CN102000199A - Method for drying extract of total saponins of leaves of rehmannia glutinosa libosch - Google Patents
Method for drying extract of total saponins of leaves of rehmannia glutinosa libosch Download PDFInfo
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- CN102000199A CN102000199A CN 201010551372 CN201010551372A CN102000199A CN 102000199 A CN102000199 A CN 102000199A CN 201010551372 CN201010551372 CN 201010551372 CN 201010551372 A CN201010551372 A CN 201010551372A CN 102000199 A CN102000199 A CN 102000199A
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Abstract
The invention relates to a method for drying the extract of total saponins of leaves of rehmannia glutinosa libosch. In the method, the extract of the total saponins of the leaves of the rehmannia glutinosa libosch is gradually dried at a low temperature in vacuum through microwave vacuum drying; and vacuum microwave drying technology is used for drying the extract of the total saponins of the leaves of the rehmannia glutinosa libosch, and has the advantages of stable process, low moisture content of a product, high retention rate of active ingredients, short drying time and the like. Full-automatic control is realized in the whole drying process, so that labor intensity is reduced, and production efficiency is improved; and compared with the quality of the product processed by the common drying method through a vacuum drying oven, the quality of the product processed by the method is greatly improved and is also higher than that of the product processed by a band drying method, so that the subsequent preparation process of the leaves of the rehmannia glutinosa libosch is facilitated.
Description
Technical field
The invention belongs to technical field of Chinese medicines, particularly relate to a kind of drying means of Folium Rehmanniae total glycoside extract.
Background technology
Folium Rehmanniae is the dried leaves of scrophulariaceae rehmannia glutinosa plant (Rehmannia glutinosa Libosch).Modern pharmacology studies show that contained main component is the Folium Rehmanniae total glycosides in the Folium Rehmanniae, wherein is representative with the verbascoside.The Folium Rehmanniae total glycosides has enriching yin and nourishing kidney, removing heat from blood and promoting blood circulation, the effect of consolidating semen hemostasis.Can be used for treating albuminuria, hematuria, chronic glomerulonephritis; Belong to syndrome of deficiency of both qi and yin.The drying of Folium Rehmanniae total glycoside extract is one of important step in the total glycosides formulation production process of Folium Rehmanniae, and product quality is had bigger influence.The drying means of Folium Rehmanniae total glycoside extract mainly adopts the vacuum and low temperature oven drying at present.At Chinese patent disclosed " Folium Rehmanniae extract and its production and use " (publication number: CN1947757A) with " preparation technology who has the verbascoside of treatment chronic glomerulonephritis effect in the Folium Rehmanniae " (publication number: CN101121740A), all adopt the cryogenic vacuum oven method.The problem that this method exists is: dark, the easy caking of the dry products color and luster that obtains, poorly soluble, i.e. Folium Rehmanniae total glycoside extract dry poor product quality; Need manually stir and discharging, easily cause the cross-contamination of people and storeroom; And can not continuous operation, drying time is long, baking temperature is high, the thermal sensitivity loss of effective components is big, and production capacity is little, and power consumption height and yield are low.
In application for a patent for invention number: in the patent of CN200910216153.9 Folium Rehmanniae total glycoside extract dry product preparation method, the Folium Rehmanniae total glycoside extract has adopted vacuum belt type drying, through production confirmation repeatedly, extractum does not reach 1～2.5 kg/h charging rate of setting, transporting velocity also is lower than the setting speed of 2～8 m/h, and the extractum straying quatity is few, and for the high slightly extractum of density, spray cream rifle easily stops up, the crawler belt running speed is slow, dried cream per hour can only receive 3～5kg, the material heated time is long, there is certain loss in the thermal sensitivity effective ingredient, heating source need be set up separately, is the relatively independent auxiliary equipment of a cover, and this has also increased the unstability of whole set of installation, energy consumption is also big, exsiccant efficient is low, and production capacity is not strong yet, needs staff on duty, batch production time is extremely long, and labor efficiency is low.Moreover, the loader of belt dryer, spray cream rifle, crawler belt, cavity all will adhere to more material when producing, cause excess loss, and these positions are difficult to clean, need with great amount of manpower, a large amount of abluent and cleaning water, this has also increased production cost in a disguised form.
