroporous resin column of having handled well by 15g, with water elution, the 100ml measuring bottle is collected eluent to scale, shakes up, precision is measured 1ml, to the 10ml measuring bottle, add dehydrated alcohol 5ml, add water to scale again, shake up, promptly.
Algoscopy
Get reference substance solution and need testing solution respectively, measure absorbance at 328nm wavelength place, press reference substance relative method calculation sample content.
The content assaying method of taraxacin B in the Herba Ixeritis Sonchifoliae injection freeze-dried powder
For further controlling product quality, the present invention adopts high performance liquid chromatography that the taraxacin B that content is the highest in total phenolic acid is carried out assay.
Chromatographic condition and system suitability test: with octadecylsilane chemically bonded silica is filler; Acetonitrile-0.4% phosphoric acid solution (20:80) is a mobile phase; The detection wavelength is 328nm; Number of theoretical plate should be not less than 5000 with taraxacin B peak compute;
It is an amount of that the preparation precision of reference substance solution takes by weighing taraxacin B reference substance, adds 50% ethanol and make the solution that every 1ml contains 0.1mg, shakes up, promptly;
This product 50mg is got in the need testing solution preparation, and accurate the title decides, and puts in the 100ml measuring bottle, adds 50% ethanol to scale, shakes up, promptly;
Algoscopy: accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, promptly.
The pharmacodynamics test of the total phenolic acid of Herba Ixeritis Sonchifoliae and toxicity test
The total phenolic acid of the Herba Ixeritis Sonchifoliae that utilizes the inventive method to make is steady quality not only, and be rich in the active component of Chinese medicine Herba Ixeritis Sonchifoliae, have pharmacological actions such as excellent anti-hemocyte is assembled, resisted myocardial ischemia, anoxia, therefore can be used for preparing good effect, the medicine of safe and reliable control cardiovascular and cerebrovascular disease.The pharmacodynamics test of the total phenolic acid of following Herba Ixeritis Sonchifoliae has proved that fully total phenolic acid of Herba Ixeritis Sonchifoliae and injectable powder thereof have good pharmacological action.
The total phenolic acid injectable powder of total phenolic acid of experimental example 1 Herba Ixeritis Sonchifoliae and Herba Ixeritis Sonchifoliae is to the influence of rat serum blood stasis syndrome model hemocyte aggregation
Adopt and inject epinephrine repeatedly and impose the method making stasis syndrome card rat model that frozen water soaks, with indexs such as whole blood viscosity and erythrocyte aggregation indexs, with turbidimetry for Determination platelet maximum agglutination rate, the result is as follows.
(1) to the influence of rat acute blood stasis model whole blood viscosity
The high, medium and low k value of cutting of stasis syndrome model group and its whole blood of normal control group comparison all obviously raises, and shows that abnormal change appears in the hemorheology status of rat model, prompting rat acute syndrome of blood stasis modeling success.The result is as shown in table 4, the total phenolic acid 10 of Herba Ixeritis Sonchifoliae, the 20mg/kg that adopt embodiment 1 to obtain, the total phenolic acid injectable powder 13.5 of the Herba Ixeritis Sonchifoliae that embodiment 4 obtains, 27mg/kg, all can obviously reduce the whole blood viscosity value of stasis syndrome rat, compare with model group, there were significant differences, shows the effect of the stasis syndrome rat model whole blood viscosity that has clear improvement.The total phenolic acid 10mg/kg of Herba Ixeritis Sonchifoliae, Herba Ixeritis Sonchifoliae total phenolic acid injectable powder 13.5mg/kg and KUDIEZI ZHUSHEYE 1g/kg effect are suitable.
