CN1810270B - Preparation process of total salvianolic acid - Google Patents
Preparation process of total salvianolic acid Download PDFInfo
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- CN1810270B CN1810270B CN 200510020270 CN200510020270A CN1810270B CN 1810270 B CN1810270 B CN 1810270B CN 200510020270 CN200510020270 CN 200510020270 CN 200510020270 A CN200510020270 A CN 200510020270A CN 1810270 B CN1810270 B CN 1810270B
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- salviae miltiorrhizae
- radix salviae
- salvianolic acid
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Abstract
The present invention discloses preparation process and use of total salvianolic acid. The preparation process includes soaking red sage in cold water, percolating extraction, macroporous resin adsorption of the percolate, elution, decompression concentrating the eluted liquid, and drying to obtain total salvianolic acid. The preparation process is simple, high in yield, low in power consumption, safe, pollution-less and easy to industrialize. The obtained total salvianolic acid is used as medicine for preventing and treating cardiac and cerebral vascular diseases, etc.
Description
Technical field
The present invention relates to a kind of preparation method of Chinese medicine extract, specifically, relate to from salviamiltiorrhizabung, extract the method for Radix Salviae Miltiorrhizae total phenolic acids, belong to medical technical field,
Background technology
Radix Salviae Miltiorrhizae is the dry root and rhizome of labiate Radix Salviae Miltiorrhizae salviz miltiorrhiza Bge., has the effect that blood circulation promoting and blood stasis dispelling, removing heat from blood eliminating carbuncle, relieving restlessness are calmed the nerves.Modern pharmacological research confirms that Radix Salviae Miltiorrhizae has blood vessel dilating, microcirculation improvement, increase myocardial oxygen delivery amount and effects such as amount of blood supply, reduction myocardial oxygen consumption.Radix Salviae Miltiorrhizae mainly contains water solublity and fat-soluble two big constituents.Liposoluble constituent is to be the quinones of representative with the TANSHINONES, has tangible antiinflammatory action; Water soluble ingredient is to be the liposoluble ingredient of representative with the protocatechualdehyde, is the main component of treatment cardiovascular system diseases.(Fu Zhijun etc. concentrate, make with extra care and dry influence to water soluble ingredient in the compound Salviae Miltiorrhizae extracting solution. Anhui Chinese Medicine College journal, 2003,22 (2): 52～54)
At present more the soluble salvianolic acid constituents of Radix Salviae Miltiorrhizae adopts water extract-alcohol precipitation, water to carry the back and crosses that resin is crossed macroporous resin (Chinese patent CN 1384090A) or polyamide column (Chinese patent CN 1242364A) behind precipitate with ethanol (Chinese patent CN 1129572A), the water extract-alcohol precipitation again, water is carried the back successively with polyamide column and macroporous resin chromatography (Chinese patent CN 1459448A), and methods such as decompression or lyophilization obtain then.But above method prepares Radix Salviae Miltiorrhizae total phenolic acids and all has some problems, has influence on the yield of industrialization and finished product.At first, majority has adopted decocting to boil or the method for long-time heating (50～60 ℃) is extracted in the above method, and salvianolic acid is a polyhydric phenols structure, and the very easily oxidative degradation of being heated loses curative effect, thereby has a strong impact on the quality and the curative effect of product; Secondly, most extracting method adopt high concentration ethanol to precipitate this step, and the industrialization production security is reduced greatly, and the ethanol consumption is big, the production cost height; The 3rd, when said method extracts, need a large amount of condensed water, be not easy to industrialized great production, operation is comparatively complicated; The 4th, it is lower that said method extracts the salvianolic acid productive rate that obtains, and generally 2～4%, low productive rate also makes industrial production cost strengthen, and brings difficulty.
Summary of the invention
Technical scheme of the present invention has provided a kind of extracting method of Radix Salviae Miltiorrhizae total phenolic acids, and the present invention also provides the pharmaceutical composition that contains the Radix Salviae Miltiorrhizae total phenolic acids extract.
The present invention is implemented by the following technical programs:
A, Radix Salviae Miltiorrhizae decontamination, steam is softening, is chopped into decoction pieces;
B, salvia piece, the cold water dipping extracts with percolation, collects percolate;
C, percolate are centrifugal, get supernatant by macroporous adsorbent resin, and eluting washes with water earlier then, and the reuse ethanol elution is collected ethanol elution;
D, eluent concentrating under reduced pressure, be drying to obtain.
Wherein, in the step (a), cold water (10～25 ℃) dip time is 6～24 hours, and the percolation time is 12～24 hours.
