CN107349247A - A kind of Radix Isatidis Optimized Extraction Process - Google Patents

A kind of Radix Isatidis Optimized Extraction Process Download PDF

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Publication number
CN107349247A
CN107349247A CN201710365797.9A CN201710365797A CN107349247A CN 107349247 A CN107349247 A CN 107349247A CN 201710365797 A CN201710365797 A CN 201710365797A CN 107349247 A CN107349247 A CN 107349247A
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Prior art keywords
water
radix isatidis
minutes
bacterium solution
fermentation
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Chinese (zh)
Inventor
苏学东
李云
王高松
李琼
胡小桂
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HUIYINBI GROUP ANHUI PHARMACEUTICAL CO Ltd
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HUIYINBI GROUP ANHUI PHARMACEUTICAL CO Ltd
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18Magnoliophyta (angiosperms)
    • A61K36/185Magnoliopsida (dicotyledons)
    • A61K36/31Brassicaceae or Cruciferae (Mustard family), e.g. broccoli, cabbage or kohlrabi
    • A61K36/315Isatis, e.g. Dyer's woad
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation 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
    • A61K2236/10Preparation or pretreatment of starting material
    • A61K2236/19Preparation or pretreatment of starting material involving fermentation using yeast, bacteria or both; enzymatic treatment
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation 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
    • A61K2236/30Extraction of the material
    • A61K2236/33Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
    • A61K2236/331Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using water, e.g. cold water, infusion, tea, steam distillation or decoction
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation 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
    • A61K2236/30Extraction of the material
    • A61K2236/39Complex extraction schemes, e.g. fractionation or repeated extraction steps
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation 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
    • A61K2236/50Methods involving additional extraction steps
    • A61K2236/51Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation 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
    • A61K2236/50Methods involving additional extraction steps
    • A61K2236/53Liquid-solid separation, e.g. centrifugation, sedimentation or crystallization

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  • Health & Medical Sciences (AREA)
  • Natural Medicines & Medicinal Plants (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Alternative & Traditional Medicine (AREA)
  • Biotechnology (AREA)
  • Botany (AREA)
  • Medical Informatics (AREA)
  • Medicinal Chemistry (AREA)
  • Microbiology (AREA)
  • Mycology (AREA)
  • Pharmacology & Pharmacy (AREA)
  • Epidemiology (AREA)
  • Animal Behavior & Ethology (AREA)
  • General Health & Medical Sciences (AREA)
  • Public Health (AREA)
  • Veterinary Medicine (AREA)
  • Medicines Containing Plant Substances (AREA)

Abstract

The present invention relates to a kind of Radix Isatidis Optimized Extraction Process, following steps are specifically included:(1)Pretreatment of raw material;(2)Water extract-alcohol precipitation operates;(3)Spray drying, obtains finished product.It is more shorter than the water extraction time in the prior art using a kind of Radix Isatidis Optimized Extraction Process provided by the invention by experiment, but it is higher to the recovery rate of active material in Radix Isatidis, the pharmacy cost of enterprise can be substantially reduced, is worth of widely use.

