CN105456735A - Method for improving leaching rate of alkaloid component in dendrobium stem - Google Patents
Method for improving leaching rate of alkaloid component in dendrobium stem Download PDFInfo
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- CN105456735A CN105456735A CN201510931335.XA CN201510931335A CN105456735A CN 105456735 A CN105456735 A CN 105456735A CN 201510931335 A CN201510931335 A CN 201510931335A CN 105456735 A CN105456735 A CN 105456735A
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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
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Abstract
The invention discloses a method for improving the leaching rate of alkaloid component in dendrobium stem. The method comprises the steps of pretreatment, extraction and aftertreatment, and specifically comprises the following steps: cleaning up raw material fresh dendrobium stem strips, airing, drying, slitting, carrying out puffing for wall breaking, adding with an organic solvent for extraction, mixing extracting solutions, filtering and concentrating for obtaining extract c; and drying and smashing the extract, and screening the extract by a sieve to obtain a target extract. The method has the advantages that the investment on production equipment is small, the technological operation is simple, the conditions are easily achieved, a preparation process is low in energy consumption and cost, and the processing is convenient; the alkaloid component in the prepared dendrobium stem product is leached out easily, and thus the leaching rate of the alkaloid component in dendrobium stem is improved.
Description
Technical field
The invention belongs to Chinese drug preparation technique field, be specifically related to a kind of method improving alkaloid component leaching rate in Dendrobium nobile.
Background technology
Dendrobium nobile
dendrobiumnobilelindl. be the fresh or dry stem of the orchid family Dendrobium Sw, the ground such as main product Yunnan Province of China, Guizhou, Sichuan, Guangxi, Mt. Funiushan In Henan Province.Dendrobium nobile is one of 2010 editions " Chinese Pharmacopoeias " medicinal dendrobium of recording, another name bracketplant, is used as medicine with stem, cold in nature, sweet in the mouth, the effects such as tool reinforcing stomach reg fluid, nourishing YIN and clearing away heat, are used for the treatment of the disease such as consumption of body fluid caused by febrile disease, xerostomia excessive thirst, after being ill deficiency-heat, tongue light few tongue, lack of appetite retch, poor vision.Modern pharmacological research shows that Dendrobium nobile mainly contains immunomodulating, defying age, contraction intestinal tube, anti-cataract, antitumor, antimutagenic, antibacterial and antioxidation.Its chemical composition mainly contains polysaccharide, alkaloid, bibenzyl, luxuriant and rich with fragrance class, sesquiterpene glucoside, volatile oil and steroidal.Wherein alkaloid is one of main physiologically active ingredient of Dendrobium nobile, has analgesia, refrigeration function, can reduce heart rate, blood pressure and breathing of slowing down.So far from Dendrobium nobile, separating dendrobium alkali, Ephemerantha lonchophylla (Hook. F) Hunt et Sum-merh. [Ephemerantha fimbrate (Bl.) Hunt et Summerh. alkali, Herba Dendrobii ammonia alkali, Herba Dendrobii magnitude more than 10 plant alkaloid.Patents is had to relate to alkaloidal extractive technique in Dendrobium Sw at present, patent " a kind of preparation method (201010557842.9) of dendrobine " provides a kind of ultrasonic assistant and extracts alkaloidal method in Herba Dendrobii, patent " a kind of method of purification (201310194424.1) of dendrobine " provides a kind of alkaloidal method in co_2 supercritical fluid extraction Herba Dendrobii, the patent method (201010300497.0) of extraction purification dendrobine " from the Dendrobium nobile " provides a kind of alkaloidal method in acidic ethanol extraction Herba Dendrobii, patent " a kind of method (201410694535.3) extracting dendrobine from Herba Dendrobii " provides a kind of alkaloidal method in aqueous acid soak extraction Herba Dendrobii, patent " a kind of method (201410816877.8) preparing content more than 95% dendrobine " provides a kind of alkaloidal method in alcohol reflux Herba Dendrobii.The most extraction ratio of these preparation methoies is low, extraction cost is high, complex operation.Therefore, develop a kind of method that can solve the problems of the technologies described above to be very important.