Table 1
To the influence of stasis syndrome rat model whole blood viscosity (
x±
S, n=6)
| Group | Dosage (mg/kg) | Height is cut | In cut | Low cutting |
| Matched group | ? | 6.91 ±0.82 | 8.41 ±0.74 | 17.75 ±3.34 |
| Model group | ? | 9.09 ±1.28 | 11.29 ±1.60 | 21.91 ±1.89 |
| ZFS | 10 | 7.21 ±1.10 * | 8.61 ±1.24 * | 18.16 ±2.24 * |
| ? | 20 | 6.72 ±0.99 * | 7.76 ±1.18 * | 15.64 ±2.09 * |
| ZFSFJ | 12 | 7.15 ±0.96 * | 8.47 ±1.16 * | 18.95 ±2.59 * |
| ? | 24 | 6.63 ±1.03 * | 7.97 ±1.07 * | 15.16 ±2.03 * |
| KDZ | 1000 | 7.03 ±1.15 * | 8.19 ±1.08 * | 17.26 ±2.15 * |
Annotate: compare * with model group
P＜0.01;
(2) to the influence of rat acute blood stasis model erythrocyte aggregation
The erythrocyte electrophoretic time of syndrome of blood stasis model group and the apparent in view prolongation of normal control group, other indexs such as erythrocyte aggregation index, deformable index, rigidity index, packed cell volume more all have certain rising trend with matched group respectively.Adopt the total phenolic acid 10 of Herba Ixeritis Sonchifoliae, 20mg/kg, the total phenolic acid injectable powder 13.5 of Herba Ixeritis Sonchifoliae, 27mg/kg, unusual erythrocyte aggregation index, deformable index and the rigidity index that raises of syndrome of blood stasis rat all had significant reduction effect, compare with model group, there were significant differences.The total phenolic acid 10mg/kg of Herba Ixeritis Sonchifoliae, Herba Ixeritis Sonchifoliae total phenolic acid injectable powder 13.5mg/kg and KUDIEZI ZHUSHEYE 1g/kg effect are suitable.
Table 2
To the influence of the erythrocyte aggregation of rat acute blood stasis model (
x±
S, n=6)
| Group | Dosage (mg/kg) | Erythrocyte aggregation index | Deformable index | Rigidity index | Packed cell volume |
| Matched group | ? | 12.64 ±3.18 | 0.92 ±0.05 | 7.55±1.86 | 0.50 ±0.02 |
| Model group | ? | 13.07 ±2.53 | 0.99 ±0.14 | 8.66 ±2.17 | 0.52 ±0.05 |
| ZFS | 10 | 11.34 ±2.15 * | 0.86 ±0.11 | 6.68 ±1.35 * | 0.50 ±0.04 |
| ? | 20 | 8.92 ±1.56 ** | 0.81 ±0.15 * | 5.55 ±1.42 * | 0.52 ±0.04 |
| ZFSFJ | 12 | 11.57 ±2.24 * | 0.87 ±0.17 | 6.75 ±1.29 * | 0.50 ±0.04 |
| ? | 24 | 9.04 ±1.65 ** | 0.80 ±0.09 * | 5.63 ±1.45 * | 0.52 ±0.04 |
| KDZ | 1000 | 10.91 ±1.92 * | 0.85 ±0.18 | 6.62 ±1.34 * | 0.50 ±0.04 |
Annotate: compare * * with model group
P＜0.01, *
P＜0.05
(3) to the influence of rat acute blood stasis model platelet aggregation
The platelet maximum agglutination rate of stasis syndrome model group and normal control group compare, and its rising effect has statistical significance.Adopt the total phenolic acid 10 of Herba Ixeritis Sonchifoliae, 20mg/kg, the total phenolic acid injectable powder 13.5 of Herba Ixeritis Sonchifoliae, 27mg/kg all can significantly reduce the platelet maximum agglutination rate of stasis syndrome rat model, with model group relatively, there were significant differences.Prompting total phenolic acid of Herba Ixeritis Sonchifoliae and the total phenolic acid injectable powder of Herba Ixeritis Sonchifoliae have tangible preventive and therapeutic effect to the platelet aggregation that the stasis syndrome card increases unusually.The total phenolic acid 10mg/kg of Herba Ixeritis Sonchifoliae, Herba Ixeritis Sonchifoliae total phenolic acid injectable powder 13.5mg/kg and KUDIEZI ZHUSHEYE 1g/kg effect are suitable.See Table 3.
Table 3
To the influence of stasis syndrome rat model platelet aggregation (
x±
S, n=6)
| Group | Dosage (mg/kg) | The platelet maximum agglutination rate | Platelet aggregation inhibition rate (%) |
| Matched group | ? | 19.25 ±9.14 | ? |
| Model group | ? | 41.14 ±15.64 | ? |
| ZFS | 10 | 24.05 ±9.81 * | 44.54 |
| ? | 20 | 20.04 ±8.64 * | 51.29 |
| ZFSFJ | 12 | 23.96 ±9.08 * | 44.76 |
| ? | 24 | 20.17 ±8.42 * | 50.97 |
| KDZ | 1000 | 23.08 ±9.41 * | 43.90 |
Annotate: compare * with model group
P＜0.05
The total phenolic acid injectable powder of total phenolic acid of experimental example 2 Herba Ixeritis Sonchifoliaes and Herba Ixeritis Sonchifoliae is to the influence of mouse cardiac muscle nutrient flow amount
Absorb with mouse cardiac muscle
86Rb ability size is an index, observes the influence to the myocardial nutrition blood flow of total phenolic acid of Herba Ixeritis Sonchifoliae (ZFS) and the total phenolic acid injectable powder of Herba Ixeritis Sonchifoliae (ZFSFJ).Under certain condition, myocardial flow is big more, and its intake is also big more, and blood flow is right with cardiac muscle
86The intake of Rb is proportional.So mouse cardiac muscle is right
86The size of the picked-up ability of Rb can reflect the variation of mouse cardiac muscle blood flow under the whole condition.