Summary of the invention
Purpose of the present invention provides a kind of new drying means of Folium Rehmanniae total glycoside extract, to solve the low problem of present Folium Rehmanniae total glycoside extract dry production efficiency.Adopt product yield that this method obtains to have significantly and promote than vacuum tank formula oven drying or vacuum belt type drying method, production efficiency height, and quality better, content height, thus help the follow-up preparation process of Folium Rehmanniae.Simultaneously, for realizing big suitability for industrialized production, reduce material and energy waste on the primary and foremost purpose basis, the equipment design defect of avoiding causes the cleaning blind area and causes that material pollutes, and a kind of preparation method of Folium Rehmanniae total glycoside extract dry product of Automatic Control is provided.
The present invention constitutes like this:
The Folium Rehmanniae preparation method of extract, take following steps:
1.. Folium Rehmanniae/stem and leaf directly or after pulverizing, is adopted solvent heating and refluxing extraction method or supercritical fluid extraction extraction method, extracting solution.
2.. with extracting liquid filtering, reclaim solvent and be concentrated into the concentrated solution a of relative density 1.01～1.10.
3.. a leaves standstill clarification with concentrated solution, get supernatant and pass through adsorption resin column, water elution adsorption resin column with 1～6 times of amount of resin column volume, discard water liquid, the concentration of 1～6 times of amount of reuse resin column volume is 20～96% ethanol elution, collect ethanol elution, reclaim ethanol and be concentrated into the concentrated solution b of relative density 1.01～1.10.
4.. b leaves standstill clarification with concentrated solution, get supernatant and pass through adsorption resin column, water eluting adsorption resin column is closely neutral to effusive liquid, discard water liquid, the concentration of 1～3 times of amount of reuse resin column volume is 10～20% ethanol elution, discards ethanol elution, and continuing with 1～6 times of resin column volume amount concentration is 60～96% ethanol elution, reclaim ethanol and be concentrated into the extractum of relative density 1.20～1.40, promptly get product Folium Rehmanniae total glycoside extract.
In the 1. described solvent heating and refluxing extraction of the above-mentioned steps method, solvent reflux, extract, 1～3 time under 50～100 ℃ of conditions, each 0.5～1.5 hour, merge extractive liquid.Solvent is selected for use:
(a). a kind of solvent in water, methanol, the ethanol; Perhaps
(b). a kind of in the mixed solvent that water or methanol or ethanol and acetic acid are formed, its consumption volume ratio is concentration 30～96% ethanol or concentration 30～96% methanol or water: acetic acid=80～99.99:20～0.01(V:V); Perhaps
(c). the mixed solvent that any two or more arbitrary proportions are formed in above-mentioned (a) and (b).
Described solvent preferred alcohol.
Contain 0.01～10% acetic acid (V:V) in the 3. described ethanol of above-mentioned steps; The 3. described adsorption resin column of step adopts a kind of in the macroporous adsorptive resins such as D201, D101, H103, X-5, NKA-II.
The 4. described adsorption resin column of above-mentioned steps adopts a kind of in the macroporous adsorptive resins such as SP825, HP-20 type.
Drying means:
Get 3～5 Kg/ dish Folium Rehmanniae and extract concentrated extract and spread out in the drip pan, set 40～60 ℃ of microwave vacuum drying sterilizer temperature of charge, running time 40～60min, vacuum degree control in-0.08～-dry under the condition of 0.09MPa, get dry extract; With broken mistake 100 orders of dried cream powder, get Folium Rehmanniae total glycosides dried cream powder and use for preparation.
In the described drying means, method for optimizing is that setting microwave vacuum drying sterilizer temperature of charge is 45～55 ℃, and be 45～55min running time.
In the described drying means, best practice is that setting microwave vacuum drying sterilizer temperature is 50 ℃, and be 50min running time.
Beneficial effect of the present invention
1, employing is carried out gradual drying at low temperature to the Radix Rehmanniae leaf total glycoside extract under vacuum condition, whole dry run gentleness, drying time lack, the rerum natura that can keep material to greatest extent, the dry products that obtains by this method have that lighter color, moisture are low, the thermal sensitivity effective ingredient keeps the characteristics many, that dissolubility is good.And the content of Folium Rehmanniae total glycosides and verbascoside all keeps stable in the dry products, and product quality improves a lot than conventional vacuum baking oven, vacuum belt type drying method.
