CN105456735B - A kind of method of alkaloid component leaching rate in raising HERBA DENDROBII - Google Patents
A kind of method of alkaloid component leaching rate in raising HERBA DENDROBII Download PDFInfo
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- CN105456735B CN105456735B CN201510931335.XA CN201510931335A CN105456735B CN 105456735 B CN105456735 B CN 105456735B CN 201510931335 A CN201510931335 A CN 201510931335A CN 105456735 B CN105456735 B CN 105456735B
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- herba dendrobii
- leaching rate
- alkaloid component
- extraction
- broken wall
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/88—Liliopsida (monocotyledons)
- A61K36/898—Orchidaceae (Orchid family)
- A61K36/8984—Dendrobium
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/10—Preparation or pretreatment of starting material
- A61K2236/15—Preparation or pretreatment of starting material involving mechanical treatment, e.g. chopping up, cutting or grinding
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/35—Extraction with lipophilic solvents, e.g. Hexane or petrol ether
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/39—Complex extraction schemes, e.g. fractionation or repeated extraction steps
Abstract
The invention discloses a kind of methods of alkaloid component leaching rate in raising HERBA DENDROBII, including pre-treatment, extraction, post-processing step, specifically the fresh HERBA DENDROBII item of raw material is cleaned up, is dried, it is dry, slitting, extruding broken wall are added organic solvent and extract, combined extract filters, is concentrated to get medicinal extract c；By the medicinal extract of extraction, medicinal extract through drying, pulverize and sieve to obtain Objective extraction object.Small investment of production equipment of the present invention, technological operation is simple, and condition is easy to reach, and low energy consumption for preparation process, at low cost, easy to process；Alkaloid component in the HERBA DENDROBII product of preparation is easy to leach, and improves the leaching rate of alkaloid component in HERBA DENDROBII.
Description
Technical field
The invention belongs to drug preparation technique fields, and in particular to alkaloid component leaching rate in a kind of raising HERBA DENDROBII
Method.
Background technique
HERBA DENDROBIIDendrobium nobile It Lindl. is the fresh of orchid family Dendrobium Sw or dry stem, main product
The ground such as Yunnan Province of China, Guizhou, Sichuan, Guangxi, Mt. Funiushan In Henan Province.It is medicinal that HERBA DENDROBII is that 2010 editions " Chinese Pharmacopoeias " record
One of dendrobium nobile, alias bracketplant, is used as medicine with stem, cold in nature, sweet in flavor, tool reinforcing stomach reg fluid, nourishing Yin and clearing heat and other effects, for treating pyreticosis
Hurt saliva, dry polydipsia, after being ill abnormal heat, tongue light less fur, deficiency of food retch, the dark diseases such as unknown of mesh.Modern pharmacological studies have shown that golden hairpin stone
Dry measure used in former times mainly has immunological regulation, anti-aging, shrinks intestinal tube, anti-cataract, antitumor, anti-mutagenesis, antibacterial and antioxidation.It is changed
Studying point mainly has polysaccharide, alkaloid, bibenzyl, luxuriant and rich with fragrance class, sequiterpene glucoside, volatile oil and steroidal.Wherein alkaloid is
One of main physiologically active ingredient of HERBA DENDROBII has analgesia, refrigeration function, can reduce heart rate, blood pressure and slow down breathing.Extremely
Modern more than 10 alkaloids such as separating dendrobium alkali, HERBA DENDROBII alkali, dendrobium nobile ammonia alkali, dendroxine from HERBA DENDROBII.There is correlation at present
Patent is related to the extractive technique of alkaloid in Dendrobium Sw, a kind of patent " preparation method of dendrobine
(201010557842.9) " a kind of method of alkaloid in ultrasonic wave assisted extraction dendrobium nobile is provided, patent be " a kind of dendrobine
Method of purification (201310194424.1) " provides a kind of method of alkaloid in co_2 supercritical fluid extraction dendrobium nobile,
Patent " method (201010300497.0) of extraction purification dendrobine from HERBA DENDROBII " provides a kind of acidic ethanol extraction
The method of alkaloid in dendrobium nobile, patent " a kind of method (201410694535.3) that dendrobine is extracted from dendrobium nobile " provide one
The method of alkaloid in kind aqueous acid soak extraction dendrobium nobile, patent " a method of prepare 95% or more dendrobine of content
(201410816877.8) " a kind of method that alcohol reflux extracts alkaloid in dendrobium nobile is provided.These preparation methods mention mostly
Take that rate is low, extraction cost is high, complex operation.Therefore, developing a kind of method that can solve above-mentioned technical problem is very must
It wants.