In the step (b), macroporous adsorbent resin is a styrene type, salvianolic acid B in the upper prop medicinal liquid: resin (weight ratio)=1: 40～50, during eluting, the water elution volume is 1～5 times of resin, and the ethanol volume is 2～5 times of resin, flow speed control 1～3 times of volume/hour.Ethanol elution concentration is 30～95%.
In the step (c), baking temperature is 50～70 ℃.
Preferably, in the step (a), the cold water dip time is 6 hours, and the percolation time is 24 hours.
Macroporous adsorbent resin is HPD100, salvianolic acid B in the upper prop medicinal liquid: resin (weight ratio)=1: 40, add the water elution volume during eluting and be 1～1.5 times of resin, the ethanol volume is 4 times of resin, flow speed control 1～1.5 times of volume/hour.Ethanol elution concentration is 70～95%.Consider from the angle of suitability for industrialized production, use 70% ethanol elution, can make cost reduce production safety.
All parameters in each step of the invention described above technical scheme comprise that dip time, percolation speed and time, macroporous resin model, effluent volume, concentration of alcohol, baking temperature are by orthogonal experiment screening gained optimum condition.
According to the Radix Salviae Miltiorrhizae total phenolic acids that method of the present invention is made, can be made into said dosage form on any pharmaceutics.As be used for forms such as oral tablet, capsule or granule, the injectable powder that is used to inject, injection etc.Also can cooperate other medicines or component to make preparation together uses.
When the Radix Salviae Miltiorrhizae total phenolic acids that utilizes the inventive method to obtain prepares the various dosage form of required medicine, can be according to the conventional production method preparation of pharmaceutical field.The Radix Salviae Miltiorrhizae total phenolic acids that for example utilizes the inventive method to obtain mixes with one or more pharmaceutically acceptable carriers, makes corresponding dosage forms then.
The present invention compared with prior art has following advantage and characteristics:
1, step simple, easy to operate, be easy to industrialization.The present invention has overcome the defective that needs a large amount of condensed water, high concentration ethanol in the prior art, has simplified production stage, has optimized working condition, and energy consumption reduces greatly, and is free from environmental pollution, makes industrialization produce easier realization.
2, loss of effective components is few, finished product yield height.The present invention has avoided in the prior art causing the phenolic acid loss of active ingredients because of heating and precipitate with ethanol, and stability increases greatly, and the raising of finished product yield is generally more than 5%, apparently higher than the method that prior art adopted.
3, cost is low.Based on the advantage of above-mentioned two aspects, production cost adopts other method to prepare Radix Salviae Miltiorrhizae total phenolic acids to reduce greatly, for the patient has brought more interests, also brought economic benefit for society more at present during industrialization of the present invention.
Mode by the following examples further specifies effect of the present invention.
Embodiment 1 extracts Radix Salviae Miltiorrhizae total phenolic acids from salviamiltiorrhizabung
Radix Salviae Miltiorrhizae 5kg, steam is softening.Cut into pieces, add deionized water 25L, merceration stain 6h, percolation 24h, flow velocity 2L/h.Collect percolate 45L, centrifugal, last macroporous adsorptive resins HPD100 uses the 7.5L water elution, adds the 20L70% ethanol elution again, collects ethanol elution, drying under reduced pressure, and temperature is controlled at 60 ℃.Get salvianolic acid dry powder 320g, finished product yield 6.4%.After testing, content of danshinolic acid B is 71.2%, and total phenolic content is 90.4%.
The detection method of salvianolic acid B and Radix Salviae Miltiorrhizae total phenolic acids:
(1) salvianolic acid B: measure with the HPLC method, detect wavelength 285nm, the standard substance salvianolic acid B is provided by Nat'l Pharmaceutical ﹠ Biological Products Control Institute, and purity is greater than 98%.
(2) Radix Salviae Miltiorrhizae total phenolic acids: measure Radix Salviae Miltiorrhizae total phenolic acids according to ultraviolet spectrophotometry (appendix VA of Chinese Pharmacopoeia version in 2000);
Reference substance solution (0.05mg/ml) 1.0,1.5,2.0,2.5,3.0ml are measured in the preparation of standard curve precision respectively, and methanol-water (1: 1) dilution and standardize solution are in 10ml.Above-mentioned two kinds of each 2ml of solution are in color comparison tube in accurate respectively absorption, add sodium nitrite (1-20) 0.5ml respectively, place 5min, add aluminum nitrate (1-10) 0.5ml again, place 5min, add sodium hydroxide test solution 5ml again, shake up, with the corresponding solvent is blank, measuring trap at 500nm wavelength place according to spectrophotography, is vertical coordinate (y) with the trap, and concentration is abscissa (x), the drawing standard curve, and obtain the computing formula of Radix Salviae Miltiorrhizae total phenolic acids:
y＝9.167x+0.0185(r＝0.9991)
Algoscopy is got this product 10mg, the accurate title, decide, and puts in the conical flask, and precision adds methanol～water (1: 1) 25ml, claim to decide weight, till the ultrasonic dissolving extremely fully, put, claim to decide weight again to room temperature, supply the weight that subtracts mistake with methanol～water (1: 1), shake up, precision is measured 2ml and is diluted to 10ml, as test liquid.Method under the sighting target directrix curve preparation is measured the trap value, and formula calculates above the substitution, promptly gets in the sample content of phenolic acid in the Radix Salviae Miltiorrhizae.
