CN108299461A - A kind of qinghaosu extracting method of environment-friendly high-efficiency - Google Patents
A kind of qinghaosu extracting method of environment-friendly high-efficiency Download PDFInfo
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- CN108299461A CN108299461A CN201810232533.0A CN201810232533A CN108299461A CN 108299461 A CN108299461 A CN 108299461A CN 201810232533 A CN201810232533 A CN 201810232533A CN 108299461 A CN108299461 A CN 108299461A
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- qinghaosu
- ethyl alcohol
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- 229930101531 artemisinin Natural products 0.000 title claims abstract description 52
- BLUAFEHZUWYNDE-NNWCWBAJSA-N artemisinin Chemical compound C([C@](OO1)(C)O2)C[C@H]3[C@H](C)CC[C@@H]4[C@@]31[C@@H]2OC(=O)[C@@H]4C BLUAFEHZUWYNDE-NNWCWBAJSA-N 0.000 title claims abstract description 52
- 229930183339 qinghaosu Natural products 0.000 title claims abstract description 52
- 238000000034 method Methods 0.000 title claims abstract description 33
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 66
- 235000019441 ethanol Nutrition 0.000 claims abstract description 33
- 239000000084 colloidal system Substances 0.000 claims abstract description 26
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000000463 material Substances 0.000 claims abstract description 24
- 238000000605 extraction Methods 0.000 claims abstract description 23
- 235000001405 Artemisia annua Nutrition 0.000 claims abstract description 21
- 240000000011 Artemisia annua Species 0.000 claims abstract description 21
- 239000012452 mother liquor Substances 0.000 claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000012065 filter cake Substances 0.000 claims abstract description 15
- 229910002092 carbon dioxide Inorganic materials 0.000 claims abstract description 14
- 229920001661 Chitosan Polymers 0.000 claims abstract description 12
- 239000001569 carbon dioxide Substances 0.000 claims abstract description 12
- 239000012043 crude product Substances 0.000 claims abstract description 12
- 239000000047 product Substances 0.000 claims abstract description 11
- 108010059892 Cellulase Proteins 0.000 claims abstract description 10
- 238000002156 mixing Methods 0.000 claims abstract description 9
- 229940106157 cellulase Drugs 0.000 claims abstract description 8
- 239000008367 deionised water Substances 0.000 claims abstract description 8
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 8
- 238000012545 processing Methods 0.000 claims abstract description 8
- 239000003480 eluent Substances 0.000 claims abstract description 6
- 238000001914 filtration Methods 0.000 claims abstract description 6
- 238000000194 supercritical-fluid extraction Methods 0.000 claims abstract description 6
- 239000007788 liquid Substances 0.000 claims abstract description 4
- 239000000203 mixture Substances 0.000 claims abstract description 4
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 13
- 238000003756 stirring Methods 0.000 claims description 9
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 8
- 239000013049 sediment Substances 0.000 claims description 7
- 238000000227 grinding Methods 0.000 claims description 6
- 235000015165 citric acid Nutrition 0.000 claims description 5
- 238000010792 warming Methods 0.000 claims description 5
- BJEPYKJPYRNKOW-REOHCLBHSA-N (S)-malic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O BJEPYKJPYRNKOW-REOHCLBHSA-N 0.000 claims description 4
- BJEPYKJPYRNKOW-UHFFFAOYSA-N alpha-hydroxysuccinic acid Natural products OC(=O)C(O)CC(O)=O BJEPYKJPYRNKOW-UHFFFAOYSA-N 0.000 claims description 4
- 239000011668 ascorbic acid Substances 0.000 claims description 4
- 235000010323 ascorbic acid Nutrition 0.000 claims description 4
- 229960005070 ascorbic acid Drugs 0.000 claims description 4
- 230000000694 effects Effects 0.000 claims description 4
- 239000001630 malic acid Substances 0.000 claims description 4
- 235000011090 malic acid Nutrition 0.000 claims description 4
- 238000002425 crystallisation Methods 0.000 claims description 3
- 230000008025 crystallization Effects 0.000 claims description 3
- 239000003292 glue Substances 0.000 claims description 3
- 238000011068 loading method Methods 0.000 claims description 2
- 238000011084 recovery Methods 0.000 abstract description 5
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 238000010828 elution Methods 0.000 abstract 1
- 241000196324 Embryophyta Species 0.000 description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- 238000004128 high performance liquid chromatography Methods 0.000 description 6
- 238000004090 dissolution Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000005070 sampling Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 239000004615 ingredient Substances 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- 108010084185 Cellulases Proteins 0.000 description 2
- 102000005575 Cellulases Human genes 0.000 description 2
- 239000004480 active ingredient Substances 0.000 description 2