Summary of the invention
The object of the present invention is to provide a kind of method improving alkaloid component leaching rate in Dendrobium nobile.
The object of the present invention is achieved like this, comprises pre-treatment, extraction, post-processing step, specifically comprise:
A, pre-treatment:
1) fresh for raw material Dendrobium nobile bar is cleaned up, dried, being placed in 85 ~ 95 DEG C of drying 3.5 ~ 4.0h is 15 ~ 25% to moisture content, is cut into the billet a of 3.5 ~ 4.0cm;
2) billet a was pulverized after expanded breaking cellular wall 100 ~ 300 mesh sieves to obtain expecting that b is for subsequent use before Dendrobium nobile extracts;
B, extraction: before adding Dendrobium nobile extraction in material b before Dendrobium nobile step A process obtained extracts, the organic solvent of material b weight ratio 4 ~ 8 times extracts 3 ~ 4 times in 55 ~ 74 DEG C, each 1 ~ 3h, merge extractive liquid, filters, concentrated obtains the extractum c that relative density is 1.1 ~ 1.3;
C, post processing: by the extractum c drying of extraction, pulverize and sieve and obtain Objective extraction thing.
Beneficial effect of the present invention is, the Dendrobium nobile goods expansion rate utilizing the production and processing of microwave bulking breaking cellular wall method to obtain is high, cell wall breaking is effective, its alkaloid component is easy to leach, improve the leaching rate of alkaloid component in Dendrobium nobile, thus substantially increase the bioavailability of Dendrobium nobile, enhance the health care of Dendrobium nobile.The method small investment of production equipment, technological operation is simple, and condition easily reaches, and preparation process energy consumption is low, and cost is low, easy to process.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is further illustrated, but limited the present invention never in any form, and any conversion done based on training centre of the present invention or replacement, all belong to protection scope of the present invention.
The present invention improves the method for alkaloid component leaching rate in Dendrobium nobile, comprises pre-treatment, extraction, post-processing step, specifically comprises:
A, pre-treatment:
1) fresh for raw material Dendrobium nobile bar is cleaned up, dried, being placed in 85 ~ 95 DEG C of drying 3.5 ~ 4.0h is 15 ~ 25% to moisture content, is cut into the billet a of 3.5 ~ 4.0cm;
2) billet a was pulverized after expanded breaking cellular wall 100 ~ 300 mesh sieves to obtain expecting that b is for subsequent use before Dendrobium nobile extracts;
B, extraction: before adding Dendrobium nobile extraction in material b before Dendrobium nobile step A process obtained extracts, the organic solvent of material b weight ratio 4 ~ 8 times extracts 3 ~ 4 times in 55 ~ 74 DEG C, each 1 ~ 3h, merge extractive liquid, filters, concentrated obtains the extractum c that relative density is 1.1 ~ 1.3;
C, post processing: by the extractum c drying of extraction, pulverize and sieve and obtain Objective extraction thing.
Moisture content described in step A is 20 ~ 25%.
Expanded breaking cellular wall described in step A adopts microwave bulking breaking cellular wall.
The power of described expanded breaking cellular wall is 650 ~ 750w, and the time of expanded breaking cellular wall is 30 ~ 40s.
Organic solvent described in step B is chloroform, methanol, ethanol or acetone.
Being extracted as dipping or refluxing described in step B.
With concrete case study on implementation, the present invention is further described below:
The information of the unit type that various embodiments of the present invention are used and manufacturer is as follows:
Microwave oven (M-NJL07-3, the long-range Science and Technology Ltd. in Chinese and Western, Beijing); Electric drying oven with forced convection (DHG-9070, Shanghai one Shanghai Yiheng Scientific Instruments Co., Ltd of permanent Science and Technology Ltd.).