As shown in table 4, adopt the total phenolic acid 10 of Herba Ixeritis Sonchifoliae, 20mg/kg, the total phenolic acid injectable powder 13.5 of Herba Ixeritis Sonchifoliae, 27mg/kg can significantly increase the cardiac muscle picked-up
86The Rb effect is compared with matched group, and there were significant differences.Show that total phenolic acid and injectable powder thereof all can significantly increase the myocardial nutritional flow amount, improve because the symptoms such as angina pectoris that myocardial ischemia causes.The total phenolic acid 20mg/kg of Herba Ixeritis Sonchifoliae, Herba Ixeritis Sonchifoliae total phenolic acid injectable powder 27mg/kg and KUDIEZI ZHUSHEYE 1g/kg effect are suitable.
The influence (n=10) of table 4 pair mouse cardiac muscle nutrient flow amount
| Group | Dosage (mg/kg) | Cardiac muscle uptake ratio (%) | Increase and decrease percentage rate (%) |
| Matched group | ? | 2.29 | ? |
| ZFS | 10 | 2.63 * | 14.85 |
| ? | 20 | 2.80 ** | 22.27 |
| ZFSFJ | 12 | 2.61 * | 13.97 |
| ? | 24 | 2.78 ** | 21.40 |
| KDZ | 1000 | 2.79 ** | 21.83 |
Annotate: compare * * with model group
P＜0.01, *
P＜0.05
The total phenolic acid injectable powder of total phenolic acid of experimental example 3 Herba Ixeritis Sonchifoliaes and Herba Ixeritis Sonchifoliae increases the influence of myocardial oxygen consumption to isoproterenol
As shown in table 5, adopt the total phenolic acid 10 of Herba Ixeritis Sonchifoliae, 20mg/kg, the total phenolic acid injectable powder 13.5 of Herba Ixeritis Sonchifoliae, 27mg/kg can obviously resist the effect that isoproterenol increases myocardial oxygen consumption.Compare with model group, there were significant differences.Prompting total phenolic acid of Herba Ixeritis Sonchifoliae and the total phenolic acid injectable powder of Herba Ixeritis Sonchifoliae have significant protective effect to myocardial ischemia.The total phenolic acid 10mg/kg of Herba Ixeritis Sonchifoliae, Herba Ixeritis Sonchifoliae total phenolic acid injectable powder 13.5mg/kg and KUDIEZI ZHUSHEYE 1g/kg effect are suitable.
Table 5 pair isoproterenol increases the influence (n=10) of myocardial oxygen consumption
| Group | Dosage (mg/kg) | Consumption rate (L/h*m 2Body surface) | Increase and decrease percentage rate (%) |
| Matched group | ? | 41.54 ±12.58 | ? |
| Model group | ? | 52.25 ±18.64 | ? |
| ZFS | 10 | 40.25 ±10.51 * | -22.97 |
| ? | 20 | 32.55 ±9.48 ** | -37.70 |
| ZFSFJ | 12 | 40.94 ±11.08 * | -21.65 |
| ? | 24 | 31.95 ±10.24 ** | -38.85 |
| KDZ | 1000 | 39.25 ±10.51 * | -24.88 |
Annotate: compare * * with model group
P＜0.01, *
P＜0.05
The toxicity test of the total phenolic acid of experimental example 4 Herba Ixeritis Sonchifoliaes
Acute toxicity: mouse mainline median lethal dose(LD 50) (LD50) is 2171.62mg/kg; Lumbar injection median lethal dose(LD 50) (LD50) is 2150.25mg/kg.The long term toxicity safe dose of rat and Canis familiaris L. is respectively 80mg/kg and 50mg/kg.As seen the toxicity of the total phenolic acid of Herba Ixeritis Sonchifoliae is very little.