- 239000003430 antimalarial agent Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 238000004440 column chromatography Methods 0.000 description 2
- 230000001351 cycling effect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000706 filtrate Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 229930014626 natural product Natural products 0.000 description 2
- 238000001953 recrystallisation Methods 0.000 description 2
- 230000001360 synchronised effect Effects 0.000 description 2
- 235000005979 Citrus limon Nutrition 0.000 description 1
- 244000131522 Citrus pyriformis Species 0.000 description 1
- 238000000944 Soxhlet extraction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000000078 anti-malarial effect Effects 0.000 description 1
- 230000000259 anti-tumor effect Effects 0.000 description 1
- 229960004191 artemisinin Drugs 0.000 description 1
- 238000009395 breeding Methods 0.000 description 1
- 230000001488 breeding effect Effects 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000000874 microwave-assisted extraction Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001256 steam distillation Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D493/00—Heterocyclic compounds containing oxygen atoms as the only ring hetero atoms in the condensed system
- C07D493/12—Heterocyclic compounds containing oxygen atoms as the only ring hetero atoms in the condensed system in which the condensed system contains three hetero rings
- C07D493/20—Spiro-condensed systems
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D493/00—Heterocyclic compounds containing oxygen atoms as the only ring hetero atoms in the condensed system
- C07D493/12—Heterocyclic compounds containing oxygen atoms as the only ring hetero atoms in the condensed system in which the condensed system contains three hetero rings
- C07D493/18—Bridged systems
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
Abstract
The present invention relates to a kind of qinghaosu extracting methods of environment-friendly high-efficiency, include the following steps：（1）The artemisia annua of crushing is mixed with cellulase, deionized water, is impregnated and is digested；（2）To by step（1）Ethyl alcohol is added in the material of processing as extractant, material is placed in colloid mill；（3）By step（2）The mixture obtained after processing carries out press filtration；（4）To step（3）Ethyl alcohol is added in the filter cake obtained and as entrainer and carries out carbon dioxide supercritical extraction；（5）By step（3）In mother liquid obtained Ι and step（4）Middle gained extract mixing, obtains mother liquor II, and chitosan, concentration is added；（6）By step（5）Extract after middle concentration is dissolved with ethyl alcohol, and eluent is concentrated and crystallized, obtains qinghaosu crude product by elution；（7）Qinghaosu crude product ethyl alcohol is dissolved and recrystallized.This method has the characteristics that environmental protection, recovery rate are high, product purity is high, extraction efficiency is fast, operability is strong.
Description
Technical field
The present invention relates to the extraction of effective ingredients in plant and its purifying process technical field more particularly to qinghaosus, specifically
It refer to a kind of qinghaosu extracting method of environment-friendly high-efficiency.
Background technology
Qinghaosu is the higher effective medicinal components of added value, and structure is as shown in Figure 1, with the medicines such as anti-malarial, antitumor
Reason acts on, and is the new antimalarial agent that China uniquely obtains international recognition.In recent years, the research of qinghaosu is in widespread attention, though
Qinghaosu can be so obtained by chemical synthesis, but since it there are multiple asymmetric carbon atoms, synthesis step is complex, unfavorable
In industrialized production, therefore medicinal artemisinin is mainly to extract to obtain from artemisia annua at present.
The acquisition methods of green high element mainly have biosynthesis, chemical synthesis, Plant Tissue Breeding and natural product extraction etc.,
It is a kind of qinghaosu preparation method of high-efficient simple that qinghaosu is extracted wherein from natural products, that is, artemisia annua, and China possesses
Apparent resources advantage.It is mainly traditional extraction side based on extracting principle from the method for extracting green high element in artemisia annua
Method mainly has soxhlet extraction, microwave―assisted extraction, refluxing extraction, extraction by steam distillation etc..And these techniques exist
The problems such as recovery rate is not high, step is complicated, solvent loss is high, dissolvent residual is more in product, can not achieve green clean manufacturing.
Invention content
The purpose of the present invention is overcoming traditional extraction technology for artemisia annua element, providing one kind can be from artemisia annua
The new process of qinghaosu is extracted, which has environmental protection, recovery rate are high, product purity is high, extraction efficiency is fast, operability is strong etc.