2, this method temperature, time can accurately be set, and controllability is strong, and dry tenacity is scalable also, so the stable of technology that can strict keep dry.
To go into to dry by the fire the extractum amount big for unit when 3, dry, can reach 50kg/ time, drying time 40～60 minutes/machine, dried cream yield can reach 5～20kg, extractum proportion is not limit.
4, this method production capacity is higher than belt, box-type drying; And the equipment easy cleaning, the cross-contamination of material has been avoided, GMP compatible in no corner or spot as yet untouched by a clean-up campaign.
The inventive method is reasonable in design, Chinese medical concrete is in vacuum, enclosed environment, dry run gentleness (40 ~ 60 ℃ of operating temperatures) can keep its rerum natura to greatest extent, obtains having that moisture content is low, dissolubility good, the desciccate of characteristics such as effective ingredient reservation amount height and color and luster are good.Comparison shows that comprehensively the vacuum microwave drying technology is used for the drying of Folium Rehmanniae total glycoside extract, advantage such as have that process stabilizing, product moisture content are low, effective ingredient retention rate height and drying time are short.Whole dry run has realized Automatic Control, not only reduce labor intensity, and improved production efficiency, the more common vacuum drying oven drying means of the product quality of utilizing this method to obtain improves a lot, also be higher than belt drying, very help the follow-up preparation process of Folium Rehmanniae.
The specific embodiment
Embodiments of the invention 1:
The drying means of Folium Rehmanniae total glycoside extract is:
Extract:
1.. Folium Rehmanniae/stem and leaf directly or after pulverizing, is adopted solvent heating and refluxing extraction method or supercritical fluid extraction extraction method, extracting solution.
2.. with extracting liquid filtering, reclaim solvent and be concentrated into the concentrated solution a of relative density 1.01～1.10.
3.. a leaves standstill clarification with concentrated solution, get supernatant and pass through adsorption resin column, water elution adsorption resin column with 1～6 times of amount of resin column volume, discard water liquid, the concentration of 1～6 times of amount of reuse resin column volume is 20～96% ethanol elution, collect ethanol elution, reclaim ethanol and be concentrated into the concentrated solution b of relative density 1.01～1.10.
4.. b leaves standstill clarification with concentrated solution, get supernatant and pass through adsorption resin column, water eluting adsorption resin column is closely neutral to effusive liquid, discard water liquid, the concentration of 1～3 times of amount of reuse resin column volume is 10～20% ethanol elution, discards ethanol elution, and continuing with 1～6 times of resin column volume amount concentration is 60～96% ethanol elution, reclaim ethanol and be concentrated into the extractum of relative density 1.20～1.40, promptly get product Folium Rehmanniae total glycoside extract.
In the 1. described solvent heating and refluxing extraction of the above-mentioned steps method, solvent reflux, extract, 1～3 time under 50～100 ℃ of conditions, each 0.5～1.5 hour, merge extractive liquid.Solvent is selected for use:
(a). a kind of solvent in water, methanol, the ethanol; Perhaps
(b). a kind of in the mixed solvent that water or methanol or ethanol and acetic acid are formed, its consumption volume ratio is concentration 30～96% ethanol or concentration 30～96% methanol or water: acetic acid=80～99.99:20～0.01(V:V); Perhaps
(c). the mixed solvent that any two or more arbitrary proportions are formed in above-mentioned (a) and (b).
Described solvent preferred alcohol.
Contain 0.01～10% acetic acid (V:V) in the 3. described ethanol of above-mentioned steps; The 3. described adsorption resin column of step adopts a kind of in the macroporous adsorptive resins such as D201, D101, H103, X-5, NKA-II.
The 4. described adsorption resin column of above-mentioned steps adopts a kind of in the macroporous adsorptive resins such as SP825, HP-20 type.
