CN104180613A - Freeze-drying method for roots of red-rooted salvia - Google Patents
Freeze-drying method for roots of red-rooted salvia Download PDFInfo
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- CN104180613A CN104180613A CN201410418542.0A CN201410418542A CN104180613A CN 104180613 A CN104180613 A CN 104180613A CN 201410418542 A CN201410418542 A CN 201410418542A CN 104180613 A CN104180613 A CN 104180613A
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- freeze
- dry
- red sage
- sage root
- vexed
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Abstract
The invention relates to a freeze-drying method for roots of red-rooted salvia. The freeze-drying method is characterized in that the fresh roots of red-rooted salvia are freeze-dried to half-dry and piled in a covered manner prior to being dried. Therefore, energy resources are saved, and the prepared roots of red-rooted salvia are high in content of main active ingredients of danshinolic acid B and tanshinone II A.
Description
Invention field
The present invention relates to medicine, particularly a kind of freeze drying process of the red sage root, belongs to medical technical field.
Background technology
The red sage root is the dry root and rhizome of the labiate red sage root, has stasis-dispelling and pain-killing, activating blood to promote menstruation, and the effects such as relieving restlessness that clear away heart-fire, are usually used in chest impediment and cardialgia, dysphoria and insomnia, irregular menstruation, the sore disease such as swell and ache.The active component of the red sage root mainly comprises take tanshin polyphenolic acid B as main liposoluble ingredient, as protocatechuic acid, protocatechualdehyde, danshensu, caffeic acid, alkannic acid, Rosmarinic acid, salviandic acid A, tanshin polyphenolic acid B and salvianolic acid C etc., with take tanshinone IIA as main tanshinone component, as Cryptotanshinone, dihydrotanshinone Ⅰ, salvia miltiorrhiza bge I, Tanshinone II etc.
Summary of the invention
The freeze drying process that the object of this invention is to provide a kind of red sage root, the effective component in red sage content of preparation is high, is used for the treatment of chest impediment and cardialgia, dysphoria and insomnia, irregular menstruation, the sore disease such as swell and ache, clinical efficacy is good.
The object of the present invention is achieved like this:
A freeze drying process for the red sage root, is characterized in that getting fresh red sage root freeze-drying to half-dried, piles vexed rear dry.
The freeze drying process of a kind of red sage root of the present invention, it is characterized in that piling vexed rear dry be that heap dries or dries or dry after vexed.
The freeze drying process of a kind of red sage root of the present invention, it is characterized in that piling vexed is the vexed 2-6 days of heap.
So far completed the present invention.
Freeze-drying of the present invention to half-dried be a fuzzy concept, the explication of non-mathematics, is to determine according to half of distillation overall process time.The time of distillation overall process is determined, is after distillation starts, and during state state before condenser temperature drops to distillation, distillation finishes, and counts the time of distillation overall process.Time and the solidification point of distillation overall process, how much relevant be dried constant pressure, sublimation temperature, material.During concrete enforcement, can determine according to test.
The steps such as freeze-drying is vacuum freeze drying by name entirely, claims again freeze drying, and freezing dry process mainly can be divided into primary drying (distillation), redrying (desorb).The difference of the present invention and existing freeze drying technology is to sublime up into approximately one half of distillation overall process time, finishes freeze-drying, takes out, and piles vexed rear dry.The effect that this difference produces is: save the energy, and red sage root main active tanshin polyphenolic acid B, the Tanshinone II of preparation
acontent higher than fresh, dry in the shade, dry, oven dry, the freeze-drying red sage root, and then known, be used for the treatment of chest impediment and cardialgia, dysphoria and insomnia, irregular menstruation, the sore sick clinical efficacy such as swell and ache is good.
Below by test example, further illustrate beneficial effect of the present invention, test example is intended to further illustrate effect of the present invention, but not restriction of the present invention.
One, salvia piece tanshin polyphenolic acid B, the Tanshinone II that prepared by different dry drying method
acontent comparative test
1, processing method:
Native fresh salvia miltiorrhiza root is played in same plot simultaneously, processes respectively by the following method:
1) the fresh red sage root: fresh salvia miltiorrhiza root soil buries, plastic bag sealing moisturizing;
2) dry the red sage root: get fresh salvia miltiorrhiza root and put shady and cool ventilation place and dry;
3) dry the red sage root: get fresh fresh salvia miltiorrhiza root and dry;
4) dry the red sage root: by fresh salvia miltiorrhiza root lower than drying at 60 ℃ of temperature;
6) the freeze-drying red sage root: get the fresh red sage root 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;
7) freeze the vexed red sage root that dries of half-dried heap: get the fresh pellet 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 ℃; Distil and after 5 hours, take out (through overtesting, how many according to material, distillation overall process is generally at 10-12), pile vexed 3 days, dry.