Feature.
The extraction technology for artemisia annua element of the present invention includes the following steps：
（1）The artemisia annua of crushing is mixed with cellulase, deionized water, 30~40 DEG C is warming up to, is impregnated and digested；
（2）To by step（1）Ethyl alcohol is added in the material of processing as extractant, material is placed in colloid mill, glue is adjusted
Body grinds the medium in chuck so that the temperature that 30~40 DEG C are kept when colloid mill is in grinding material, by colloid mill grinding
The fineness of material is between 2~10 μm；
（3）By step（2）The mixture obtained after processing carries out press filtration, obtains mother liquor Ι and filter cake；
（4）To step（3）Ethyl alcohol is added in the filter cake obtained and as entrainer and carries out carbon dioxide supercritical extraction, obtains
Extract；
（5）By step（3）In mother liquid obtained Ι and step（4）Middle gained extract mixing, obtains mother liquor II, chitosan is added, stirs
After mixing and standing, sediment is filtered out, is concentrated；
（6）By step（5）Extract after middle concentration is dissolved with ethyl alcohol, is eluted by chromatographic column, simultaneously by eluent concentration
Crystallization, obtains qinghaosu crude product；
（7）The qinghaosu crude product ethyl alcohol is dissolved and recrystallized, the qinghaosu finished product is obtained.
Preferably, the step（1）In cellulase enzyme activity ranging from ten thousand u/ml of CMC130（g）~150 ten thousand u/
ml（g）, the ratio of deionized water and artemisia annua is 15.0L/kg~24.0L/kg, the cellulase in water a concentration of
0.2g/L~0.5g/L, impregnates and the time of enzymolysis is 2~4h.
Preferably, the step（1）Lemon is added with when the artemisia annua of middle crushing mixes with cellulase, deionized water
It is one or more in acid, ascorbic acid or malic acid, it is one or more in the citric acid, ascorbic acid or malic acid
A concentration of 0.025g/L~0.05g/L in water.
Preferably, the step（2）The ethyl alcohol of middle addition and the step（1）In crushing artemisia annua quality
Than being 0.8:1~1:1, temperature sensor is provided in the loading hopper of the colloid mill, the temperature detected according to temperature sensor
Degree, control system control the cold and hot medium in chuck.
Preferably, the step（4）The condition of middle carbon dioxide supercritical extraction is：332~335.4K of temperature, pressure
19.8~21.1MPa, the flow of carbon dioxide are 2.8~3.2kg/min, the volume ratio of filter cake and ethyl alcohol entrainer is 15~
35：1, extraction time is 3.1~4.0h.
Preferably, the step（5）The chitosan of middle addition makes its concentration be reached for 0.015g/ml, respectively stirring and
Stand 0.5~1h.
Preferably, a concentration of the 90%~99% of the ethyl alcohol used in the method.
Compared with prior art, the advantageous effect of qinghaosu extracting method of the present invention is：
（1）Plant cell structures can tentatively be destroyed by being pre-processed to artemisia annua using biologic enzymolysis method, increased considerably
Imitate the dissolution rate of ingredient qinghaosu.
（2）The material after enzymolysis is crushed using colloid mill, the high shear forces that colloid mill has can be by material
2~10 μm are crushed to, plant cell structures can be further destroyed, increases the dissolution rate of active ingredient；Meanwhile colloid mill chuck
Medium can effectively control temperature in colloid mill, can will crush progress synchronous with extraction, significantly simplification of flowsheet,
Reduce equipment cost.
（3）Reextraction is carried out using supercritical carbon dioxide, selects ethyl alcohol for entrainer, qinghaosu is carried out with this method
Extracting operation, the recovery rate of qinghaosu is to use pure carbon dioxide for 2.0 times or more of extractant.
（4）Technique using the present invention, qinghaosu crude product obtain refined qinghaosu, purity after column chromatography, recrystallization
98.0% or more, yield is more than 85.0%.
Description of the drawings
Fig. 1 is the structural schematic diagram of qinghaosu.
Fig. 2 is the process flow diagram of the qinghaosu extracting method of the environment-friendly high-efficiency of the present invention.
Specific implementation mode
In order to more clearly describe the technology contents of the present invention, carried out with reference to specific embodiment further
Description.
The present invention provides a kind of new process that can extract qinghaosu from artemisia annua, which has environmental protection, extraction
The features such as rate is high, product purity is high, extraction efficiency is fast, operability is strong.