Assay method the present invention being prepared to alkaloid component content in Objective extraction thing is as follows:
(1) preparation of standard curve: essence claims dendrobine reference substance 1mg, puts 100ml volumetric flask, adds chloroform to scale.Essence gets 1.0,2.0,3.0,4.0,5.0ml is placed in separatory funnel respectively, 10.0ml is diluted to chloroform, add pH4.5 buffer 5.0ml and 0.04% bromocresol green solution 2.0ml, violent jolting 3 minutes, leave standstill 30 minutes, chloroform layer is filtered by the absorbent cotton also dry through chloroform immersion treatment.Get subsequent filtrate 5.0ml, add 0.01molL-1 sodium hydroxide ethanol solution 1.0ml, shake up.With chloroform 10.0ml, with method operation, as blank, record trap with ultraviolet-visible spectrophotometer in 620nm place.Take absorbance as vertical coordinate, concentration is abscissa drawing standard curve.
(2) sample solution preparation and mensuration: get various sample coarse powder 0.2g, with appropriate ammonia (5 dropper) moistening close plug 30min, precision adds chloroform 20ml and weighs, heating in water bath backflow 2h, after cooling, chloroform supplies weightlessness, filters, essence gets subsequent filtrate 10ml in separatory funnel, as sample liquid.Method under sighting target directrix curve preparation, measures absorbance in accordance with the law, tests parallel 3 times from " adding pH4.5 buffer 5.0ml ".
Comparative example:
A, fresh for fresh Dendrobium nobile bar to be cleaned up, dry;
B, that the fresh bar of Dendrobium nobile that A walks is placed in drying baker is dry;
C, by B walk the expanded breaking cellular wall of Dendrobium nobile billet screw food extruder or other conventional wall-breaking method breaking cellular walls and get final product;
D, the breaking cellular wall part cooling walked by C, pack through pulverizing (crossing 200 mesh sieves) and get final product.
The chloroform solvent adding 60 milliliters in E, the Dendrobium nobile powder (10 grams) that obtains in D step process extracts 3 times in 60 DEG C, each 3h, merge extractive liquid, filters, concentratedly obtains the extractum that relative density is 1.2;
F, the extractum that E step process obtained after dry 10 hours, pulverize and sieve at 60 DEG C, and (crossing 200 mesh sieves) obtains Objective extraction thing.
After measured, before the expanded breaking cellular wall of Dendrobium nobile, alkaloidal stripping quantity accounts for 0.30% of sample total amount, and the alkaloidal stripping quantity after above-mentioned various wall-breaking method breaking cellular wall accounts for 0.33 ~ 0.37% of sample total amount.
Embodiment 1
A, fresh for fresh Dendrobium nobile bar to be cleaned up, dry;
B, the fresh bar of Dendrobium nobile that A walks is placed in drying baker, at 90 DEG C dry 3.7 hours, makes its moisture be 20%, be cut into the billet of 3.7 centimetres;
C, by B walk Dendrobium nobile billet microwave bulking breaking cellular wall and get final product; The process conditions of described microwave bulking breaking cellular wall are power 700 watts, and expanded broken time is 35 seconds, obtain expanded breaking cellular wall goods;
D, the expanded breaking cellular wall part cooling after 10 minutes walked by C, pack through pulverizing (crossing 200 mesh sieves) and get final product.
The chloroform solvent adding 60 milliliters in E, the Dendrobium nobile powder (10 grams) that obtains in D step process extracts 3 times in 60 DEG C, each 3h, merge extractive liquid, filters, concentratedly obtains the extractum that relative density is 1.2;
F, the extractum that E step process obtained after dry 10 hours, pulverize and sieve at 60 DEG C, and (crossing 200 mesh sieves) obtains Objective extraction thing.