Summary of the invention
The purpose of the present invention is to provide a kind of methods of alkaloid component leaching rate in raising HERBA DENDROBII.
The object of the present invention is achieved like this, including pre-treatment, extraction, post-processing step, specifically includes:
A, pre-treatment:
1) the fresh HERBA DENDROBII item of raw material cleaned up, dried, being placed in 85 ~ 95 DEG C of dry 3.5 ~ 4.0h to moisture content is
15 ~ 25%, it is cut into the billet a of 3.5 ~ 4.0cm；
2) billet a crushed to 100 ~ 300 meshes to obtain expecting that b is spare before HERBA DENDROBII extracts after extruding broken wall；
B, it extracts: being added before HERBA DENDROBII extracts in material b before the HERBA DENDROBII that step A is handled extracts and expect b weight
Organic solvent than 4 ~ 8 times extracts 3 ~ 4 times in 55 ~ 74 DEG C, and 1 ~ 3h, combined extract, filter, are concentrated to get relative density every time
For 1.1 ~ 1.3 medicinal extract c；
C, post-process: by the medicinal extract c of extraction through drying, pulverize and sieve to obtain Objective extraction object.
The beneficial effects of the present invention are the HERBA DENDROBII product extrudings produced and processed using microwave bulking broken wall method
Rate is high, and breaking-wall cell effect is good, and alkaloid component is easy to leach, and improves the leaching of alkaloid component in HERBA DENDROBII
Rate enhances the healthcare function of HERBA DENDROBII to substantially increase the bioavilability of HERBA DENDROBII.This method production equipment
Small investment, technological operation is simple, and condition is easy to reach, and low energy consumption for preparation process, at low cost, easy to process.
Specific embodiment
Below with reference to embodiment, the present invention is further illustrated, but the present invention is limited in any way,
Based on present invention teach that it is made it is any transform or replace, all belong to the scope of protection of the present invention.
The method that the present invention improves alkaloid component leaching rate in HERBA DENDROBII, including pre-treatment, extraction, post-processing step
Suddenly, it specifically includes:
A, pre-treatment:
1) the fresh HERBA DENDROBII item of raw material cleaned up, dried, being placed in 85 ~ 95 DEG C of dry 3.5 ~ 4.0h to moisture content is
15 ~ 25%, it is cut into the billet a of 3.5 ~ 4.0cm；
2) billet a crushed to 100 ~ 300 meshes to obtain expecting that b is spare before HERBA DENDROBII extracts after extruding broken wall；
B, it extracts: being added before HERBA DENDROBII extracts in material b before the HERBA DENDROBII that step A is handled extracts and expect b weight
Organic solvent than 4 ~ 8 times extracts 3 ~ 4 times in 55 ~ 74 DEG C, and 1 ~ 3h, combined extract, filter, are concentrated to get relative density every time
For 1.1 ~ 1.3 medicinal extract c；
C, post-process: by the medicinal extract c of extraction through drying, pulverize and sieve to obtain Objective extraction object.
Moisture content described in step A is 20 ~ 25%.
Extruding broken wall described in step A is using microwave bulking broken wall.