The method of the offer of the present invention includes the following steps：
（1）The artemisia annua of crushing is mixed with cellulase, deionized water, 30~40 DEG C is warming up to, is impregnated and digested；
（2）To by step（1）Ethyl alcohol is added in the material of processing as extractant, material is placed in colloid mill, glue is adjusted
Body grinds the medium in chuck so that the temperature that 30~40 DEG C are kept when colloid mill is in grinding material, by colloid mill grinding
The fineness of material is between 2~10 μm；
（3）By step（2）The mixture obtained after processing carries out press filtration, obtains mother liquor Ι and filter cake；
（4）To step（3）Ethyl alcohol is added in the filter cake obtained and as entrainer and carries out carbon dioxide supercritical extraction, obtains
Extract；
（5）By step（3）In mother liquid obtained Ι and step（4）Middle gained extract mixing, obtains mother liquor II, chitosan is added, stirs
After mixing and standing, sediment is filtered out, is concentrated；
（6）By step（5）Extract after middle concentration is dissolved with ethyl alcohol, is eluted by chromatographic column, simultaneously by eluent concentration
Crystallization, obtains qinghaosu crude product；
（7）The qinghaosu crude product ethyl alcohol is dissolved and recrystallized, the qinghaosu finished product is obtained.
Embodiment 1：
The artemisia annua dry product 100kg for taking crushing, is uniformly mixed with 1500L water, under stirring condition be added 300g cellulases and
37.5g citric acids are warming up to 35 DEG C after mixing, carry out enzymolysis 3h.100kg ethyl alcohol is added into the material after enzymolysis and mixes
It closes uniformly, mixed material is put into colloid mill and crushes, and it is 35 DEG C that colloid mill chuck, which is passed through warm water and maintains temperature in colloid mill,.
By the press filtration while hot of levigate material, mother liquor Ι and filter cake are obtained, mother liquor Ι samplings carry out high performance liquid chromatography（HPLC）Test measures
Artemislnin content.The supercritical extracting equipment that filter cake is put into 50L connects pipeline, opens general supply and each instrument power source, with
Opening device control system afterwards, setting extracting pressure be 20.0MPa, extraction temperature 332.0K, CO2Flow is 3.0kg/min,
After system pressure and system temperature reach setting value, start entrainer feed pump, entrainer selects ethyl alcohol, filter cake to be carried secretly with ethyl alcohol
The volume ratio of agent is 25:1, start timing, cycling extraction 3.5h.Extraction terminates, and closes refrigerator, pump and various heat cycles and opens
It closes, turns off total power switch.Pressure in extraction cylinder is put into subsequent separator, after pressure balance, is taken out from separating still
Extract is simultaneously mixed to get mother liquor II with mother liquor Ι, the sampling progress HPLC tests from mother liquor II.
Chitosan is added into mother liquor II, the addition of chitosan is that 1.5g chitosans, stirring are added per 100ml mother liquors II
And after standing, sediment is filtered out, sediment is washed 3 times with hot methanol, and filtrate carries out heating and is concentrated into closely dry state, concentration production
Object mixes after being dissolved with ethyl alcohol with cleaning solution, is eluted by chromatographic column, and eluent is concentrated and crystallized, it is thick to obtain qinghaosu
Product.Qinghaosu crude product ethyl alcohol is dissolved and is recrystallized, and recrystallizer sets in constant temperature oven the drying blueness punt-pole at 60~70 DEG C
Element.The purity of sterling is tested by HPLC, and qinghaosu weighs and carries out mass balance calculated yield.
1 embodiment of table, 1 qinghaosu purity and yield
。
Embodiment 2：
The artemisia annua dry product 100kg for taking crushing, is uniformly mixed with 1500L water, and 750g cellulases and 75g are added under stirring condition
Citric acid is warming up to 40 DEG C after mixing, carries out enzymolysis 4h.80kg ethyl alcohol is added into the material after enzymolysis and mixes equal
Even, mixed material is put into colloid mill and crushes, and it is 30~40 DEG C that colloid mill chuck, which is passed through warm water and maintains temperature in colloid mill,.