Embodiment 2 extracts Radix Salviae Miltiorrhizae total phenolic acids from salviamiltiorrhizabung
Radix Salviae Miltiorrhizae 5kg, steam is softening.Cut into pieces, add deionized water 25L, merceration stain 24h, percolation 18h, flow velocity 2L/h.Collect percolate 45L, centrifugal, last macroporous adsorptive resins HPD100 uses the 7.5L water elution, adds 20L 95% ethanol elution again, collects ethanol elution, drying under reduced pressure, and temperature is controlled at 60 ℃.Get salvianolic acid dry powder 300g, finished product yield 6%.Press embodiment 1 method and measure, content of danshinolic acid B is 62.7%, and total phenolic content is 86.4%.
Embodiment 3 extracts Radix Salviae Miltiorrhizae total phenolic acids from salviamiltiorrhizabung
Radix Salviae Miltiorrhizae 5kg, steam is softening.Cut into pieces, add deionized water 25L, merceration stain 12h, percolation 12h, flow velocity 2L/h.Collect percolate 45L, centrifugal, last macroporous adsorptive resins HPD100 uses the 7.5L water elution, adds the 20L80% ethanol elution again, collects ethanol elution, drying under reduced pressure, and temperature is controlled at 60 ℃.Get salvianolic acid dry powder 275g, finished product yield 5.5%.Press embodiment 1 method and measure, content of danshinolic acid B is 61.5%, and total phenolic content is 82.5%.
The preparation of embodiment 4 capsules
Radix Salviae Miltiorrhizae total phenolic acids extract 360g
Microcrystalline silicon 10.8g
Make 1000 altogether
Get Radix Salviae Miltiorrhizae total phenolic acids extract and microcrystalline silicon and cross 80 mesh sieve mix homogeneously, filling is in No. 1 capsule, that is, every contains Radix Salviae Miltiorrhizae total phenolic acids extract 360mg.
The preparation of embodiment 5 tablets
Radix Salviae Miltiorrhizae total phenolic acids extract 360g
PEG6000 70g
Pulvis Talci 1.4%
Make 1000 altogether
Get Radix Salviae Miltiorrhizae total phenolic acids extract and PEG6000, the Pulvis Talci mix homogeneously that sieves, dry powder direct tabletting, that is, every contains Radix Salviae Miltiorrhizae total phenolic acids extract 360mg.
The preparation of embodiment 6 granules
Radix Salviae Miltiorrhizae total phenolic acids extract 360g
Microcrystalline Cellulose 70g
Pulvis Talci 1.4%
3% polyvidone alcoholic solution is an amount of
Make 500 bags altogether
Get Radix Salviae Miltiorrhizae total phenolic acids extract and microcrystalline Cellulose mix homogeneously, add 3% polyvidone alcoholic solution system soft material, cross 18 mesh sieve system granules, 50 ℃ of drying 30～60min, granulate adds Pulvis Talci, mixing, pack, that is, every bag contains Radix Salviae Miltiorrhizae total phenolic acids extract 720mg.
The preparation of embodiment 7 injectable powder
Radix Salviae Miltiorrhizae total phenolic acids extract 100g
Mannitol 30g
Calcium disodium edetate 5g
Water for injection 5ml
After said components is mixed, lyophilization, 1000 of packing promptly get the injection lyophilized powder.
Embodiment 8 Radix Salviae Miltiorrhizae total phenolic acids extracts are to the influence of renal hypertensive rat blood pressure
Modeling method: male and female SD rat, body weight 200～220g, Experimental Animal Center provides.Lumbar injection pentobarbital 30mg/kg anesthetized rat at rat left side waist skidding otch, goes out the left kidney tractive, separates the renal artery initial part, clamps renal artery with the 0.2mm silver brain clip, makes it narrow; And only to separate renal artery but without the narrow renal artery of silver brain clip (being the sham-operation rat) in contrast, skin suture.Per two weeks of postoperative are measured blood pressure once, blood pressure determination is measured the arteria caudalis systolic pressure with RBP-1B rat blood pressure meter (by the development of Beijing China-Japan Friendship Hospital), when measuring at every turn, and triplicate, average as blood pressure on the same day, postoperative 5 all blood pressures are considered as Hypertensive Rats greater than 18kPa person.