Dry:
Get 3～5 Kg/ dish Folium Rehmanniae and extract concentrated extract and spread out in the drip pan, set 45 ℃ of microwave vacuum drying sterilizer temperature of charge, running time 45min, vacuum degree control in-0.08～-dry under the condition of 0.09MPa, get dry extract; With broken mistake 100 orders of dried cream powder, get Folium Rehmanniae total glycosides dried cream powder and use for preparation.
Embodiments of the invention 2:
The drying means of Folium Rehmanniae total glycoside extract is:
Extract:
1.. Folium Rehmanniae/stem and leaf directly or after pulverizing, is adopted solvent heating and refluxing extraction method or supercritical fluid extraction extraction method, extracting solution.
2.. with extracting liquid filtering, reclaim solvent and be concentrated into the concentrated solution a of relative density 1.01～1.10.
3.. a leaves standstill clarification with concentrated solution, get supernatant and pass through adsorption resin column, water elution adsorption resin column with 1～6 times of amount of resin column volume, discard water liquid, the concentration of 1～6 times of amount of reuse resin column volume is 20～96% ethanol elution, collect ethanol elution, reclaim ethanol and be concentrated into the concentrated solution b of relative density 1.01～1.10.
4.. b leaves standstill clarification with concentrated solution, get supernatant and pass through adsorption resin column, water eluting adsorption resin column is closely neutral to effusive liquid, discard water liquid, the concentration of 1～3 times of amount of reuse resin column volume is 10～20% ethanol elution, discards ethanol elution, and continuing with 1～6 times of resin column volume amount concentration is 60～96% ethanol elution, reclaim ethanol and be concentrated into the extractum of relative density 1.20～1.40, promptly get product Folium Rehmanniae total glycoside extract.
In the 1. described solvent heating and refluxing extraction of the above-mentioned steps method, solvent reflux, extract, 1～3 time under 50～100 ℃ of conditions, each 0.5～1.5 hour, merge extractive liquid.Solvent is selected for use:
(a). a kind of solvent in water, methanol, the ethanol; Perhaps
(b). a kind of in the mixed solvent that water or methanol or ethanol and acetic acid are formed, its consumption volume ratio is concentration 30～96% ethanol or concentration 30～96% methanol or water: acetic acid=80～99.99:20～0.01(V:V); Perhaps
(c). the mixed solvent that any two or more arbitrary proportions are formed in above-mentioned (a) and (b).
Described solvent preferred alcohol.
Contain 0.01～10% acetic acid (V:V) in the 3. described ethanol of above-mentioned steps; The 3. described adsorption resin column of step adopts a kind of in the macroporous adsorptive resins such as D201, D101, H103, X-5, NKA-II.
The 4. described adsorption resin column of above-mentioned steps adopts a kind of in the macroporous adsorptive resins such as SP825, HP-20 type.
Dry:
Get 3～5 Kg/ dish Folium Rehmanniae and extract concentrated extract and spread out in the drip pan, set 50 ℃ of microwave vacuum drying sterilizer temperature of charge, running time 50min, vacuum degree control in-0.08～-dry under the condition of 0.09MPa, get dry extract; With broken mistake 100 orders of dried cream powder, get Folium Rehmanniae total glycosides dried cream powder and use for preparation.
Embodiments of the invention 3:
The drying means of Folium Rehmanniae total glycoside extract is:
Extract:
1.. Folium Rehmanniae/stem and leaf directly or after pulverizing, is adopted solvent heating and refluxing extraction method or supercritical fluid extraction extraction method, extracting solution.
2.. with extracting liquid filtering, reclaim solvent and be concentrated into the concentrated solution a of relative density 1.01～1.10.
3.. a leaves standstill clarification with concentrated solution, get supernatant and pass through adsorption resin column, water elution adsorption resin column with 1～6 times of amount of resin column volume, discard water liquid, the concentration of 1～6 times of amount of reuse resin column volume is 20～96% ethanol elution, collect ethanol elution, reclaim ethanol and be concentrated into the concentrated solution b of relative density 1.01～1.10.
4.. b leaves standstill clarification with concentrated solution, get supernatant and pass through adsorption resin column, water eluting adsorption resin column is closely neutral to effusive liquid, discard water liquid, the concentration of 1～3 times of amount of reuse resin column volume is 10～20% ethanol elution, discards ethanol elution, and continuing with 1～6 times of resin column volume amount concentration is 60～96% ethanol elution, reclaim ethanol and be concentrated into the extractum of relative density 1.20～1.40, promptly get product Folium Rehmanniae total glycoside extract.