Description

A kind of Radix Isatidis Optimized Extraction Process
Technical field
A kind of purification technique field of bioactive substance of the present invention, and in particular to Radix Isatidis Optimized Extraction Process.
Background technology
Radix Isatidis is the dry root of cruciferae isatis, has extensive cultivation in China, is that China commonly uses for many years Heat-clearing and detoxifying drug, have antiviral, antiendotoxin, antipyretic-antalgic, anti-inflammatory, activate blood circulation and disperse blood clots, anticancer the effect of.
The technique of the extensive extraction Radix Isatidis of industrialization, is often water extraction and alcohol precipitation method, because its have it is inexpensive, simple to operate etc. Advantage, but this method extraction efficiency is low, expends time length, there is very big optimization space.
The content of the invention
In order to solve the above problems, the invention provides a kind of Radix Isatidis Optimized Extraction Process, traditional industry water is optimized Alcohol deposition method is carried, makes Radix Isatidis.
The present invention is achieved through the following technical solutions:
A kind of Radix Isatidis Optimized Extraction Process, specifically includes following steps:
(1)Pretreatment of raw material
Raw material Radix Isatidis is put into medicine-washing machine, the sodium bicarbonate aqueous solution that use quality fraction is 2% embathes 5-8 minute heel row Water, converting, clear water is secondary to embathe 1-2 minutes, filters out medicinal material, drains away the water, and is placed in medicine cutter and cuts into slices, is then fed into fermentation tank In, the compound bacteria bacterium solution of 0.3-0.6 times of Radix Isatidis mass fraction is added, 90-120 minutes are sealed by fermentation at a temperature of 20-25 DEG C, Filtered after washing, obtain fermentation medicinal material, then fermentation medicinal material is dried to water content 1% using 10-15 DEG C of cold wind cyclic drying system Hereinafter, freezing processing 45-55 minutes in -15 DEG C of freezers are subsequently placed in, are taken out after the completion of freezing processing, are ground to 80 mesh, Obtain medicinal powder;The compound bacteria bacterium solution, by lactobacillus bacterium solution, Bifidobacterium bacterium solution, Bacillus licheniformis liquid in mass ratio 5:3: It is made after 8-12 mixing;
(2)Water extract-alcohol precipitation operates
By step(1)The obtained medicinal powder is added in extractor, adds the water of the 20-25 times of medicinal powder mass fraction, is carried out Abundant water extraction, is first heated to 80-85 DEG C during water extraction, be incubated 5-10 minutes, then treats that it naturally cools to 45-50 DEG C, then Secondary 80-85 DEG C of heating, so handles 1.5-2 hours, filters to obtain filter residue and first-time filtrate, the filter residue then is used into phase repeatedly Carried with method secondary water, filtering and impurity removing obtains secondary filtrate, merges the first-time filtrate and secondary filtrate, is concentrated under reduced pressure into relatively close Degree 1.24, obtains concentrate, concentrate is slowly added into dense ethanol solution, until concentration of alcohol reaches 62-65%, stands, centrifuging and taking Supernatant, the supernatant recovery ethanol produce decoction;
(3)Spray drying, obtains finished product.
Beneficial effects of the present invention:Raw material Radix Isatidis is embathed by the sodium bicarbonate aqueous solution that mass fraction is 2%, energy The acid impurities remained in medicinal material are effectively removed, while play the effect of sterilizing, it is effective by the Radix Isatidis of cold fermentation Eliminate the impurity such as protein, lipid, facilitate subsequent purification to handle, at the same avoid fermentation temperature it is too high caused by medicine effectively into Analyze, then dried using cold wind, cryogenic freezing carries out pulverization process again, further avoid the precipitation of effective ingredient, The efficiency of follow-up water extraction operation is improved simultaneously;Using the method for alternating temperature water extraction, avoid effective ingredient and divide at high temperature Solution, while the hydrolysis of water-solubility impurity is effectively reduced, the generation of impurity is avoided, improves the recovery rate of Radix Isatidis, simultaneously The method of alternating temperature reduces heating cost, improves the economic benefit of enterprise;By experiment, a kind of plate provided by the invention is used Blue root Optimized Extraction Process, it is more shorter than the water extraction time in the prior art, but it is higher to the recovery rate of active material in Radix Isatidis, The pharmacy cost of enterprise can be substantially reduced, is worth of widely use.
Embodiment
Embodiment 1
A kind of Radix Isatidis Optimized Extraction Process, specifically includes following steps:
(1)Pretreatment of raw material
Raw material Radix Isatidis is put into medicine-washing machine, the sodium bicarbonate aqueous solution that use quality fraction is 2% embathes draining after 5 minutes, Converting, clear water is secondary to be embathed 1 minute, is filtered out medicinal material, is drained away the water, and is placed in medicine cutter and is cut into slices, is then fed into fermentation tank, adds Enter the compound bacteria bacterium solution of 0.3 times of Radix Isatidis mass fraction, be sealed by fermentation 90 minutes at a temperature of 20 DEG C, filter, must send out after washing Ferment medicinal material, then fermentation medicinal material is dried to water content below 1% using 10 DEG C of cold wind cyclic drying systems, it is subsequently placed in -15 DEG C Freezing processing 45 minutes, take out after the completion of freezing processing in freezer, grind to 80 mesh, obtain medicinal powder;The compound bacteria bacterium solution, By lactobacillus bacterium solution, Bifidobacterium bacterium solution, Bacillus licheniformis liquid in mass ratio 5:3:It is made after 8 mixing;Raw material plate is blue Root embathes by the sodium bicarbonate aqueous solution that mass fraction is 2%, can effectively remove the acid impurities remained in medicinal material, rise simultaneously To the effect of sterilizing, the Radix Isatidis by cold fermentation effectively eliminates the impurity such as protein, lipid, facilitates subsequent purification Processing, while avoid the too high caused effective ingredient of fermentation temperature from separating out, then dried using cold wind, cryogenic freezing is entered again Row pulverization process, further avoids the precipitation of effective ingredient, while improves the efficiency of follow-up water extraction operation;
