CN104147115A - Preparation method of high-activity salviae miltiorrhizae - Google Patents
Preparation method of high-activity salviae miltiorrhizae Download PDFInfo
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- CN104147115A CN104147115A CN201410418789.2A CN201410418789A CN104147115A CN 104147115 A CN104147115 A CN 104147115A CN 201410418789 A CN201410418789 A CN 201410418789A CN 104147115 A CN104147115 A CN 104147115A
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- salviae miltiorrhizae
- radix salviae
- dry
- lyophilizing
- vexed
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Abstract
The invention relates to a preparation method of high-activity salviae miltiorrhizae. The method is characterized in that a freeze-drying process is carried out after a stacked covering process being 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 to pile vexed after lyophilizing Radix Salviae Miltiorrhizae, 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, pile vexed dry Radix Salviae Miltiorrhizae and lyophilizing Radix Salviae Miltiorrhizae high.And then the vexed rear lyophilizing Radix Salviae Miltiorrhizae good effect of known heap.
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: pile vexed rear lyophilizing.
The preparation method of a kind of high activity Radix Salviae Miltiorrhizae of the present invention, is characterized in that: piling vexed is to get the fresh Radix Salviae Miltiorrhizae newly digging out to pile vexed 2-6 days.
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 below, 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 8 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) pile vexed dry Radix Salviae Miltiorrhizae: fresh red sage root is piled and dried for vexed 3 days again;
6) pile vexed lyophilizing Radix Salviae Miltiorrhizae: get the fresh Radix Salviae Miltiorrhizae newly digging out and pile vexed 3 days, in value freeze dryer, solidification point is controlled at-30 ℃, and drying chamber pressure is controlled at below 50Pa, and the temperature of distillation is controlled at below 40 ℃; Resolution temperature is controlled at below 45 ℃, to dry.
7) 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.Result: in dry product, Tanshinone II
ameasurement result is in Table 1, and salvianolic acid B measurement result is in Table 2.
Table 1 fresh salvia miltiorrhiza and different dry drying method Tanshinone II
acontent (%)
| Medical material | Fresh | Dry in the shade | Dry | Dry | Diaphoresis is dry | Pile vexed lyophilizing | Lyophilizing |
| Content | 0.08 | 0.25 | 0.19 | 0.11 | 0.24 | 0.38 | 0.08 |
The red phenol decoction pieces acid of table 2 fresh salvia miltiorrhiza and different dry drying method Radix Salviae Miltiorrhizae B content (%)
| Medical material | Fresh | Dry in the shade | Dry | Dry | Diaphoresis is dry | Pile vexed lyophilizing | Lyophilizing |
| Content | 0.73 | 4.21 | 3.95 | 2.98 | 4.37 | 7.42 | 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, the Tanshinone II of freezing dry Radix Salviae Miltiorrhizae and the vexed lyophilizing Radix Salviae Miltiorrhizae of heap
acontent is the highest.Salvianolic acid B, Tanshinone II
athe main active of Radix Salviae Miltiorrhizae, through heap vexed lyophilizing and freezing after dry Radix Salviae Miltiorrhizae activity high.
Two, Their Dissolution Test in vitro
1, prepare sample
Dry Radix Salviae Miltiorrhizae: get fresh Radix Salviae Miltiorrhizae and dry.
Pile vexed rear lyophilizing Radix Salviae Miltiorrhizae: get fresh salvia miltiorrhiza and pile vexed 3 days, lyophilizing.
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 | Dry Radix Salviae Miltiorrhizae | Pile vexed rear lyophilizing Radix Salviae Miltiorrhizae |
| Dissolution | 3.48 | 5.36 |
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.Dry Radix Salviae Miltiorrhizae not identical with the content of salvianolic acid B in the vexed rear lyophilizing Radix Salviae Miltiorrhizae of heap, 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 50 r/ 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 | Dry | Pile vexed rear lyophilizing | p |
| m | 1.31±3.03 | 1.44±1.92 | >0.05 |
| T 50 | 84.14±32.03 | 43.13±13.12 | <0.05 |
| T d | 108.40±36.03 | 54.35±13.93 | <0.05 |
Stripping parameter analysis result is shown, through the T of the vexed lyophilizing Radix Salviae Miltiorrhizae of heap
50and T
dbe less than and dry Radix Salviae Miltiorrhizae, both comparing differences have statistical significance (p<0.05), show to pile vexed lyophilizing effective component in red sage In Vitro Dissolution rate and be significantly higher than and dry Radix Salviae Miltiorrhizae, and then the vexed lyophilizing Radix Salviae Miltiorrhizae of known heap activity is high, clinical efficacy is better than and dries Radix Salviae Miltiorrhizae.
As well known to those skilled in the art, efficiently medicine is should active constituent content high, and dissolution rate is high, quality homogeneous.The explanation of above result of the test, piles vexed lyophilizing effective component in red sage content high, and 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, and dysphoria and insomnia, menoxenia, the skin infection disease such as swell and ache, clinical efficacy is good.
The specific embodiment
embodiment 1
Get the fresh Radix Salviae Miltiorrhizae newly digging out and pile vexed 2 days, clean roguing, be cut into the segment of length 5cm, lyophilizing: solidification point is controlled at-28 ℃; Drying chamber pressure is controlled at below 50Pa; The temperature of China is controlled at below 40 ℃; Resolution temperature is controlled at below 45 ℃.
embodiment 2
Get the fresh Radix Salviae Miltiorrhizae newly digging out and pile vexed 3 days, clean roguing, be cut into the Radix Salviae Miltiorrhizae section of length 3cm; By the sabot of Radix Salviae Miltiorrhizae section, loading amount is 8Kg/ ㎡; Solidification point is controlled at-32 ℃; Reach and control after temperature, open immediately vacuum pump and be evacuated to below drying chamber pressure 50Pa; Subliming by heating, the temperature of distillation is controlled at below 40 ℃; Resolution temperature is controlled at below 45 ℃, to dry, takes out.
embodiment 3
Get the fresh Radix Salviae Miltiorrhizae newly digging out and pile vexed 6 days, clean roguing, be cut into the Radix Salviae Miltiorrhizae section of length 2cm, lyophilizing.
embodiment 4
Get the fresh Radix Salviae Miltiorrhizae newly digging out and pile vexed 3 days, clean roguing, sabot, thickness is 15～20 mm, in freezing process, with 0.3 ℃/min cooling, solidification point is controlled at-30 ℃; The vacuum degree control of distillation is at 60pa, and temperature is controlled at below 40 ℃; The vacuum degree control of desorbing is at 50pa; Temperature is controlled at below 45 ℃, to dry.
embodiment 5
Get the fresh Radix Salviae Miltiorrhizae newly digging out, entrucking on the same day, is transported to lyophilizing factory after 2 days, after unloading, cleans roguing, lyophilizing.
With reference to method under Chinese Pharmacopoeia 2010 editions () Radix Salviae Miltiorrhizae item, measure result: Tanshinone II
acontent is 0.41%, the content of phenolic acid B is 7.26%.
Claims (2)
1. a preparation method for high activity Radix Salviae Miltiorrhizae, is characterized in that: pile vexed rear lyophilizing.
2. according to the preparation method of a kind of high activity Radix Salviae Miltiorrhizae of claim 1, it is characterized in that: piling vexed is to get the fresh Radix Salviae Miltiorrhizae newly digging out to pile vexed 2-6 days.
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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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- 2014-08-25 CN CN201410418789.2A patent/CN104147115A/en active Pending
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》 * |
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