CN104147112A - Preparation method of high-activity salviae miltiorrhizae - Google Patents
Preparation method of high-activity salviae miltiorrhizae Download PDFInfo
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- CN104147112A CN104147112A CN201410418544.XA CN201410418544A CN104147112A CN 104147112 A CN104147112 A CN 104147112A CN 201410418544 A CN201410418544 A CN 201410418544A CN 104147112 A CN104147112 A CN 104147112A
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- salviae miltiorrhizae
- radix salviae
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- freezing
- tanshinone
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Abstract
The invention relates to a preparation method of high-activity salviae miltiorrhizae. The method is characterized in that a drying process is carried out after a freezing process is carried out. Prepared salviae miltiorrhizae is high in contents of salvianolic acid B and tanshinone II A, is high in dissolution rate and is high in dissolution speed.
Description
Invention field
The present invention relates to medicine method for making, particularly a kind of preparation method of high activity Radix Salviae Miltiorrhizae, belongs to medical technical field.
Background technology
Radix Salviae Miltiorrhizae is the dry root and rhizome of labiate Radix Salviae Miltiorrhizae, has stasis-dispelling and pain-killing, promoting blood circulation to restore menstrual flow, and the effects such as relieving restlessness that clear away heart-fire, are usually used in obstruction of qi in the chest and cardialgia, dysphoria and insomnia, menoxenia, the skin infection disease such as swell and ache.The active component of Radix Salviae Miltiorrhizae mainly comprises take salvianolic acid B as main liposoluble ingredient, as protocatechuic acid, protocatechualdehyde, danshensu, caffeic acid, alkannic acid, rosmarinic acid, salvianolic acid A, salvianolic acid B and salvianolic acid C etc., with take tanshinone IIA as main tanshinone component, as cryptotanshinone, dihydrotanshinone Ⅰ, tanshinone Ⅰ, Tanshinone II etc.
Through test repeatedly, we find through freezing red rooted salvia, main active salvianolic acid B, the fresher Radix Salviae Miltiorrhizae of tanshinone IIA content, the Radix Salviae Miltiorrhizae that dries in the shade, dry Radix Salviae Miltiorrhizae, dry Radix Salviae Miltiorrhizae and lyophilizing Radix Salviae Miltiorrhizae high.And then known Radix Salviae Miltiorrhizae is through freezing red rooted salvia good effect.
Summary of the invention
The preparation method that the object of this invention is to provide a kind of high activity Radix Salviae Miltiorrhizae.
The object of the present invention is achieved like this:
A preparation method for high activity Radix Salviae Miltiorrhizae, is characterized in that: freezing rear dry.
The preparation method of a kind of high activity Radix Salviae Miltiorrhizae of the present invention, is characterized in that: freezing rear dry be get fresh Radix Salviae Miltiorrhizae freezing after, dry in the shade or dry or dry.
The preparation method of a kind of high activity Radix Salviae Miltiorrhizae of the present invention, is characterized in that: freezing is to be refrigerated to-10 ℃ to freeze below.
So far completed the present invention.
High activity Radix Salviae Miltiorrhizae of the present invention, refers to that main active salvianolic acid B, tanshinone IIA content are high, and dissolution is high, and dissolution rate is fast.And then the Radix Salviae Miltiorrhizae that obtains of known method of the present invention, be used for the treatment of obstruction of qi in the chest and cardialgia, dysphoria and insomnia, menoxenia, the skin infection symptom clinical efficacy such as swell and ache is good.
Below by test example, usefulness of the present invention is described.Test example is intended to further illustrate beneficial effect of the present invention, but not restriction of the present invention.
One, different dry drying method salvianolic acid B of Radix Salviae Miltiorrhizae, Tanshinone II
acontent comparative test
1, processing method:
Fresh red sage root picked up from Wulian County, Shandong in October, 2012, and the fresh salvia miltiorrhiza root of being gathered in same plot is simultaneously processed respectively by following 6 kinds of methods:
1) fresh Radix Salviae Miltiorrhizae: fresh salvia miltiorrhiza root soil buries, plastic bag sealing moisturizing;
2) dry Radix Salviae Miltiorrhizae: fresh red sage root is put to shady and cool ventilation place and dry;
3) dry Radix Salviae Miltiorrhizae: fresh red sage root is directly put under daylight and dried;
4) dry Radix Salviae Miltiorrhizae: fresh red sage root is put at 60 ℃ of temperature and dried;
5) freezing dry Radix Salviae Miltiorrhizae: fresh salvia miltiorrhiza root is refrigerated to-20 ℃ and stops cooling, rise to after room temperature, take out, dry.