The power of the extruding broken wall is 650 ~ 750w, and the time of extruding broken wall is 30 ~ 40s.
Organic solvent described in step B is chloroform, methanol, ethyl alcohol or acetone.
It is extracted as impregnating described in step B or flow back.
Case is embodied, invention is further explained below:
Device model used in various embodiments of the present invention and the information of manufacturer are as follows:
Micro-wave oven (M-NJL07-3, the long-range Science and Technology Ltd. in Beijing Chinese and Western)；Electric drying oven with forced convection (DHG-9070, on
Shanghai Yiheng Scientific Instruments Co., Ltd, Hai Yiheng Science and Technology Ltd.).
The measuring method that alkaloid component content in Objective extraction object is prepared to the present invention is as follows:
(1) preparation of standard curve: essence claims dendrobine reference substance 1mg, sets 100ml volumetric flask, chlorination is imitated to scale.Essence takes
1.0,2.0,3.0,4.0,5.0ml is respectively placed in separatory funnel, is diluted to 10.0ml with chloroform, pH4.5 buffer is added
5.0ml and 0.04% bromocresol green solution 2.0ml, acutely shaking 3 minutes, stand 30 minutes, and chloroform layer is by through chloroform immersion
The absorbent cotton filtration managed and dried.Subsequent filtrate 5.0ml is taken, adds 0.01molL-1 sodium hydroxide ethanol solution 1.0ml, shakes
It is even.With chloroform 10.0ml, is operated with method, as blank control, measure absorption at 620nm with ultraviolet-visible spectrophotometer
Degree.It is that abscissa draws standard curve using absorbance as ordinate, concentration.
(2) sample solution preparation and measurement: taking various sample coarse powder 0.2g, soaks close plug with suitable ammonium hydroxide (5 dropper)
Chloroform 20ml weighing is added in 30min, precision, and heating water bath reflux 2h, after cooling, chloroform supplies weightlessness, and filtering, essence takes subsequent filtrate
10ml is in separatory funnel, as sample liquid.Method under sighting target directrix curve preparation, from " pH4.5 buffer 5.0ml is added "
It rises and measures absorbance in accordance with the law, test parallel 3 times.
Comparative example:
A, the fresh fresh item of HERBA DENDROBII is cleaned up, is dried；
B, the A fresh item of HERBA DENDROBII walked is placed in drying box dry；
C, the HERBA DENDROBII billet screw food extruder extruding broken wall of B step or other conventional wall-breaking methods are broken
Wall to obtain the final product；
D, the broken wall part cooling for walking C is crushed and (crosses 200 meshes) and packed to obtain the final product.
E, 60 milliliters of chloroform solvent is added in the HERBA DENDROBII powder (10 grams) that D step process obtains to extract in 60 DEG C
3 times, each 3h, combined extract filters, is concentrated to get the medicinal extract that relative density is 1.2；
F, it after the medicinal extract for obtaining E step process is dried 10 hours at 60 DEG C, pulverizes and sieves and (crosses 200 meshes) and obtain
Objective extraction object.
After measured, the amount of dissolution of alkaloid accounts for the 0.30% of sample total amount before HERBA DENDROBII extruding broken wall, above-mentioned various broken walls
The amount of dissolution of alkaloid after method broken wall accounts for the 0.33 ~ 0.37% of sample total amount.
Embodiment 1
A, the fresh fresh item of HERBA DENDROBII is cleaned up, is dried；
B, the A fresh item of HERBA DENDROBII walked is placed in drying box, it is 3.7 hours dry at 90 DEG C, make its moisture content
20%, it is cut into 3.7 centimetres of billet；
C, by B step HERBA DENDROBII billet with microwave bulking broken wall to obtain the final product；The process conditions of the microwave bulking broken wall are
700 watts of power, extruding broken time is 35 seconds, obtains extruding broken wall product；
D, it after ten minutes by the extruding broken wall part cooling of C step, is crushed and (crosses 200 meshes) and packed to obtain the final product.