After measured, the stripping quantity of Dendrobium nobile expanded breaking cellular wall artifact alkali accounts for 0.46% of sample total amount, and the alkaloidal stripping quantity of stripping quantity opposing compression expanded breaking cellular wall method or other conventional breaking cellular wall method breaking cellular walls adds 24.3 ~ 39.4%.
Embodiment 2
A, fresh for fresh Dendrobium nobile bar to be cleaned up, dry;
B, the fresh bar of Dendrobium nobile that A walks is placed in drying baker, at 85 DEG C dry 4.0 hours, makes its moisture be 25%, be cut into the billet of 3.5 centimetres;
C, by B walk Dendrobium nobile billet microwave bulking breaking cellular wall and get final product; The process conditions of described microwave bulking breaking cellular wall are power 650w, and expanded broken time is 40 seconds, obtain expanded breaking cellular wall goods;
D, the expanded breaking cellular wall part cooling after 13 minutes walked by C, pack through pulverizing (crossing 300 mesh sieves) and get final product.
The alcohol solvent adding 80 milliliters in E, the Dendrobium nobile powder (10 grams) that obtains in D step process extracts 3 times in 74 DEG C, each 3h, merge extractive liquid, filters, concentratedly obtains the extractum that relative density is 1.3;
F, the extractum that E step process obtained after dry 8 hours, pulverize and sieve at 60 DEG C, and (crossing 300 mesh sieves) obtains Objective extraction thing.
After measured, the stripping quantity of Dendrobium nobile expanded breaking cellular wall artifact alkali accounts for 0.43% of sample total amount, and the alkaloidal stripping quantity of stripping quantity opposing compression expanded breaking cellular wall method or other conventional breaking cellular wall method breaking cellular walls adds 16.2 ~ 30.3%.
Embodiment 3
A, fresh for fresh Dendrobium nobile bar to be cleaned up, dry;
B, the fresh bar of Dendrobium nobile that A walks is placed in drying baker, at 95 DEG C dry 3.5 hours, makes its moisture be 15%, be cut into the billet of 4.0 centimetres;
C, by B walk Dendrobium nobile billet microwave bulking breaking cellular wall and get final product; The process conditions of described microwave bulking breaking cellular wall are power 750w, and expanded broken time is 30 seconds, obtain expanded breaking cellular wall goods;
D, the expanded breaking cellular wall part cooling after 15 minutes walked by C, pack through pulverizing (crossing 100 mesh sieves) and get final product.
The methanol solvate adding 40 milliliters in E, the Dendrobium nobile powder (10 grams) that obtains in D step process extracts 3 times in 64 DEG C, each 1h, merge extractive liquid, filters, concentratedly obtains the extractum that relative density is 1.1;
F, the extractum that E step process obtained after dry 6 hours, pulverize and sieve at 60 DEG C, and (crossing 100 mesh sieves) obtains Objective extraction thing.
After measured, the stripping quantity of Dendrobium nobile expanded breaking cellular wall artifact alkali accounts for 0.45% of sample total amount, and the alkaloidal stripping quantity of stripping quantity opposing compression expanded breaking cellular wall method or other conventional breaking cellular wall method breaking cellular walls adds 21.6 ~ 36.4%.
Embodiment 4
A, fresh for fresh Dendrobium nobile bar to be cleaned up, dry;
B, the fresh bar of Dendrobium nobile that A walks is placed in drying baker, at 90 DEG C dry 3.7 hours, makes its moisture be 20%, be cut into the billet of 3.7 centimetres;
C, by B walk Dendrobium nobile billet microwave bulking breaking cellular wall and get final product; The process conditions of described microwave bulking breaking cellular wall are power 700 watts, and expanded broken time is 35 seconds, obtain expanded breaking cellular wall goods;
D, the expanded breaking cellular wall part cooling after 10 minutes walked by C, pack through pulverizing (crossing 200 mesh sieves) and get final product.