6) lyophilizing Radix Salviae Miltiorrhizae: get the fresh Radix Salviae Miltiorrhizae newly digging out, in value freeze dryer, solidification point is controlled at-30 ℃, reaches and controls after temperature, is evacuated to below drying chamber pressure 50Pa, and then heating promotes distillation; The temperature of distillation is controlled at below 40 ℃; Resolution temperature is controlled at below 45 ℃, to dry;
2, salvianolic acid B, Tanshinone II
aassay: measure according to method under 2010 editions (one) Radix Salviae Miltiorrhizae items of Chinese Pharmacopoeia.
1) instrument and reagent: HPLC system: G1314AVDW UV-detector; G1311A quaternary pump; AgiletChemstation chromatographic work station; Reference substance Tanshinone II
a, phenolic acid B is all purchased from Nat'l Pharmaceutical & Biological Products Control Institute.
[determation of tanshinone ⅡA] measured according to high performance liquid chromatography (appendix VI D of Chinese Pharmacopoeia).Chromatographic condition and system suitability be take octadecylsilane chemically bonded silica as filler; The methanol-water (75:25) of take is mobile phase; Detection wavelength is 270nm.Number of theoretical plate calculates and should be not less than 2000 by tanshinone IIA peak.
Tanshinone II is got in the preparation of reference substance solution
areference substance is appropriate, accurately weighed, puts in brown measuring bottle, adds methanol and makes every 1ml containing Tanshinone II
athe solution of 16 μ g, obtains.
The above processed sample of preparation of need testing solution, pulverizes, and crosses sieve No. three, gets respectively about 0.3g, accurately weighed; The about 0.9g of fresh salvia miltiorrhiza root rubs, accurately weighed, puts respectively in tool plug conical flask, and precision adds methanol 50ml, weighed weight, and reflux 1 hour, lets cool, more weighed weight, supplies the weight of less loss with methanol, shakes up, and filters, and gets subsequent filtrate, obtains.
Algoscopy is accurate reference substance Fu liquid and each 5 μ l of need testing solution of drawing respectively, and injection liquid chromatography, measures, and obtains.
[content of danshinolic acid B mensuration] is measured according to high performance liquid chromatography (appendix VI D of Chinese Pharmacopoeia).
Chromatographic condition and system suitability be take octadecylsilane chemically bonded silica as filling chaste tree; Methanol-acetonitrile-formic acid-the water (30:10:1:59) of take is mobile phase; Detection wavelength is 286nm.Number of theoretical plate calculates and should be not less than 2000 by salvianolic acid B honeybee.
It is appropriate that salvianolic acid B reference substance is got in the preparation of reference substance solution, accurately weighed, adds 75% methanol and make every 1ml containing the solution of 0.14mg, obtains.
The preparation of need testing solution get respectively dry in the shade, dry, oven dry, diaphoresis are dry, lyophilizing, lyophilization salvia piece, pulverize, and cross sieve No. three, each about 0.2g, accurately weighed; Fresh red sage root rubs, and gets about 0.6g, accurately weighed, puts in tool plug conical flask, and precision adds 75% methanol 50ml; Weighed weight, reflux 1 hour, lets cool, more weighed weight, supplies the weight of less loss with 75% methanol, broadcasts evenly, filters, and gets subsequent filtrate, obtains.
Algoscopy is accurate respectively to be drawn reference substance solution and supplies each 10 μ l of the brilliant solution of examination, injects hplc determination, obtains.
Result: in dry product, the results are shown in Table 1.
Table 1 different dry drying method salvianolic acid B of Radix Salviae Miltiorrhizae, Tanshinone II
acontent (%)
| Medical material | Fresh | Dry in the shade | Dry | Dry | Freezing dry | Lyophilizing |
| Tanshinone II A | 0.08 | 0.25 | 0.19 | 0.11 | 0.32 | 0.08 |
| Salvianolic acid B | 0.73 | 4.21 | 3.95 | 2.98 | 5.94 | 1.06 |
Salvianolic acid B, Tanshinone II
ait is the main active of Radix Salviae Miltiorrhizae.Comparative result is known, salvianolic acid B of Radix Salviae Miltiorrhizae, Tanshinone II in freezing rear dry Radix Salviae Miltiorrhizae
acontent is the highest.Salvianolic acid B, Tanshinone II
abe the main active of Radix Salviae Miltiorrhizae, freezing rear dry Radix Salviae Miltiorrhizae activity is high.
Two, dry salvianolic acid B of Radix Salviae Miltiorrhizae, the Tanshinone II of the freezing rear distinct methods of Radix Salviae Miltiorrhizae
acontent comparative test
1, processing method:
The fresh salvia miltiorrhiza of getting test one, is refrigerated to-20 ℃ of end, rises to after room temperature, takes out, dry by the method for drying, dry, drying respectively.