E, 60 milliliters of chloroform solvent is added in the HERBA DENDROBII powder (10 grams) that D step process obtains to extract in 60 DEG C
3 times, each 3h, combined extract filters, is concentrated to get the medicinal extract that relative density is 1.2；
F, it after the medicinal extract for obtaining E step process is dried 10 hours at 60 DEG C, pulverizes and sieves and (crosses 200 meshes) and obtain
Objective extraction object.
After measured, the amount of dissolution of alkaloid accounts for the 0.46% of sample total amount after HERBA DENDROBII extruding broken wall, and the amount of dissolution is squeezed relatively
The amount of dissolution of the alkaloid of pressure extruding broken wall method or other conventional broken wall method broken walls increases 24.3 ~ 39.4%.
Embodiment 2
A, the fresh fresh item of HERBA DENDROBII is cleaned up, is dried；
B, the A fresh item of HERBA DENDROBII walked is placed in drying box, it is 4.0 hours dry at 85 DEG C, make its moisture content
25%, it is cut into 3.5 centimetres of billet；
C, by B step HERBA DENDROBII billet with microwave bulking broken wall to obtain the final product；The process conditions of the microwave bulking broken wall are
Power 650w, extruding broken time are 40 seconds, obtain extruding broken wall product；
D, it by after extruding broken wall part cooling 13 minutes of C step, is crushed and (crosses 300 meshes) and packed to obtain the final product.
E, 80 milliliters of alcohol solvent is added in the HERBA DENDROBII powder (10 grams) that D step process obtains to extract in 74 DEG C
3 times, each 3h, combined extract filters, is concentrated to get the medicinal extract that relative density is 1.3；
F, it after the medicinal extract for obtaining E step process is dried 8 hours at 60 DEG C, pulverizes and sieves and (crosses 300 meshes) and obtain mesh
Mark extract.
After measured, the amount of dissolution of alkaloid accounts for the 0.43% of sample total amount after HERBA DENDROBII extruding broken wall, and the amount of dissolution is squeezed relatively
The amount of dissolution of the alkaloid of pressure extruding broken wall method or other conventional broken wall method broken walls increases 16.2 ~ 30.3%.
Embodiment 3
A, the fresh fresh item of HERBA DENDROBII is cleaned up, is dried；
B, the A fresh item of HERBA DENDROBII walked is placed in drying box, it is 3.5 hours dry at 95 DEG C, make its moisture content
15%, it is cut into 4.0 centimetres of billet；
C, by B step HERBA DENDROBII billet with microwave bulking broken wall to obtain the final product；The process conditions of the microwave bulking broken wall are
Power 750w, extruding broken time are 30 seconds, obtain extruding broken wall product；
D, it by after extruding broken wall part cooling 15 minutes of C step, is crushed and (is sieved with 100 mesh sieve) and packed to obtain the final product.
E, 40 milliliters of methanol solvate is added in the HERBA DENDROBII powder (10 grams) that D step process obtains to extract in 64 DEG C
3 times, each 1h, combined extract filters, is concentrated to get the medicinal extract that relative density is 1.1；
F, the medicinal extract for obtaining E step process is at 60 DEG C after dry 6 hours, pulverizes and sieves and (sieves with 100 mesh sieve) and obtains mesh
Mark extract.
After measured, the amount of dissolution of alkaloid accounts for the 0.45% of sample total amount after HERBA DENDROBII extruding broken wall, and the amount of dissolution is squeezed relatively
The amount of dissolution of the alkaloid of pressure extruding broken wall method or other conventional broken wall method broken walls increases 21.6 ~ 36.4%.
