CN107522713A - A kind of preparation method of high-purity extraction qinghaosu - Google Patents
A kind of preparation method of high-purity extraction qinghaosu Download PDFInfo
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- CN107522713A CN107522713A CN201710520829.8A CN201710520829A CN107522713A CN 107522713 A CN107522713 A CN 107522713A CN 201710520829 A CN201710520829 A CN 201710520829A CN 107522713 A CN107522713 A CN 107522713A
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- qinghaosu
- purity
- preparation
- sweet wormwood
- normal temperature
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- 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
Abstract
The present invention relates to a kind of preparation method of high-purity extraction qinghaosu, it comprises the following steps：Step 1：Selection；Step 2：Enzymolysis；Step 3：Dry；Step 4：Produce extract solution；Step 5：Concentration；Step 6：Crude crystalline；Step 7：Purification；Step 8：It is high-purity crystallized to produce；The present invention has the advantages of technique is simple, purification rate is high, cost is low.
Description
Technical field
The invention belongs to medicinal product separation and extraction technology field, and in particular to a kind of preparation of high-purity extraction qinghaosu
Method.
Background technology
Qinghaosu is a kind of antimalarial specific drug, has especially for encephalic malaria and anti-chlorine quinoline malaria and significantly treats
Effect, have it is quick-acting and less toxic the characteristics of, artemisinine anti-schistosome, regulation or suppress body fluid immunologic function, raising lymph it is thin
Tempting prospect is also showed that in the treatment of the conversion ratio of born of the same parents, qinghaosu can be extracted from sweet wormwood and obtained, and there are a variety of extractions at present
The method of qinghaosu, but the qinghaosu recovery rate of production technology mostly is low, the qinghaosu purity produced is low, it is impossible to meet higher
Demand, qinghaosu is extracted using biological enzymolysis technology, can obtain destroying the effect of cell membrane, improve the recovery rate of qinghaosu
10%, suitable solvent extraction concentration can obtain qinghaosu crystallization, have high excellent of significant recovery rate compared to other extracting methods
Gesture, and with the advantages of technique is simple, purification rate is high, cost is low, can meet the needs of high concentration qinghaosu.
The content of the invention
The invention aims to overcome the deficiencies in the prior art, and provide that a kind of technique is simple, purification rate is high, cost
The preparation method of low high-purity extraction qinghaosu.
The object of the present invention is achieved like this：A kind of preparation method of high-purity extraction qinghaosu, it includes following step
Suddenly：
Step 1：Selection；Fresh and alive artemisia leaf is plucked, and does sterilization processing；
Step 2：Enzymolysis：In the uniformly cellulase of 0.2% -0.5% sweet wormwood weight of sprinkling and the pectase mixing of sweet wormwood blade face
Enzyme agent processed, stack in the dark and cover layer of plastic film, keeping temperature is 40 DEG C-48 DEG C, is allowed to ferment 2-3 days；
Step 3：Dry；The sweet wormwood blade after digesting that will ferment fully is dried at low temperature；
Step 4：Produce extract solution；Sweet wormwood cured leaf after drying process is inserted into reaction vessel, adds 5-8 times of green grass or young crops in a reservoir
The ethyl acetate of wormwood artemisia cured leaf quality, 1.5h-2.5h is stirred at 55 DEG C-60 DEG C, filtered, and repeatedly 2-3 times, fully
Extraction, and each secondary filtered fluid is merged to obtain extract solution；
Step 5：Concentration；Obtained extract solution in step 4 is evaporated and is concentrated into 6%-the 9% of original volume, and reclaims second
Acetoacetic ester；
Step 6：Crude crystalline；The concentrate produced in step 5 is stood under 25 DEG C -28 DEG C normal temperature, naturally cools to knot
It is brilliant；Leaching is crystallized to obtain qinghaosu crude crystalline, and 2-3 washings, natural wind are carried out to crude crystalline using ethyl acetate
It is dry, it is dried at 25 DEG C -28 DEG C under normal temperature；Collect filtrate and make lower batch of raw materials for production use；
Step 7：Purification；The high concentration ethanol of 100-120 times of quality of obtained dry crude crystalline in step 6 is dissolved,
Filtering, is concentrated into 8%-the 10% of original volume, and reclaim ethanol by filtered fluid；
Step 8：It is high-purity crystallized to produce；Concentrate in step 7 is stood under 25 DEG C -28 DEG C normal temperature, naturally cooled to
Crystallization, leaching crystallize and collect mother liquor；Crystallization is carried out 2-3 times using high concentration ethanol, natural air drying, at 25 DEG C-28 DEG C
It is dried under lower normal temperature, that is, high-purity qinghaosu is made.
Low temperature in described step 3 is 25 DEG C -30 DEG C.
The mass ratio of cellulase and pectase in described step 2 is 0.7：1—1：0.7.
High concentration ethanol concentration in described step 7 is 80% -95%.
Stirring in described step 4 uses silica gel product.
The advantageous effects of the present invention：The technological process of production of the present invention is simple, easily operation, to working condition requirement
Low, cellulase and pectase mixing enzyme preparation play and promote loose sweet wormwood leaf wall, reduction resistance to mass tranfer, effectively remove egg
The effect of the impurity such as white matter, the recovery rate for improving qinghaosu can be imitated significantly, the purity of increase extraction qinghaosu, can be met higher
The qinghaosu demand of purity.