2, salvianolic acid B, Tanshinone II
aassay: measure according to method under 2010 editions (one) Radix Salviae Miltiorrhizae items of Chinese Pharmacopoeia.Result: in dry product, Tanshinone II
ameasurement result is in Table 5, and salvianolic acid B measurement result is in Table 2.
Table 2 freezes the dry salvianolic acid B of Radix Salviae Miltiorrhizae of rear distinct methods, Tanshinone II
acontent (%)
| Medical material | Freezing drying in the shade | Freezing drying | Freezing oven dry |
| Tanshinone II A | 0.32 | 0.31 | 0.31 |
| Salvianolic acid B | 5.94 | 5.83 | 5.12 |
More known, the dry Radix Salviae Miltiorrhizae making of the freezing rear distinct methods of Radix Salviae Miltiorrhizae, salvianolic acid B, Tanshinone II
acontent does not significantly change.Illustrate that Radix Salviae Miltiorrhizae adopts the Radix Salviae Miltiorrhizae that first freezing rear dry method obtains, active constituent content is high, and then known clinical efficacy is good.
Three, Their Dissolution Test in vitro
1, prepare sample
Radix Salviae Miltiorrhizae 1: get fresh Radix Salviae Miltiorrhizae and dry.
Radix Salviae Miltiorrhizae 2: get the fresh Radix Salviae Miltiorrhizae newly digging out, be refrigerated to below-10 ℃, room temperature to be risen to, dries.
2, content of danshinolic acid B is measured according to method under 2010 editions (one) Radix Salviae Miltiorrhizae items of < < Chinese Pharmacopoeia > > and is measured.
Result: in dry product, content of danshinolic acid B is in Table 3.
Each decoction pieces content of danshinolic acid B (%) of table 3
| Decoction pieces | Radix Salviae Miltiorrhizae 1 | Radix Salviae Miltiorrhizae 2 |
| Dissolution | 3.48 | 5.31 |
3, Their Dissolution Test in vitro
This test adopts the solution (sodium chloride 2.0g, adds water and dissolve in right amount, adds hydrochloric acid 7ml, is diluted with water to 1000 ml, obtains) of pH1.2 to simulate normal person's simulated gastric fluid.Salvia piece is not identical with the content of salvianolic acid B in salvia piece of the present invention, and dissolution calculates respectively according to content separately.Because food is 90-120min at the emptying time of people's gastric, therefore this test is at each point in time sampling of 5-120min.
Sample thief, pulverize, cross sieve No. 6, get respectively 6 parts, every part of 0.2g, according to < < Chinese Pharmacopoeia > > Their Dissolution Test in vitro method, measure, the solution 600ml of pH1.2 of take is solvent, rotating speed is 50r/min, through 5, 10, 15, 30, 45, 60, 90, during 120 min, get respectively solution 5ml, with 0.45 μ m microporous filter membrane, filter, get subsequent filtrate as need testing solution, and immediately in process container, supplement dissolution medium, according to content of danshinolic acid B algoscopy, measure, take sample size as 100%, by external standard method, with calculated by peak area, go out sample at the stripping quantity of different time.The results are shown in Table 4.
Each Radix Salviae Miltiorrhizae dissolution in vitro comparison (%, n=6) of table 4
According to Weibull distribution, stripping percentage rate and the functional relationship of time have been set up, choose m (dissolution rate curve shape parameter, the i.e. slope of curve), T50 (dissolution rate reaches 50% required time), 3 parameters of Td (dissolution rate reaches 63.2% required time) compare, and the results are shown in Table 5.
Each Radix Salviae Miltiorrhizae In Vitro Dissolution parameter comparison (x ± s, n=6) of table 5
| Stripping parameter | Radix Salviae Miltiorrhizae 1 | Radix Salviae Miltiorrhizae 2 | p |
| m | 1.31±3.03 | 1.45±1.84 | >0.05 |
| T 50 | 84.14±32.03 | 43.11±12.10 | <0.05 |
| T d | 108.40±36.03 | 54.31±13.78 | <0.05 |
Stripping parameter analysis result is shown to the T of freezing rear dry Radix Salviae Miltiorrhizae
50and T
dbe less than and dry Radix Salviae Miltiorrhizae, both comparing differences have statistical significance (p<0.05), showing that freezing rear dry effective component in red sage In Vitro Dissolution rate is significantly higher than dries Radix Salviae Miltiorrhizae, and then known freezing rear dry Radix Salviae Miltiorrhizae activity is high, and clinical efficacy is better than and dries Radix Salviae Miltiorrhizae.