By the press filtration while hot of levigate material, mother liquor Ι and filter cake are obtained, mother liquor Ι samplings carry out high performance liquid chromatography（HPLC）Test measures
Artemislnin content.The supercritical extracting equipment that filter cake is put into 50L connects pipeline, opens general supply and each instrument power source, with
Opening device control system afterwards, setting extracting pressure be 21.1MPa, extraction temperature 335.4K, CO2Flow is 3.2kg/min,
After system pressure and system temperature reach setting value, start entrainer feed pump, the volume ratio of filter cake and ethyl alcohol entrainer is 30:
1, start timing, cycling extraction 3.8h.Extraction terminates, and closes refrigerator, pump and various heat cycles switch, turns off general supply
Switch.Extraction cylinder in pressure be put into subsequent separator, after pressure balance, from separating still take out extract and with mother liquor Ι
It is mixed to get mother liquor II, the sampling progress HPLC tests from mother liquor II.
Chitosan is added into mother liquor II, the addition of chitosan is that 1.5g chitosans, stirring are added per 100ml mother liquors II
And after standing, sediment is filtered out, sediment is washed 3 times with hot methanol, and filtrate carries out heating and is concentrated into closely dry state, concentration production
Object mixes after being dissolved with ethyl alcohol with cleaning solution, is eluted by chromatographic column, and eluent is concentrated and crystallized, it is thick to obtain qinghaosu
Product.Qinghaosu crude product ethyl alcohol is dissolved and is recrystallized, and recrystallizer sets in constant temperature oven the drying blueness punt-pole at 60~70 DEG C
Element.The purity of sterling is tested by HPLC, and qinghaosu weighs and carries out mass balance calculated yield.
2 embodiment of table, 2 qinghaosu purity and yield
。
Compared with prior art, the advantageous effect of qinghaosu extracting method of the present invention is：
（1）Plant cell structures can tentatively be destroyed by being pre-processed to artemisia annua using biologic enzymolysis method, increased considerably
Imitate the dissolution rate of ingredient qinghaosu.
（2）The material after enzymolysis is crushed using colloid mill, the high shear forces that colloid mill has can be by material
2~10 μm are crushed to, plant cell structures can be further destroyed, increases the dissolution rate of active ingredient；Meanwhile colloid mill chuck
Medium can effectively control temperature in colloid mill, can will crush progress synchronous with extraction, significantly simplification of flowsheet,
Reduce equipment cost.
（3）Reextraction is carried out using supercritical carbon dioxide, selects ethyl alcohol for entrainer, qinghaosu is carried out with this method
Extracting operation, the recovery rate of qinghaosu is to use pure carbon dioxide for 2.0 times or more of extractant.
（4）Technique using the present invention, qinghaosu crude product obtain refined qinghaosu, purity after column chromatography, recrystallization
98.0% or more, yield is more than 85.0%.
In this description, the present invention is described with reference to its specific embodiment.But it is clear that can still make
Various modifications and alterations are without departing from the spirit and scope of the invention.Therefore, the description and the appended drawings should be considered as illustrative
And not restrictive.
Claims (7)
1. a kind of qinghaosu extracting method of environment-friendly high-efficiency, which is characterized in that the method includes the following steps：
（1）The artemisia annua of crushing is mixed with cellulase, deionized water, 30~40 DEG C is warming up to, is impregnated and digested；
（2）To by step（1）Ethyl alcohol is added in the material of processing as extractant, material is placed in colloid mill, glue is adjusted
Body grinds the medium in chuck so that the temperature for keeping 30~40 DEG C when grinding material in colloid mill, by colloid mill grinding
The fineness of material is between 2~10 μm；
（3）By step（2）The mixture obtained after processing carries out press filtration, obtains mother liquor Ι and filter cake；
（4）To step（3）Ethyl alcohol is added in the filter cake obtained and as entrainer and carries out carbon dioxide supercritical extraction, obtains
Extract；
（5）By step（3）In mother liquid obtained Ι and step（4）Middle gained extract mixing, obtains mother liquor II, chitosan is added, stirs
After mixing and standing, sediment is filtered out, is concentrated；
（6）By step（5）Extract after middle concentration is dissolved with ethyl alcohol, is eluted by chromatographic column, simultaneously by eluent concentration
Crystallization, obtains qinghaosu crude product；
（7）The qinghaosu crude product ethyl alcohol is dissolved and recrystallized, the qinghaosu finished product is obtained.