Claims (4)
1. the preparation method of the total phenolic acid of Herba Ixeritis Sonchifoliae is characterized in that comprising following processing step:
Carry out percolation with adding 0.1% ~ 0.5% sodium bicarbonate solution after the Herba Ixeritis Sonchifoliae pulverizing medicinal materials as solvent, collect the percolate of 5 ~ 15 times of amounts, regulate pH value to 2 ~ 3, filter, precipitate standby with dilute sulfuric acid; Filtrate, is continued and used 90% ethanol elution earlier with 1 ~ 5 times of water gaging flush away impurity by polyamide column, collects 5 ~ 15 times of amount ethanol elution, and is standby; Above-mentioned precipitation is measured 90% ethanol extractions 3 times with 2 ~ 10 times, filters, and filtrate and above-mentioned ethanol liquid merge, and 40 ~ 70 ℃ are reclaimed ethanol, and concentrating under reduced pressure adds 4% sodium hydroxide solution and makes dissolving, filters, and drying promptly gets the total phenolic acid of Herba Ixeritis Sonchifoliae; The total phenolic acid of Herba Ixeritis Sonchifoliae is no less than 16% by weight percentage.
2. the preparation method of the total phenolic acid of Herba Ixeritis Sonchifoliae according to claim 1 is characterized in that the total phenolic acid of the Herba Ixeritis Sonchifoliae that is prepared into can make the injection freeze-dried powder, contains the total phenolic acid of Herba Ixeritis Sonchifoliae and is no less than 80%.
3. according to the injection freeze-dried powder of the total phenolic acid of the described Herba Ixeritis Sonchifoliae of claim 2, it is characterized in that preparation method comprises the following steps:
Get the total phenolic acid of Herba Ixeritis Sonchifoliae; add an amount of water for injection and make dissolving; regulate pH value to 7.0 with 10% sodium hydroxide solution, add proppant mannitol, addition is 1:0.1-1 in weight ratio Herba Ixeritis Sonchifoliae total phenols acid ratio mannitol; add protective agent sodium thiosulfate again; addition is 0.1-1% by weight percentage, and proper amount of water for injection, adds the 5g active carbon in every 1000ml solution; regulate pH value to 7.0; be heated to and boil and kept 15 minutes, cooling filters; sterilization; filter fill, lyophilization; gland, promptly.
4. the preparation method of the total phenolic acid of Herba Ixeritis Sonchifoliae according to claim 2 is characterized in that the total phenols acidity test method of the injection freeze-dried powder that is prepared into comprising following processing step:
A. the preparation of reference substance solution
Get taraxacin B reference substance 8mg, the accurate title, decide, and puts in the 10ml measuring bottle, adds 50% ethanol to scale, shakes up; Precision is measured 1ml, puts the 100ml measuring bottle, adds 50% ethanol to scale, shakes up, promptly;
B. the preparation of need testing solution
Get this product 10mg, accurate claim surely, add water 5ml and make dissolving, the AB-8 type macroporous resin column of having handled well by 15g is with water elution, the 100ml measuring bottle is collected eluent to scale, shakes up, and precision is measured 1ml, to the 10ml measuring bottle, add dehydrated alcohol 5ml, add water to scale again, shake up, promptly;
C. algoscopy
Get reference substance solution and need testing solution respectively, measure absorbance at 328nm wavelength place, press reference substance relative method calculation sample content.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110001528 CN102293805B (en) | 2011-01-06 | 2011-01-06 | Total phenolic acid of ixeris sonchifolia (Bunge) hance, and preparation method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110001528 CN102293805B (en) | 2011-01-06 | 2011-01-06 | Total phenolic acid of ixeris sonchifolia (Bunge) hance, and preparation method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102293805A true CN102293805A (en) | 2011-12-28 |
| CN102293805B CN102293805B (en) | 2013-04-17 |
Family
ID=45354641
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 201110001528 Active CN102293805B (en) | 2011-01-06 | 2011-01-06 | Total phenolic acid of ixeris sonchifolia (Bunge) hance, and preparation method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102293805B (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2003090767A1 (en) * | 2002-04-23 | 2003-11-06 | Wang, Maoxiang | An injection made from ixeris sonchifolia for treatment of cardio-cerebral vascular disease and fundus diseases and method of producing thereof |
| CN1634395A (en) * | 2004-10-15 | 2005-07-06 | 张平 | Freeze dried injection of seeding of autumnal sowthistle-leaf ixeris and preparation method thereof |