(2)Water extract-alcohol precipitation operates
By step(1)The obtained medicinal powder is added in extractor, adds the water of 20 times of medicinal powder mass fractions, is carried out abundant Water extraction, 80 DEG C are first heated to during water extraction, are incubated 5 minutes, then treat that it naturally cools to 45 DEG C, heat 80 DEG C again, such as This is handled 1.5 hours repeatedly, filters to obtain filter residue and first-time filtrate, and the filter residue then is used into the secondary water extraction of same procedure, mistake Miscellaneous secondary filtrate is filtered out, merges the first-time filtrate and secondary filtrate, is concentrated under reduced pressure into relative density 1.24, obtains concentrate, Concentrate is slowly added to dense ethanol solution, until concentration of alcohol reaches 62%, stood, centrifuging and taking supernatant, the supernatant returns Receive ethanol and produce decoction;Using the method for alternating temperature water extraction, avoid effective ingredient and decompose at high temperature, while effectively reduce The hydrolysis of water-solubility impurity, avoids the generation of impurity, improves the recovery rate of Radix Isatidis, while the method for alternating temperature reduces Heating cost, improve the economic benefit of enterprise;
(3)Spray drying, obtains finished product.
Embodiment 2
A kind of Radix Isatidis Optimized Extraction Process, specifically includes following steps:
(1)Pretreatment of raw material
Raw material Radix Isatidis is put into medicine-washing machine, the sodium bicarbonate aqueous solution that use quality fraction is 2% embathes draining after 8 minutes, Converting, clear water is secondary to be embathed 2 minutes, is filtered out medicinal material, is drained away the water, and is placed in medicine cutter and is cut into slices, is then fed into fermentation tank, adds Enter the compound bacteria bacterium solution of 0.6 times of Radix Isatidis mass fraction, be sealed by fermentation 120 minutes at a temperature of 25 DEG C, filter, must send out after washing Ferment medicinal material, then fermentation medicinal material is dried to water content below 1% using 15 DEG C of cold wind cyclic drying systems, it is subsequently placed in -15 DEG C Freezing processing 55 minutes, take out after the completion of freezing processing in freezer, grind to 80 mesh, obtain medicinal powder;The compound bacteria bacterium solution, By lactobacillus bacterium solution, Bifidobacterium bacterium solution, Bacillus licheniformis liquid in mass ratio 5:3:It is made after 12 mixing;Raw material plate is blue Root embathes by the sodium bicarbonate aqueous solution that mass fraction is 2%, can effectively remove the acid impurities remained in medicinal material, rise simultaneously To the effect of sterilizing, the Radix Isatidis by cold fermentation effectively eliminates the impurity such as protein, lipid, facilitates subsequent purification Processing, while avoid the too high caused effective ingredient of fermentation temperature from separating out, then dried using cold wind, cryogenic freezing is entered again Row pulverization process, further avoids the precipitation of effective ingredient, while improves the efficiency of follow-up water extraction operation;
(2)Water extract-alcohol precipitation operates
By step(1)The obtained medicinal powder is added in extractor, adds the water of 25 times of medicinal powder mass fractions, is carried out abundant Water extraction, 85 DEG C are first heated to during water extraction, are incubated 10 minutes, then treat that it naturally cools to 50 DEG C, heat 85 DEG C again, such as This is handled 2 hours repeatedly, filters to obtain filter residue and first-time filtrate, and the filter residue then is used into the secondary water extraction of same procedure, filtering Clean to obtain secondary filtrate, merges the first-time filtrate and secondary filtrate, is concentrated under reduced pressure into relative density 1.24, obtains concentrate, will Concentrate is slowly added to dense ethanol solution, until concentration of alcohol reaches 65%, stands, centrifuging and taking supernatant, the supernatant recovery Ethanol produces decoction;Using the method for alternating temperature water extraction, avoid effective ingredient and decompose at high temperature, effectively reduce simultaneously The hydrolysis of water-solubility impurity, the generation of impurity is avoided, improve the recovery rate of Radix Isatidis, while the method for alternating temperature is reduced and added Hot cost, improve the economic benefit of enterprise;
(3)Spray drying, obtains finished product.
Comparative example 1
This comparative example 1 compared with Example 1, without step(1)The operation, using existing Radix Isatidis pretreatment side Method, method and step all same in addition.
Comparative example 2
This comparative example 2 compared with Example 2, without step(2)The operation, operated using only conventional water extract-alcohol precipitation, Method and step all same in addition.
Control group
Existing industrial Extraction Technology of Radix Isatidis.
The extraction of Radix Isatidis is carried out using above-mentioned 5 kinds of methods respectively, in the extraction time and extract that determine every kind of method The content of active component, as a result such as table 1:
Table 1
Extraction time(min) Active component content(%)
Embodiment 1 90 0.5%
Embodiment 2 120 0.6%
Comparative example 1 90 0.2%
Comparative example 2 180 0.4%
Control group 180 0.5%
As shown in Table 1, using a kind of Radix Isatidis Optimized Extraction Process provided by the invention, than the water extraction time in the prior art more It is short, but it is higher to the recovery rate of active material in Radix Isatidis, the pharmacy cost of enterprise can be substantially reduced, being worthy to be popularized makes With.