2, determination of moisture: according to the moisture analysis content of Chinese pharmacopoeia 2010 editions ().Specific as follows: testing sample is placed in the culture dish that is dried to constant weight and precise weighing, after precision weighing initial weight, be placed in drier, 105 ℃ are dried to constant weight, the moisture of calculation sample.The results are shown in Table 1.
Table 1 distinct methods is dried red sage root water content (%)
| Medicinal material | Fresh | Dry in the shade | Dry | Dry | Freeze-drying | Freeze that half-dried heap is vexed to be dried |
| Water content | 75.21 | 11.42 | 8.75 | 6.62 | 7.82 | 7.83 |
As shown in Table 1, the red sage root that distinct methods is dry, its moisture can reach below 13.0% of < < Chinese pharmacopoeia > > regulation.
3, tanshin polyphenolic acid B, Tanshinone II
aassay: measure according to method under 2010 editions (one) red sage root items of Chinese pharmacopoeia.
1) instrument and reagent: HPLC system: G1314AVWD 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.
2) method
Chromatographic condition: adopt YMC C18 (250mm * 4.6mm, 5 μ m chromatographic columns, 25 ℃ of column temperatures; With methyl alcohol (A)-0.5% aqueous formic acid (B) mobile phase, carry out gradient elution [0-30min, A-B (35:65); 30-35 min, A-B (35:65) → A-B (80:20); 35-50 min; A-B (80:20), flow velocity 1.OmL/ min; Detect wavelength: tanshin polyphenolic acid B is 286 nm (0-30 min), and tanshinone IIA is 270nm (30-50min); Sample size 20 μ L.
The preparation of reference substance storing solution: precision takes reference substance Tanshinone II
a5mg, puts in the brown measuring bottle of 25mL, adds methanol constant volume to scale, shakes up, and obtains Tanshinone II
acontrast storing solution; Precision takes tanshin polyphenolic acid B 5mg, puts in the brown measuring bottle of 10mL, adds methanol constant volume to scale, shakes up, and obtains root of red-rooted salvia phenolic acid B reference substance storing solution.
Prepare need testing solution: get fresh salvia miltiorrhiza root and rub, cross sieve No. 6, get 150g, accurately weighed; More than the red sage root of preparation, pulverizes, and crosses sieve No. 6, gets respectively about 50g, accurately weighed; Put in tool plug conical flask, soak 20min, utilize supersonic wave cleaning machine ultrasonic wave room temperature to extract 3 times; Each precision adds 75% ethanol 400mL, and extraction time is respectively 30,25,20min, and standing 10min, filters, and merges 3 times filtrate, concentrates, and obtains medicinal extract, accurately weighed.Precision takes medicinal extract 50mg, puts in the brown measuring bottle of 50mL, with methyl alcohol, dissolves and is diluted to scale, with miillpore filter (0.45 μ m), filters, standby.Make respectively the salvia piece need testing solution of fresh salvia miltiorrhiza root, different dry drying method.
Result: in dry product, Tanshinone II
ameasurement result is in Table 2, and tanshin polyphenolic acid B measurement result is in Table 3.
Table 2 fresh salvia miltiorrhiza and distinct methods are dried tanshinone in salvia miltiorrhiza bunge II
acontent (%)
| Medicinal material | Fresh | Dry in the shade | Dry | Dry | Freeze-drying | Freeze that half-dried heap is vexed to be dried |
| Content | 0.08 | 0.26 | 0.21 | 0.18 | 0.08 | 0.39 |
Content of danshinolic acid B (%) in the dry red sage root of table 3 fresh salvia miltiorrhiza distinct methods
| Medicinal material | Fresh | Dry in the shade | Dry | Dry | Freeze-drying | Freeze that half-dried heap is vexed to be dried |
| Content | 0.77 | 4.28 | 3.94 | 2.93 | 1.06 | 7.54 |
Comparative result, to freeze vexed tanshin polyphenolic acid B, the Tanshinone II that dries the red sage root of half-dried heap
acontent is the highest.Tanshin polyphenolic acid B, Tanshinone II
abe the main active of the red sage root, known according to result, distillation finishes rear heap, and vexed to dry red sage root clinical efficacy good.