2. the qinghaosu extracting method of environment-friendly high-efficiency according to claim 1, which is characterized in that the step（1）In
Cellulase enzyme activity ranging from CMC 1,300,000 u/g~1,500,000 u/g, the ratio of deionized water and artemisia annua is 15.0L/kg
~24.0L/kg, a concentration of 0.2g/L~0.5g/L of the cellulase in water, impregnate and enzymolysis time be 2~
4h。
3. the qinghaosu extracting method of environment-friendly high-efficiency according to claim 1, which is characterized in that the step（1）In
When the artemisia annua of crushing mixes with cellulase, deionized water added in citric acid, ascorbic acid or malic acid one kind or
It is a variety of, one or more a concentration of 0.025g/L in water in the citric acid, ascorbic acid or malic acid~
0.05g/L。
4. the qinghaosu extracting method of environment-friendly high-efficiency according to claim 1, which is characterized in that the step（2）In
The ethyl alcohol of addition and the step（1）In crushing artemisia annua mass ratio be 0.8:1~1:1, the colloid mill
Temperature sensor is provided in loading hopper, according to the temperature that temperature sensor detects, control system controls cold and hot Jie in chuck
Matter.
5. the qinghaosu extracting method of environment-friendly high-efficiency according to claim 1, which is characterized in that the step（4）In
The condition of carbon dioxide supercritical extraction is：The flow of 332~335.4K of temperature, 19.8~21.1MPa of pressure, carbon dioxide is
The volume ratio of 2.8~3.2kg/min, filter cake and ethyl alcohol entrainer is 15~35：1, extraction time is 3.1~4.0h.
6. the qinghaosu extracting method of environment-friendly high-efficiency according to claim 1, which is characterized in that the step（5）In
Chitosan is added, its concentration is made to be reached for 0.015g/ml, stirs and stand 0.5~1h respectively.
7. the qinghaosu extracting method of environment-friendly high-efficiency according to claim 1, which is characterized in that used in the method
Ethyl alcohol a concentration of 90%~99%.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110681182A (en) * | 2019-10-14 | 2020-01-14 | 中国科学院过程工程研究所 | Method for enhancing purification and separation of artemisinin by chitosan functional membrane |
| CN110698495A (en) * | 2019-09-24 | 2020-01-17 | 天马（安徽）国药科技股份有限公司 | Separation preparation method for rapidly preparing artemisinin |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103304576A (en) * | 2012-03-07 | 2013-09-18 | 中国人民解放军第三军医大学 | Method for extracting artemisinin through enzymatic hydrolysis |
| CN103467480A (en) * | 2013-10-10 | 2013-12-25 | 南京正亮医药科技有限公司 | Method for extracting artemisinin and application of artemisinin |
| CN104140433A (en) * | 2013-05-10 | 2014-11-12 | 天津瑞信医药科技有限公司 | Artemisinin preparation method |
| CN104327092A (en) * | 2014-10-13 | 2015-02-04 | 庞群 | Method for extracting artemisinin from artemisia annua L |
| CN107522708A (en) * | 2017-06-30 | 2017-12-29 | 禹州市天源生物科技有限公司 | A kind of production technology of enzymatic isolation method extraction qinghaosu |
| CN107522713A (en) * | 2017-06-30 | 2017-12-29 | 禹州市天源生物科技有限公司 | A kind of preparation method of high-purity extraction qinghaosu |
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Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103304576A (en) * | 2012-03-07 | 2013-09-18 | 中国人民解放军第三军医大学 | Method for extracting artemisinin through enzymatic hydrolysis |
| CN104140433A (en) * | 2013-05-10 | 2014-11-12 | 天津瑞信医药科技有限公司 | Artemisinin preparation method |
| CN103467480A (en) * | 2013-10-10 | 2013-12-25 | 南京正亮医药科技有限公司 | Method for extracting artemisinin and application of artemisinin |
| CN104327092A (en) * | 2014-10-13 | 2015-02-04 | 庞群 | Method for extracting artemisinin from artemisia annua L |
| CN107522708A (en) * | 2017-06-30 | 2017-12-29 | 禹州市天源生物科技有限公司 | A kind of production technology of enzymatic isolation method extraction qinghaosu |
| CN107522713A (en) * | 2017-06-30 | 2017-12-29 | 禹州市天源生物科技有限公司 | A kind of preparation method of high-purity extraction qinghaosu |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110698495A (en) * | 2019-09-24 | 2020-01-17 | 天马（安徽）国药科技股份有限公司 | Separation preparation method for rapidly preparing artemisinin |
| CN110681182A (en) * | 2019-10-14 | 2020-01-14 | 中国科学院过程工程研究所 | Method for enhancing purification and separation of artemisinin by chitosan functional membrane |
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