Four, freezing processing is on the decoction pieces impact of drying time
Salvia piece dries in the shade: get and dry red rooted salvia, spray a small amount of water profit to softening, be cut into the sheet of 2～4mm, put shady and cool ventilation place, 4 days drying times.
Freezing dry salvia piece: get freezing dry red rooted salvia, spray a small amount of water profit to softening, be cut into the sheet of 2～4mm, put shady and cool ventilation place, 2 days drying times.
Result is known, and it is short drying time that freezing dry Radix Salviae Miltiorrhizae is prepared decoction pieces, and efficiency is high.
As well known to those skilled in the art, efficiently medicine is should active constituent content high, and dissolution rate is high, quality homogeneous.Above result of the test explanation, high with freezing rear dry effective component in red sage content, In Vitro Dissolution rate is high, product quality homogeneous, and then Radix Salviae Miltiorrhizae prepared by known the inventive method is used for the treatment of obstruction of qi in the chest and cardialgia, dysphoria and insomnia, menoxenia, the skin infection disease such as swell and ache, clinical efficacy is good.
The specific embodiment
embodiment 1
Get fresh Radix Salviae Miltiorrhizae, be refrigerated to-10 ℃ and stop cooling, naturally rise to after room temperature, put shady and cool ventilation place and dry.
embodiment 2
Get fresh Radix Salviae Miltiorrhizae, be refrigerated to-15 ℃ and stop cooling, naturally rise to after room temperature, cut into chunks, dry.
embodiment 3
Adopt ZG-100 ㎡ type vacuum freeze drier, get fresh Radix Salviae Miltiorrhizae, be refrigerated to-20 ℃ and stop cooling, naturally rise to room temperature, take out, cut into short section, put in baking oven, at 60 ℃ of following temperature, dry.
embodiment 4
Get fresh Radix Salviae Miltiorrhizae, be refrigerated to-32 ℃ and stop cooling, take out, be cut into long section, put shady and cool ventilation place and dry.
embodiment 5
Get fresh Radix Salviae Miltiorrhizae, be refrigerated to-35 ℃ and stop cooling, naturally rise to room temperature, take out, put in baking oven, at 60 ℃ of following temperature, dry, pulverize.
embodiment 6
Get fresh Radix Salviae Miltiorrhizae, be refrigerated to-30 ℃ and stop cooling, naturally rise to after room temperature, dry, be crushed to impalpable powder.
embodiment 7
Get fresh Radix Salviae Miltiorrhizae, be refrigerated to-25 ℃ and stop cooling, take out, cut into thin slice, put in microwave vacuum drying case, 55 ℃ of design temperatures, microwave is to dry.
embodiment 8
Get fresh Radix Salviae Miltiorrhizae, be refrigerated to-25 ℃ and stop cooling, take out, cut into thin slice, put in vacuum drying oven, 60 ℃ of design temperatures, to dry.
Claims (3)
1. a preparation method for high activity Radix Salviae Miltiorrhizae, is characterized in that: freezing rear dry.
2. according to the preparation method of a kind of high activity Radix Salviae Miltiorrhizae of claim 1, it is characterized in that: freezing rear dry be get fresh Radix Salviae Miltiorrhizae freezing after, dry in the shade or dry or dry.
3. according to the preparation method of a kind of high activity Radix Salviae Miltiorrhizae of claim 1, it is characterized in that: freezing is to be refrigerated to-10 ℃ to freeze below.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107184649A (en) * | 2017-07-14 | 2017-09-22 | 济南大学 | A kind of red sage root adopts rear drying means |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20100209388A1 (en) * | 2003-08-02 | 2010-08-19 | Elizabeth Anne Mazzio | Nutraceutical composition and method of use for treatment / prevention of cancer |
| CN102526190A (en) * | 2012-02-21 | 2012-07-04 | 复旦大学 | Production method and application of high-quality stable red-rooted salvia medicinal material |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20100209388A1 (en) * | 2003-08-02 | 2010-08-19 | Elizabeth Anne Mazzio | Nutraceutical composition and method of use for treatment / prevention of cancer |
| CN102526190A (en) * | 2012-02-21 | 2012-07-04 | 复旦大学 | Production method and application of high-quality stable red-rooted salvia medicinal material |
Non-Patent Citations (2)
| Title |
|---|
| 唐晓清等: "丹参采收后不同干燥法对丹参酮ⅡA和丹参素的影响", 《中草药》 * |
| 苏子仁等: "丹参醇提工艺中丹参酮ⅡA降解动力学研究", 《中成药》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107184649A (en) * | 2017-07-14 | 2017-09-22 | 济南大学 | A kind of red sage root adopts rear drying means |
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Application publication date: 20141119 |