The acetone solvent adding 60 milliliters in E, the Dendrobium nobile powder (10 grams) that obtains in D step process extracts 3 times in 55 DEG C, each 3h, merge extractive liquid, filters, concentratedly obtains the extractum that relative density is 1.2;
F, the extractum that E step process obtained after dry 10 hours, pulverize and sieve at 60 DEG C, and (crossing 200 mesh sieves) obtains Objective extraction thing.
After measured, the stripping quantity of Dendrobium nobile expanded breaking cellular wall artifact alkali accounts for 0.44% of sample total amount, and the alkaloidal stripping quantity of stripping quantity opposing compression expanded breaking cellular wall method or other conventional breaking cellular wall method breaking cellular walls adds 18.9 ~ 33.3%.
More than show and describe ultimate principle of the present invention, principal character and advantage of the present invention.The technical staff of the industry should understand; the present invention is not restricted to the described embodiments; what describe in above-described embodiment and description just illustrates principle of the present invention; do not departing from the prerequisite of spirit and scope of the invention; the present invention also has various changes and modifications, and these changes and improvements all fall in the claimed scope of the invention.Application claims protection domain is defined by appending claims and equivalent thereof.
Claims (6)
1. improve a method for alkaloid component leaching rate in Dendrobium nobile, it is characterized in that comprising pre-treatment, extraction, post-processing step, specifically comprise:
A, pre-treatment:
1) fresh for raw material Dendrobium nobile bar is cleaned up, dried, being placed in 85 ~ 95 DEG C of drying 3.5 ~ 4.0h is 15 ~ 25% to moisture content, is cut into the billet a of 3.5 ~ 4.0cm;
2) billet a was pulverized after expanded breaking cellular wall 100 ~ 300 mesh sieves to obtain expecting that b is for subsequent use before Dendrobium nobile extracts;
B, extraction: before adding Dendrobium nobile extraction in material b before Dendrobium nobile step A process obtained extracts, the organic solvent of material b weight ratio 4 ~ 8 times extracts 3 ~ 4 times in 55 ~ 74 DEG C, each 1 ~ 3h, merge extractive liquid, filters, concentrated obtains the extractum c that relative density is 1.1 ~ 1.3;
C, post processing: by the extractum c drying of extraction, pulverize and sieve and obtain Objective extraction thing.
2. the method for alkaloid component leaching rate in raising Dendrobium nobile according to claim 1, is characterized in that the moisture content described in step A is 20 ~ 25%.
3. the method for alkaloid component leaching rate in raising Dendrobium nobile according to claim 1, is characterized in that the expanded breaking cellular wall described in step A adopts microwave bulking breaking cellular wall.
4. the method for alkaloid component leaching rate in the raising Dendrobium nobile according to claim 1 or 3, is characterized in that the power of described expanded breaking cellular wall is 650 ~ 750w, and the time of expanded breaking cellular wall is 30 ~ 40s.
5. the method for alkaloid component leaching rate in raising Dendrobium nobile according to claim 1, is characterized in that the organic solvent described in step B is chloroform, methanol, ethanol or acetone.
6. the method for alkaloid component leaching rate in raising Dendrobium nobile according to claim 1, is characterized in that being extracted as dipping or backflow described in step B.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108244433A (en) * | 2018-01-26 | 2018-07-06 | 合肥工业大学 | A kind of preparation method for improving the fresh middle total alkaloid stripping quantity of squeezing the juice of the stem of noble dendrobium |
| 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 |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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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2015
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Non-Patent Citations (1)
| Title |
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| 黄小燕等: ""正交试验法优化金钗石斛生物碱的提取工艺"", 《贵州师范大学学报（自然科学版）》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108244433A (en) * | 2018-01-26 | 2018-07-06 | 合肥工业大学 | A kind of preparation method for improving the fresh middle total alkaloid stripping quantity of squeezing the juice of the stem of noble dendrobium |
| 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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