In the 1. described solvent heating and refluxing extraction of the above-mentioned steps method, solvent reflux, extract, 1～3 time under 50～100 ℃ of conditions, each 0.5～1.5 hour, merge extractive liquid.Solvent is selected for use:
(a). a kind of solvent in water, methanol, the ethanol; Perhaps
(b). a kind of in the mixed solvent that water or methanol or ethanol and acetic acid are formed, its consumption volume ratio is concentration 30～96% ethanol or concentration 30～96% methanol or water: acetic acid=80～99.99:20～0.01(V:V); Perhaps
(c). the mixed solvent that any two or more arbitrary proportions are formed in above-mentioned (a) and (b).
Described solvent preferred alcohol.
Contain 0.01～10% acetic acid (V:V) in the 3. described ethanol of above-mentioned steps; The 3. described adsorption resin column of step adopts a kind of in the macroporous adsorptive resins such as D201, D101, H103, X-5, NKA-II.
The 4. described adsorption resin column of above-mentioned steps adopts a kind of in the macroporous adsorptive resins such as SP825, HP-20 type.
Dry:
Get 3～5 Kg/ dish Folium Rehmanniae and extract concentrated extract and spread out in the drip pan, set 55 ℃ of microwave vacuum drying sterilizer temperature of charge, running time 55min, vacuum degree control in-0.08～-dry under the condition of 0.09MPa, get dry extract; With broken mistake 100 orders of dried cream powder, get Folium Rehmanniae total glycosides dried cream powder and use for preparation.
Claims (3)
1. the drying means of a Folium Rehmanniae total glycoside extract, it is characterized in that: described drying means is, getting 3～5 Kg/ dish Folium Rehmanniae extraction concentrated extract spreads out in the drip pan, set 40～60 ℃ of microwave vacuum drying sterilizer temperature of charge, running time 40～60min, vacuum degree control in-0.08～-dry under the condition of 0.09MPa, get dry extract; With broken mistake 100 orders of dried cream powder, get Folium Rehmanniae total glycosides dried cream powder and use for preparation.
2. the drying means of Folium Rehmanniae total glycoside extract according to claim 1 is characterized in that: in the described drying means, setting microwave vacuum drying sterilizer temperature of charge is 45～55 ℃, and be 45～55min running time.
3. the drying means of Folium Rehmanniae total glycoside extract according to claim 1 is characterized in that: in the described drying means, setting microwave vacuum drying sterilizer temperature is 50 ℃, and be 50min running time.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104666585A (en) * | 2015-03-16 | 2015-06-03 | 河南中医学院 | Application of radix rehmanniae leaf extract in preparation of blood glucose-reducing medicines |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1947757A (en) * | 2006-09-16 | 2007-04-18 | 四川美大康药业股份有限公司 | Leave of glutinous rehmannia extractive, its prepn. method and use, medicines prepd. with said extractives |
| CN101700314A (en) * | 2009-11-13 | 2010-05-05 | 四川美大康药业股份有限公司 | Traditional Chinese medicine extract drying method for preparing drug for curing osteoporosis |
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- 2010-11-19 CN CN 201010551372 patent/CN102000199A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1947757A (en) * | 2006-09-16 | 2007-04-18 | 四川美大康药业股份有限公司 | Leave of glutinous rehmannia extractive, its prepn. method and use, medicines prepd. with said extractives |
| CN101700314A (en) * | 2009-11-13 | 2010-05-05 | 四川美大康药业股份有限公司 | Traditional Chinese medicine extract drying method for preparing drug for curing osteoporosis |
Non-Patent Citations (1)
| Title |
|---|
| 《能源研究与信息》 20031231 严平等 真空微波低温干燥技术探讨 242-246 1-3 第19卷, 第4期 2 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104666585A (en) * | 2015-03-16 | 2015-06-03 | 河南中医学院 | Application of radix rehmanniae leaf extract in preparation of blood glucose-reducing medicines |
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Open date: 20110406 |