Embodiment 4
A, the fresh fresh item of HERBA DENDROBII is cleaned up, is dried；
B, the A fresh item of HERBA DENDROBII walked is placed in drying box, it is 3.7 hours dry at 90 DEG C, make its moisture content
20%, it is cut into 3.7 centimetres of billet；
C, by B step HERBA DENDROBII billet with microwave bulking broken wall to obtain the final product；The process conditions of the microwave bulking broken wall are
700 watts of power, extruding broken time is 35 seconds, obtains extruding broken wall product；
D, it after ten minutes by the extruding broken wall part cooling of C step, is crushed and (crosses 200 meshes) and packed to obtain the final product.
E, 60 milliliters of acetone solvent is added in the HERBA DENDROBII powder (10 grams) that D step process obtains to extract in 55 DEG C
3 times, each 3h, combined extract filters, is concentrated to get the medicinal extract that relative density is 1.2；
F, it after the medicinal extract for obtaining E step process is dried 10 hours at 60 DEG C, pulverizes and sieves and (crosses 200 meshes) and obtain
Objective extraction object.
After measured, the amount of dissolution of alkaloid accounts for the 0.44% of sample total amount after HERBA DENDROBII extruding broken wall, and the amount of dissolution is squeezed relatively
The amount of dissolution of the alkaloid of pressure extruding broken wall method or other conventional broken wall method broken walls increases 18.9 ~ 33.3%.
The above shows and describes the basic principle, main features and advantages of the invention.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the above embodiments and description only describe this
The principle of invention, in the premise for not departing from spirit and scope of the invention, various changes and improvements may be made to the invention, these variations
It all fall within the protetion scope of the claimed invention with improvement.The claimed scope of the invention is by appended claims and its waits
Effect object defines.
Claims (4)
1. a kind of method for improving alkaloid component leaching rate in HERBA DENDROBII, it is characterised in that including pre-treatment, extraction, rear place
Step is managed, is specifically included:
A, pre-treatment:
1) the fresh HERBA DENDROBII item of raw material cleaned up, dried, be placed in 85 ~ 95 DEG C of dry 3.5 ~ 4.0h to moisture content be 15 ~
25%, it is cut into the billet a of 3.5 ~ 4.0cm；
2) billet a crushed after 30 ~ 40s of microwave bulking broken wall of 650 ~ 750W of power to 100 ~ 300 meshes and obtains golden hairpin stone
Material b is spare before dry measure used in former times extracts；
B, it extracts: being added before HERBA DENDROBII extracts in material b before the HERBA DENDROBII that step A is handled extracts and expect b weight ratio 4 ~ 8
Times organic solvent extracted 3 ~ 4 times in 55 ~ 74 DEG C, 1 ~ 3h, combined extract every time, filtering, being concentrated to get relative density is 1.1
~ 1.3 medicinal extract c；
C, post-process: by the medicinal extract c of extraction through drying, pulverize and sieve to obtain Objective extraction object.
2. the method according to claim 1 for improving alkaloid component leaching rate in HERBA DENDROBII, it is characterised in that step A
Described in moisture content be 20 ~ 25%.
3. the method according to claim 1 for improving alkaloid component leaching rate in HERBA DENDROBII, it is characterised in that step B
Described in organic solvent be chloroform, methanol, ethyl alcohol or acetone.
4. the method according to claim 1 for improving alkaloid component leaching rate in HERBA DENDROBII, it is characterised in that step B
Described in be extracted as impregnate or flow back.
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| CN113332383A (en) * | 2021-03-05 | 2021-09-03 | 杭州蚕宝生物技术有限公司 | Method for efficiently extracting alkaloid from dendrobium officinale |
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| CN102302156A (en) * | 2011-08-23 | 2012-01-04 | 安徽六万寨石斛开发有限公司 | Method for improving water soaking leaching rate of active ingredients of dendrobium huoshanense finished product |
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| "正交试验法优化金钗石斛生物碱的提取工艺";黄小燕等;《贵州师范大学学报（自然科学版）》;20110831;第29卷(第3期);第132-134页 |
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