The specific embodiment
embodiment 1
Get the fresh red sage root and clean impurity elimination, be cut into the segment of length 5cm; By segment sabot, loading amount is 4Kg/ ㎡ left and right; Solidification point is controlled at-28 ℃; Reach and control after temperature, open immediately vavuum pump and be evacuated to below drying chamber pressure 50Pa, then start heater switch, promote distillation; The temperature of distillation is controlled at below 40 ℃; Distil and take out after 5 hours, pile vexed 2 days, dry.
embodiment 2
Get the fresh red sage root, clean impurity elimination, be cut into the red sage root section of length 3cm; By the sabot of red sage root section, loading amount is 8Kg/ ㎡; Solidification point is controlled between-32 ℃; Reach and control after temperature, open immediately vavuum pump and be evacuated to below drying chamber pressure 50Pa, then start heater switch, promote distillation; The temperature of distillation is controlled at below 40 ℃; Distil and take out after 6 hours, pile vexed 3 days, dry.
embodiment 3
Get the fresh red sage root and clean impurity elimination, be cut into the red sage root section of length 2cm, sabot, sabot weight is 7kg/ ㎡ left and right, puts in ZG-100 ㎡ type vacuum freeze drier, after lowering the temperature gradually 2 hours, freezes to-28 ℃; Be evacuated to system absolute pressure 40Pa, be heated to 35 ℃ of lyophilizations, distil and take out after 5 hours, take out, pile vexed 4 days, dry.
embodiment 4
Get the fresh pellet newly digging out, clean impurity elimination, 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 ℃; Distil and take out after 7 hours, pile infrared drying vexed 6 days.
embodiment 5
Get the fresh red sage root and clean impurity elimination, be cut into the segment of length 5cm; By segment sabot, loading amount is 3Kg/ ㎡ left and right; Solidification point is controlled at-28 ℃; Reach and control after temperature, open immediately vavuum pump and be evacuated to below drying chamber pressure 50Pa, then start heater switch, promote distillation; The temperature of distillation is controlled at below 40 ℃; Distil and take out after 4 hours, pile vexed 2 days, dry.
Claims (3)
1. a freeze drying process for the red sage root, is characterized in that getting fresh red sage root freeze-drying to half-dried, piles vexed rear dry.
2. according to the freeze drying process of a kind of red sage root of claim 1, it is characterized in that piling vexed rear dry be that heap dries or dries or dry after vexed.
3. according to the freeze drying process of a kind of red sage root of claim 1, it is characterized in that piling vexed is the vexed 2-6 days of heap.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113251749A (en) * | 2021-05-18 | 2021-08-13 | 甘肃省方熙药业科技有限公司 | Method for freeze drying salvia miltiorrhiza |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH09152268A (en) * | 1995-11-30 | 1997-06-10 | Liquid Gas:Kk | Freeze dryer |
| CN103055022A (en) * | 2013-01-10 | 2013-04-24 | 济南康众医药科技开发有限公司 | Method for processing rehmannia and application for rehmannia in preparation for medicine |
| CN103948638A (en) * | 2014-05-15 | 2014-07-30 | 济南康众医药科技开发有限公司 | Drying method of medical fungi |
| CN103948642A (en) * | 2014-05-15 | 2014-07-30 | 济南康众医药科技开发有限公司 | Application of refrigeration technique in phellinus igniarius drying |
-
2014
- 2014-08-25 CN CN201410418542.0A patent/CN104180613A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH09152268A (en) * | 1995-11-30 | 1997-06-10 | Liquid Gas:Kk | Freeze dryer |
| CN103055022A (en) * | 2013-01-10 | 2013-04-24 | 济南康众医药科技开发有限公司 | Method for processing rehmannia and application for rehmannia in preparation for medicine |
| CN103948638A (en) * | 2014-05-15 | 2014-07-30 | 济南康众医药科技开发有限公司 | Drying method of medical fungi |
| CN103948642A (en) * | 2014-05-15 | 2014-07-30 | 济南康众医药科技开发有限公司 | Application of refrigeration technique in phellinus igniarius drying |
Non-Patent Citations (1)
| Title |
|---|
| 饶伟文等: "中药产地加工规范化研究发展", 《中国中医药信息杂质》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113251749A (en) * | 2021-05-18 | 2021-08-13 | 甘肃省方熙药业科技有限公司 | Method for freeze drying salvia miltiorrhiza |
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Application publication date: 20141203 |