Claims (2)

1. a kind of Radix Isatidis Optimized Extraction Process, it is characterised in that specifically include following steps:
(1)Pretreatment of raw material
Raw material Radix Isatidis is put into medicine-washing machine, the sodium bicarbonate aqueous solution that use quality fraction is 2% embathes 5-8 minute heel row Water, converting, clear water is secondary to embathe 1-2 minutes, filters out medicinal material, drains away the water, and is placed in medicine cutter and cuts into slices, is then fed into fermentation tank In, the compound bacteria bacterium solution of 0.3-0.6 times of Radix Isatidis mass fraction is added, 90-120 minutes are sealed by fermentation at a temperature of 20-25 DEG C, Filtered after washing, obtain fermentation medicinal material, then fermentation medicinal material is dried to water content 1% using 10-15 DEG C of cold wind cyclic drying system Hereinafter, freezing processing 45-55 minutes in -15 DEG C of freezers are subsequently placed in, are taken out after the completion of freezing processing, are ground to 80 mesh, Obtain medicinal powder;The compound bacteria bacterium solution, by lactobacillus bacterium solution, Bifidobacterium bacterium solution, Bacillus licheniformis liquid in mass ratio 5:3: It is made after 8-12 mixing;
(2)Water extract-alcohol precipitation operates
By step(1)The obtained medicinal powder is added in extractor, adds the water of the 20-25 times of medicinal powder mass fraction, is carried out Abundant water extraction, is first heated to 80-85 DEG C during water extraction, be incubated 5-10 minutes, then treats that it naturally cools to 45-50 DEG C, then Secondary 80-85 DEG C of heating, so handles 1.5-2 hours, filters to obtain filter residue and first-time filtrate, the filter residue then is used into phase repeatedly Carried with method secondary water, filtering and impurity removing obtains secondary filtrate, merges the first-time filtrate and secondary filtrate, is concentrated under reduced pressure into relatively close Degree 1.24, obtains concentrate, concentrate is slowly added into dense ethanol solution, until concentration of alcohol reaches 62-65%, stands, centrifuging and taking Supernatant, the supernatant recovery ethanol produce decoction;
(3)Spray drying, obtains finished product.
2. a kind of Radix Isatidis Optimized Extraction Process according to claim 1, it is characterised in that specifically include following steps:
(1)Pretreatment of raw material
Raw material Radix Isatidis is put into medicine-washing machine, the sodium bicarbonate aqueous solution that use quality fraction is 2% embathes draining after 8 minutes, Converting, clear water is secondary to be embathed 2 minutes, is filtered out medicinal material, is drained away the water, and is placed in medicine cutter and is cut into slices, is then fed into fermentation tank, adds Enter the compound bacteria bacterium solution of 0.6 times of Radix Isatidis mass fraction, be sealed by fermentation 120 minutes at a temperature of 25 DEG C, filter, must send out after washing Ferment medicinal material, then fermentation medicinal material is dried to water content below 1% using 15 DEG C of cold wind cyclic drying systems, it is subsequently placed in -15 DEG C Freezing processing 55 minutes, take out after the completion of freezing processing in freezer, grind to 80 mesh, obtain medicinal powder;The compound bacteria bacterium solution, By lactobacillus bacterium solution, Bifidobacterium bacterium solution, Bacillus licheniformis liquid in mass ratio 5:3:It is made after 12 mixing;
(2)Water extract-alcohol precipitation operates
By step(1)The obtained medicinal powder is added in extractor, adds the water of 25 times of medicinal powder mass fractions, is carried out abundant Water extraction, 85 DEG C are first heated to during water extraction, are incubated 10 minutes, then treat that it naturally cools to 50 DEG C, heat 85 DEG C again, such as This is handled 2 hours repeatedly, filters to obtain filter residue and first-time filtrate, and the filter residue then is used into the secondary water extraction of same procedure, filtering Clean to obtain secondary filtrate, merges the first-time filtrate and secondary filtrate, is concentrated under reduced pressure into relative density 1.24, obtains concentrate, will Concentrate is slowly added to dense ethanol solution, until concentration of alcohol reaches 65%, stands, centrifuging and taking supernatant, the supernatant recovery Ethanol produces decoction;
(3)Spray drying, obtains finished product.
CN201710365797.9A 2017-05-23 2017-05-23 A kind of Radix Isatidis Optimized Extraction Process Pending CN107349247A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109010407A (en) * 2018-09-11 2018-12-18 华润三九(雅安)药业有限公司 A kind of Radix Isatidis syrup and preparation method thereof

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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Application publication date: 20171117