Experimental rat is divided into four groups: i.e. sham operated rats, model group, positive group, Radix Salviae Miltiorrhizae total phenolic acids extract group (hereinafter to be referred as the Radix Salviae Miltiorrhizae group), with ramipril (German Hirst company, lot number: 40H542) positive control drug, dosage are 1mg/kg/d; Radix Salviae Miltiorrhizae group dosage is 500mg/kg/d, and in 4 weeks of successive administration, sham operated rats and model group are irritated the isopyknic normal saline of stomach, respectively at measuring the rat blood pressure value after 2 weeks of administration, 4 weeks.The result is as shown in table 1.
Table 1 Radix Salviae Miltiorrhizae total phenolic acids extract to the influence of renal hypertensive rat blood pressure (X ± s, n=6)
Annotate: compare with sham operated rats:
*P＜0.05; With before the administration relatively:
▲P＜0.05,
▲ ▲P＜0.01
From table 1 result as seen, blood pressure significant difference between model group and the sham operated rats illustrates the modeling success; After 2 weeks of administration, 4 weeks, compare with model group, Radix Salviae Miltiorrhizae group blood pressure obviously reduces (P＜0.05), illustrates that the Radix Salviae Miltiorrhizae total phenolic acids extract has the effect of tangible blood pressure lowering.
The present invention overcomes the existing deficiency of extracting in the technology of preparing of Radix Salviae Miltiorrhizae total phenolic acids, provides that a kind of step is simple, easy to operate, finished product yield high (generally more than 5%), cost are low, less energy consumption, pollution-free, the method that is easy to suitability for industrialized production.
Claims (5)
1. a preparing salvianolic acids is characterized in that, comprise the steps,
A, salvia piece, the cold water dipping extracts with percolation, collects percolate; Described cold water temperature is: 10～25 ℃, dip time is 6～24 hours, and the percolation time is 12～24 hours;
B, percolate are centrifugal, get supernatant by macroporous adsorbent resin, and eluting washes with water earlier then, and the reuse ethanol elution is collected ethanol elution; Described macroporous adsorbent resin is a styrene type, upper prop medicinal liquid salvianolic acid B: the weight ratio of resin=1: 40～50, add water volume during eluting and be 1～5 times of resin, and the ethanol volume is 2～5 times of resin, ethanol elution concentration is 30～95%;
C, eluent concentrating under reduced pressure, be drying to obtain.
2. preparing salvianolic acids according to claim 1 is characterized in that, among the step a, the cold water dip time is 6 hours, and the percolation time is 24 hours.
3. preparing salvianolic acids according to claim 2, it is characterized in that, among the step b, macroporous adsorbent resin is HPD100, salvianolic acid B in the upper prop medicinal liquid: the weight ratio of resin=1: 40, add water volume during eluting and be 1～1.5 times of resin, the ethanol volume is 4 times of resin, and ethanol elution concentration is 70～95%.
4. preparing salvianolic acids according to claim 3 is characterized in that, among the step b, ethanol elution concentration is 70%.
5. preparing salvianolic acids according to claim 1 is characterized in that, among the step c, baking temperature is 50～70 ℃.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1384090A (en) * | 2001-09-26 | 2002-12-11 | 中国医学科学院药物研究所 | Extraction process of tanshin general phenolic acid and its prepn and use |
| CN1470255A (en) * | 2002-07-22 | 2004-01-28 | 王智民 | Preparation extracted from the root of red-rooted solvia and pseudo-ginseng and its compound preparation and medical use |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1384090A (en) * | 2001-09-26 | 2002-12-11 | 中国医学科学院药物研究所 | Extraction process of tanshin general phenolic acid and its prepn and use |
| CN1470255A (en) * | 2002-07-22 | 2004-01-28 | 王智民 | Preparation extracted from the root of red-rooted solvia and pseudo-ginseng and its compound preparation and medical use |
Non-Patent Citations (2)
| Title |
|---|
| 高小平.从丹参中筛选血管紧张素转换酶抑制剂.中国中药杂志29 4.2004,29(4),359-362. |
| 高小平.从丹参中筛选血管紧张素转换酶抑制剂.中国中药杂志29 4.2004,29(4),359-362. * |
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