| CN1817351A (en) * | 2005-02-07 | 2006-08-16 | 中国科学院上海药物研究所 | Production of variolaria amra medicinal extract and its medicinal preparation |
| CN1872122A (en) * | 2006-04-29 | 2006-12-06 | 沈阳斯佳科技发展有限公司 | Method for preparing freeze-dry powder and injection preparation of Kudiezi |
| CN101524387A (en) * | 2009-04-21 | 2009-09-09 | 沈阳双鼎制药有限公司 | Ixeri sonhifolia injection preparing technology and application thereof for treating cardiovascular and cerebrovascular disease |
-
2011
- 2011-01-06 CN CN 201110001528 patent/CN102293805B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2003090767A1 (en) * | 2002-04-23 | 2003-11-06 | Wang, Maoxiang | An injection made from ixeris sonchifolia for treatment of cardio-cerebral vascular disease and fundus diseases and method of producing thereof |
| CN1634395A (en) * | 2004-10-15 | 2005-07-06 | 张平 | Freeze dried injection of seeding of autumnal sowthistle-leaf ixeris and preparation method thereof |
| CN1817351A (en) * | 2005-02-07 | 2006-08-16 | 中国科学院上海药物研究所 | Production of variolaria amra medicinal extract and its medicinal preparation |
| CN1872122A (en) * | 2006-04-29 | 2006-12-06 | 沈阳斯佳科技发展有限公司 | Method for preparing freeze-dry powder and injection preparation of Kudiezi |
| CN101524387A (en) * | 2009-04-21 | 2009-09-09 | 沈阳双鼎制药有限公司 | Ixeri sonhifolia injection preparing technology and application thereof for treating cardiovascular and cerebrovascular disease |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102293805B (en) | 2013-04-17 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101057890B (en) | Traditional Chinese medicinal composition for treating coronary heart disease and its preparation method, preparations and its application | |
| CN101502549B (en) | Notoginsen triterpenes capsule as well as preparation method thereof and method for measuring content | |
| CN102805767B (en) | Heat stranguria removal granule raw material polygonum capitatum extract with anti-gonococcus effect | |
| CN101306134B (en) | Compound Nanxing pain paste and cataplasm combination and its preparation method | |
| CN101224246B (en) | Preparing method of loquat leaf total triterpenic acid and antidiabetic use thereof | |
| CN101375935A (en) | Method for extracting and determining Chinese medicine Schisandra chinensis | |
| CN100502880C (en) | Notoginseng glycol-saponin composition and its preparation method and use | |
| CN112159451A (en) | Gynostemma pentaphylla saponin extract and preparation method thereof | |
| CN102846704B (en) | A Leonurus japonicus injection, its preparation method, and method for detecting total alkaloids | |
| CN102293805B (en) | Total phenolic acid of ixeris sonchifolia (Bunge) hance, and preparation method | |
| CN102327324B (en) | Mulberry leaf total alkali extract and preparation method and application thereof | |
| CN101618069B (en) | Capsule preparation for treating bruise as well as bleeding and easing pain and preparation method and use thereof | |
| CN1943647B (en) | The method for preparing triterpenic acid extract from the loquat leaves | |
| CN110568120B (en) | Loranthus parasiticus quality control method based on double-substance components | |
| CN107693597B (en) | Traditional Chinese medicine composition for resisting myocardial ischemia and preparation method and application thereof | |
| CN101912565B (en) | Turmeric and astragalus capsules for treating diabetes and incipient diabetic nephropathy | |
| CN101744859B (en) | Pharmaceutical composition for promoting blood circulation, removing blood stasis and relieving pain and preparation method thereof | |
| CN104546952A (en) | Active component of selaginella doederleinii hieron as well as preparation method and use thereof | |
| CN105377280B (en) | A kind of drug and preparation method thereof for enriching blood | |
| CN108159109A (en) | Radix Astragali flavone extract is preparing the application in treating Neuroleptic Leukocytopenia disease drug | |
| CN101244220A (en) | Black thorn chinaroot greenbrier total saponin extract and preparation thereof | |
| CN1824005A (en) | Compound wurenchun capsule fortreating organizing and chronic hepatitis | |
| CN102526151B (en) | Medicinal composition and application thereof | |
| CN103127214A (en) | Folium orthosiphoni effective part for treating diabetic nephropathy and preparation method | |
| CN104288658A (en) | Preparation method of fomes officinalis cough and asthma treating tablets and application of fomes officinalis cough and asthma treating tablets in preparation of medicine for inhibiting cell proliferation of mouse myeloma cell SP2/0 |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |