CN108299461B - A kind of qinghaosu extracting method - Google Patents
A kind of qinghaosu extracting method Download PDFInfo
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- CN108299461B CN108299461B CN201810232533.0A CN201810232533A CN108299461B CN 108299461 B CN108299461 B CN 108299461B CN 201810232533 A CN201810232533 A CN 201810232533A CN 108299461 B CN108299461 B CN 108299461B
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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 34
- 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 28
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000000605 extraction Methods 0.000 claims abstract description 24
- 239000000463 material Substances 0.000 claims abstract description 24
- 239000012452 mother liquor Substances 0.000 claims abstract description 21
- 235000001405 Artemisia annua Nutrition 0.000 claims abstract description 20
- 240000000011 Artemisia annua Species 0.000 claims abstract description 20
- 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
- 239000000284 extract Substances 0.000 claims abstract description 14
- 108010059892 Cellulase Proteins 0.000 claims abstract description 12
- 239000001569 carbon dioxide Substances 0.000 claims abstract description 12
- 229940106157 cellulase Drugs 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
- 229920001661 Chitosan Polymers 0.000 claims abstract description 10
- 239000008367 deionised water Substances 0.000 claims abstract description 8
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 8
- 239000003480 eluent Substances 0.000 claims abstract description 6
- 238000003825 pressing Methods 0.000 claims abstract description 6
- 238000000194 supercritical-fluid extraction Methods 0.000 claims abstract description 5
- 239000007788 liquid Substances 0.000 claims abstract description 4
- 239000000203 mixture Substances 0.000 claims abstract description 4
- 238000012545 processing Methods 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 15
- 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
- 230000007071 enzymatic hydrolysis Effects 0.000 claims description 8
- 238000006047 enzymatic hydrolysis reaction Methods 0.000 claims description 8
- 239000013049 sediment Substances 0.000 claims description 7
- 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
- 108090000790 Enzymes Proteins 0.000 claims description 4
- 102000004190 Enzymes Human genes 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
- 229940088598 enzyme Drugs 0.000 claims description 4
- 238000000227 grinding Methods 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
- 230000000694 effects Effects 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 238000011068 loading method Methods 0.000 claims description 2
- 240000006891 Artemisia vulgaris Species 0.000 claims 1
- 241000723353 Chrysanthemum Species 0.000 claims 1
- 235000007516 Chrysanthemum Nutrition 0.000 claims 1
- 239000003292 glue Substances 0.000 claims 1
- 238000011084 recovery Methods 0.000 abstract description 5
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 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
- 238000005070 sampling Methods 0.000 description 4
- 238000003786 synthesis reaction Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 235000016127 added sugars Nutrition 0.000 description 2
- 239000003430 antimalarial agent Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000004140 cleaning 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
- 239000000706 filtrate Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000007654 immersion Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229930014626 natural product Natural products 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 238000001953 recrystallisation Methods 0.000 description 2
- 230000001360 synchronised effect Effects 0.000 description 2
- 244000248349 Citrus limon Species 0.000 description 1
- 235000005979 Citrus limon Nutrition 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
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000004615 ingredient 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The present invention relates to a kind of qinghaosu extracting methods of environment-friendly high-efficiency, comprising the following steps: (1) mixes the artemisia annua of crushing with cellulase, deionized water, impregnated and digested；(2) ethyl alcohol is added into the material handled by step (1) as extractant, material is placed in colloid mill；(3) mixture obtained after step (2) processing is subjected to filters pressing；(4) ethyl alcohol is added into step (3) filter cake obtained and as entrainer and carries out carbon dioxide supercritical extraction；(5) mother liquid obtained Ι in step (3) is mixed with gained extract in step (4), obtains mother liquor II, chitosan, concentration is added；(6) extract after concentration in step (5) is dissolved with ethyl alcohol, elutes, eluent is concentrated and is crystallized, qinghaosu crude product is obtained；(7) qinghaosu crude product ethyl alcohol is dissolved and is recrystallized.This method has the characteristics that environmental protection, recovery rate are high, product purity is high, extraction efficiency is fast, strong operability.
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
Refer to a kind of qinghaosu extracting method of environment-friendly high-efficiency.
Background technique
Qinghaosu is the higher effective medicinal components of added value, and structure is as shown in Figure 1, have the medicines such as anti-malarial, antitumor
Reason effect, 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.,
The qinghaosu preparation method that qinghaosu is a kind of high-efficient simple is wherein extracted 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 many and diverse, solvent loss is high, dissolvent residual is more in product, can not achieve green clean manufacturing.
Summary of the invention
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 high environmental protection, recovery rate, product purity height, the fast, strong operability of extraction efficiency etc.
Feature.
Extraction technology for artemisia annua element of the invention the following steps are included:
(1) artemisia annua of crushing is mixed with cellulase, deionized water, is warming up to 30~40 DEG C, carry out immersion and enzyme
Solution；
(2) ethyl alcohol is added into the material handled by step (1) as extractant, material is placed in colloid mill, is adjusted
The medium in colloid mill collet is saved, so that 30~40 DEG C of temperature is kept when colloid mill is in grinding material, by colloid barreling
The fineness of the material of mill is between 2~10 μm；
(3) mixture obtained after step (2) processing is subjected to filters pressing, obtains mother liquor Ι and filter cake；
(4) ethyl alcohol is added into step (3) filter cake obtained and as entrainer and carries out carbon dioxide supercritical extraction,
Obtain extract；
(5) mother liquid obtained Ι in step (3) is mixed with gained extract in step (4), obtains mother liquor II, it is poly- that shell is added
Sugar filters out sediment after stirring and standing, concentration；
(6) extract after concentration in step (5) is dissolved with ethyl alcohol, is eluted by chromatographic column, eluent is dense
It contracts crystallization, obtains qinghaosu crude product；
(7) the qinghaosu crude product ethyl alcohol is dissolved and is recrystallized, obtain the qinghaosu finished product.
Preferably, the enzyme activity range of the cellulase in the step (1) is ten thousand u/ml(g of CMC130)~1,500,000 u/
Ml(g), deionized water and the ratio of artemisia annua are 15.0L/kg~24.0L/kg, and the concentration of the cellulase in water is
0.2g/L~0.5g/L, impregnates and the time of enzymatic hydrolysis is 2~4h.
Preferably, added with lemon when the artemisia annua crushed in the step (1) mixes with cellulase, deionized water
One of acid, ascorbic acid or malic acid or a variety of, one of described citric acid, ascorbic acid or malic acid or a variety of
Concentration in water is 0.025g/L~0.05g/L.
Preferably, the quality of the artemisia annua of the ethyl alcohol and the crushing in the step (1) that are added in the step (2)
Than being provided with temperature sensor in the loading hopper of the colloid mill for 0.8:1~1:1, the temperature detected according to temperature sensor
Degree, control system control the cold and hot medium in collet.
Preferably, in the step (4) carbon dioxide supercritical extraction condition are as follows: 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 are 3.1~4.0h.
Preferably, the chitosan being added in the step (5), makes its concentration be reached for 0.015g/ml, respectively stirring and
Stand 0.5~1h.
Preferably, the concentration of ethyl alcohol used in the method is 90%~99%.
Compared with prior art, the beneficial effect of qinghaosu extracting method of the present invention is:
(1) plant cell structures can tentatively be destroyed by being pre-processed using biologic enzymolysis method to artemisia annua, significantly be increased
Add the dissolution rate of effective component qinghaosu.
(2) material after enzymatic hydrolysis 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 effective component；Meanwhile colloid mill collet
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, carries out qinghaosu 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 of the invention is used, qinghaosu crude product is chromatographed by column, after recrystallization, obtains purification qinghaosu, purity
98.0% or more, yield is greater than 85.0%.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of qinghaosu.
Fig. 2 is the process flow diagram of the qinghaosu extracting method of environment-friendly high-efficiency of the invention.
Specific embodiment
It is further to carry out combined with specific embodiments below in order to more clearly describe technology contents of the invention
Description.
The present invention provides the new process that one kind can extract qinghaosu from artemisia annua, which has environmental protection, extracts
The features such as rate is high, product purity is high, extraction efficiency is fast, strong operability.
The method of offer of the invention the following steps are included:
(1) artemisia annua of crushing is mixed with cellulase, deionized water, is warming up to 30~40 DEG C, carry out immersion and enzyme
Solution；
(2) ethyl alcohol is added into the material handled by step (1) as extractant, material is placed in colloid mill, is adjusted
The medium in colloid mill collet is saved, so that 30~40 DEG C of temperature is kept when colloid mill is in grinding material, by colloid barreling
The fineness of the material of mill is between 2~10 μm；
(3) mixture obtained after step (2) processing is subjected to filters pressing, obtains mother liquor Ι and filter cake；
(4) ethyl alcohol is added into step (3) filter cake obtained and as entrainer and carries out carbon dioxide supercritical extraction,
Obtain extract；
(5) mother liquid obtained Ι in step (3) is mixed with gained extract in step (4), obtains mother liquor II, it is poly- that shell is added
Sugar filters out sediment after stirring and standing, concentration；
(6) extract after concentration in step (5) is dissolved with ethyl alcohol, is eluted by chromatographic column, eluent is dense
It contracts crystallization, obtains qinghaosu crude product；
(7) the qinghaosu crude product ethyl alcohol is dissolved and is recrystallized, obtain the qinghaosu finished product.
Embodiment 1:
The artemisia annua dry product 100kg for taking crushing, is uniformly mixed with 1500L water, and 300g cellulase is added under stirring condition
With 37.5g citric acid, it is warming up to 35 DEG C after mixing, carries out enzymatic hydrolysis 3h.100kg ethyl alcohol is added simultaneously into the material after enzymatic hydrolysis
It is uniformly mixed, mixed material is put into colloid mill and is crushed, and it is 35 that colloid mill collet, which is passed through warm water and maintains temperature in colloid mill,
℃.By the filters pressing while hot of levigate material, mother liquor Ι and filter cake are obtained, mother liquor Ι sampling carries out high performance liquid chromatography (HPLC) test,
Measure artemislnin content.By the supercritical extracting equipment of filter cake investment 50L, pipeline is connected, opens general supply and each instrument electricity
Source, later on apparatus control system, setting extracting pressure be 20.0MPa, extraction temperature 332.0K, CO2Flow is
After 3.0kg/min, system pressure and system temperature reach setting value, start entrainer feed pump, entrainer selects ethyl alcohol, filter cake
Volume ratio with ethyl alcohol entrainer is 25:1, starts timing, cycling extraction 3.5h.Extraction terminates, and closes refrigerator, pump and various
Heat cycles switch, turns off total power switch.Extraction cylinder in pressure be put into subsequent separator, after pressure balance, from point
From taking out extract in kettle and being mixed to get mother liquor II with mother liquor Ι, sampling carries out HPLC test from mother liquor II.
Chitosan is added into mother liquor II, the additional amount of chitosan is that 1.5g chitosan, stirring is added in every 100ml mother liquor 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, and concentration produces
Object mixes after being dissolved with ethyl alcohol with cleaning solution, is eluted by chromatographic column, and eluent is concentrated and is 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 blueness punt-pole obtained by drying 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 cellulase is added under stirring condition
With 75g citric acid, it is warming up to 40 DEG C after mixing, carries out enzymatic hydrolysis 4h.80kg ethyl alcohol is added into the material after enzymatic hydrolysis and mixes
Close uniformly, mixed material is put into colloid mill and is crushed, colloid mill collet be passed through warm water and maintain in colloid mill temperature be 30~
40℃.By the filters pressing while hot of levigate material, mother liquor Ι and filter cake are obtained, mother liquor Ι sampling carries out high performance liquid chromatography (HPLC) and surveys
Examination measures artemislnin content.By the supercritical extracting equipment of filter cake investment 50L, pipeline is connected, opens general supply and each instrument
Power supply, later on apparatus control system, setting extracting pressure be 21.1MPa, extraction temperature 335.4K, CO2Flow is
After 3.2kg/min, system pressure and system temperature reach setting value, start entrainer feed pump, filter cake and ethyl alcohol entrainer
Volume ratio is 30:1, starts timing, cycling extraction 3.8h.Extraction terminates, and closes refrigerator, pump and various heat cycles switch,
Turn off total power switch.Pressure in extraction cylinder is put into subsequent separator, and after pressure balance, extraction is taken out from separating still
Object is simultaneously mixed to get mother liquor II with mother liquor Ι, and sampling carries out HPLC test from mother liquor II.
Chitosan is added into mother liquor II, the additional amount of chitosan is that 1.5g chitosan, stirring is added in every 100ml mother liquor 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, and concentration produces
Object mixes after being dissolved with ethyl alcohol with cleaning solution, is eluted by chromatographic column, and eluent is concentrated and is 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 blueness punt-pole obtained by drying 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 beneficial effect of qinghaosu extracting method of the present invention is:
(1) plant cell structures can tentatively be destroyed by being pre-processed using biologic enzymolysis method to artemisia annua, significantly be increased
Add the dissolution rate of effective component qinghaosu.
(2) material after enzymatic hydrolysis 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 effective component；Meanwhile colloid mill collet
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, carries out qinghaosu 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 of the invention is used, qinghaosu crude product is chromatographed by column, after recrystallization, obtains purification qinghaosu, purity
98.0% or more, yield is greater 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, which is characterized in that the method the following steps are included:
(1) artemisia annua of crushing is mixed with cellulase, deionized water, is warming up to 30~40 DEG C, impregnated and digested；
(2) ethyl alcohol is added into the material handled by step (1) as extractant, material is placed in colloid mill, glue is adjusted
Body grinds the medium in collet, so that 30~40 DEG C of temperature is kept when grinding material in colloid mill, by colloid mill grinding
The fineness of material is between 2~10 μm；
(3) mixture obtained after step (2) processing is subjected to filters pressing, obtains mother liquor Ι and filter cake；
(4) ethyl alcohol is added into step (3) filter cake obtained and as entrainer and carries out carbon dioxide supercritical extraction, obtain
Extract；
(5) mother liquid obtained Ι in step (3) is mixed with gained extract in step (4), obtains mother liquor II, chitosan is added, stirs
After mixing and standing, sediment is filtered out, is concentrated；
(6) extract after concentration in step (5) 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 is recrystallized, obtain the qinghaosu finished product.
2. qinghaosu extracting method according to claim 1, which is characterized in that the cellulase in the step (1)
Enzyme activity range be 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, the concentration of the cellulase in water are 0.2g/L~0.5g/L, impregnate and the time of enzymatic hydrolysis is 2~4h.
3. qinghaosu extracting method according to claim 1, which is characterized in that the chrysanthemum crushed in the step (1)
One of citric acid, ascorbic acid or malic acid or a variety of are added with when wormwood artemisia mixes with cellulase, deionized water, it is described
One of citric acid, ascorbic acid or malic acid or a variety of concentration in water are 0.025g/L~0.05g/L.
4. qinghaosu extracting method according to claim 1, which is characterized in that the ethyl alcohol added in the step (2)
Mass ratio with the artemisia annua of the crushing in the step (1) is 0.8:1~1:1, is set in the loading hopper of the colloid mill
It is equipped with temperature sensor, according to the temperature that temperature sensor detects, control system controls the cold and hot medium in collet.
5. qinghaosu extracting method according to claim 1, which is characterized in that carbon dioxide is super in the step (4)
The condition of critical extraction are as follows: 332~335.4K of temperature, 19.8~21.1MPa of pressure, the flow of carbon dioxide is 2.8~
The volume ratio of 3.2kg/min, filter cake and ethyl alcohol entrainer is 15~35:1, and extraction time is 3.1~4.0h.
6. qinghaosu extracting method according to claim 1, which is characterized in that chitosan is added in the step (5),
So that its concentration is reached for 0.015g/ml, stirs and stand 0.5~1h respectively.
7. qinghaosu extracting method according to claim 1, which is characterized in that ethyl alcohol used in the method it is dense
Degree is 90%~99%.
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| 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 |
| CN110681182B (en) * | 2019-10-14 | 2020-11-20 | 中国科学院过程工程研究所 | Method for enhancing purification and separation of artemisinin by chitosan functional membrane |
Citations (6)
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| 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 |
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