Specific embodiment
Embodiment 1
Fresh and alive 500kg artemisia leafs are plucked, and do sterilization processing；1.5kg, cellulase and pectin are uniformly sprayed on sweet wormwood blade face
Enzyme mass ratio is 0.9：1 mixing enzyme agent, stack in the dark and cover layer of plastic film, keeping temperature is 42 DEG C, is allowed to
Fermentation 2 days；The sweet wormwood blade after digesting that will ferment fully is dried at 26 DEG C；Sweet wormwood cured leaf after drying process is inserted into reaction
Container, add 2000L ethyl acetate in a reservoir every time, 2h is stirred at 58 DEG C, filter, and be repeated 2 times, fully carry
Take, and filtered fluid will merge to obtain extract solution three times；Obtained extract solution is evaporated and is concentrated into original volume
7%, and reclaim ethyl acetate；The concentrate produced is stood under 26 DEG C of normal temperature, naturally cools to crystallization；Leaching crystallizes to obtain
Qinghaosu crude crystalline, and 3 washings are carried out to crude crystalline using ethyl acetate, natural air drying, enter at 25 DEG C under normal temperature
Row drying, is weighed as 2.55kg；Collect filtrate and make lower batch of raw materials for production use；By obtained dry crude crystalline 1200L,
The ethanol dissolving of 85% concentration, filtering, is concentrated into the 8% of original volume, and reclaim ethanol by filtered fluid；Concentrate is normal at 27 DEG C
Temperature is lower to be stood, and naturally cools to crystallization, leaching crystallizes and collects mother liquor；Crystallization is carried out 3 times using high concentration ethanol, natural wind
It is dry, it is dried at 28 DEG C under normal temperature, that is, high-purity qinghaosu is made, is weighed as 1.81kg, high purity 98%.
The technological process of production of the present invention is simple, easily operation, requires low to working condition, cellulase and pectase mix
Synthase preparation plays a part of promoting loose sweet wormwood leaf wall, reduction resistance to mass tranfer, effectively removes the impurity such as isolating protein, can be big
Big effect improves the recovery rate of qinghaosu, and the purity of qinghaosu is extracted in increase, can meet the qinghaosu demand of higher purity.
Embodiment 2
Fresh and alive 450kg artemisia leafs are plucked, and do sterilization processing；1.8kg, cellulase and pectin are uniformly sprayed on sweet wormwood blade face
Enzyme mass ratio is 1：0.9 mixing enzyme agent, stack in the dark and cover layer of plastic film, keeping temperature is 46 DEG C, is allowed to
Fermentation 3 days；The sweet wormwood blade after digesting that will ferment fully is dried at 25 DEG C；Sweet wormwood cured leaf after drying process is inserted into reaction
Container, add 1800L ethyl acetate in a reservoir every time, 2.5h is stirred at 60 DEG C, filter, and be repeated 3 times, fully carry
Take, and four filtered fluids are merged to obtain extract solution；Obtained extract solution is evaporated and is concentrated into original volume
9%, and reclaim ethyl acetate；The concentrate produced is stood under 25 DEG C of normal temperature, naturally cools to crystallization；Leaching crystallizes to obtain
Qinghaosu crude crystalline, and 2 washings are carried out to crude crystalline using ethyl acetate, natural air drying, enter at 26 DEG C under normal temperature
Row drying, is weighed as 2.31kg；Collect filtrate and make lower batch of raw materials for production use；By obtained dry crude crystalline 1100L,
The ethanol dissolving of 95% concentration, filtering, is concentrated into the 10% of original volume, and reclaim ethanol by filtered fluid；By concentrate at 27 DEG C
Stood under normal temperature, naturally cool to crystallization, leaching crystallizes and collects mother liquor；Crystallization is carried out 2 times using high concentration ethanol, it is natural
Air-dry, be dried at 26 DEG C under normal temperature, that is, high-purity qinghaosu is made, is weighed as 1.64kg, high purity 99%.
The technological process of production of the present invention is simple, easily operation, requires low to working condition, cellulase and pectase mix
Synthase preparation plays a part of promoting loose sweet wormwood leaf wall, reduction resistance to mass tranfer, effectively removes the impurity such as isolating protein, can be big
Big effect improves the recovery rate of qinghaosu, and the purity of qinghaosu is extracted in increase, can meet the qinghaosu demand of higher purity.
Claims (5)
- A kind of 1. preparation method of high-purity extraction qinghaosu, it is characterised in that：It comprises the following steps：Step 1：Selection；Fresh and alive artemisia leaf is plucked, and does sterilization processing；Step 2：Enzymolysis：In the uniformly cellulase of 0.2% -0.5% sweet wormwood weight of sprinkling and the pectase mixing of sweet wormwood blade face Enzyme agent processed, stack in the dark and cover layer of plastic film, keeping temperature is 40 DEG C-48 DEG C, is allowed to ferment 2-3 days；Step 3：Dry；The sweet wormwood blade after digesting that will ferment fully is dried at low temperature；Step 4：Produce extract solution；Sweet wormwood cured leaf after drying process is inserted into reaction vessel, adds 5-8 times of green grass or young crops in a reservoir The ethyl acetate of wormwood artemisia cured leaf quality, 1.5h-2.5h is stirred at 55 DEG C-60 DEG C, filtered, and repeatedly 2-3 times, fully Extraction, and each secondary filtered fluid is merged to obtain extract solution；Step 5：Concentration；Obtained extract solution in step 4 is evaporated and is concentrated into 6%-the 9% of original volume, and reclaims second Acetoacetic ester；Step 6：Crude crystalline；The concentrate produced in step 5 is stood under 25 DEG C -28 DEG C normal temperature, naturally cools to knot It is brilliant；Leaching is crystallized to obtain qinghaosu crude crystalline, and 2-3 washings, natural wind are carried out to crude crystalline using ethyl acetate It is dry, it is dried at 25 DEG C -28 DEG C under normal temperature；Collect filtrate and make lower batch of raw materials for production use；Step 7：Purification；The high concentration ethanol of 100-120 times of quality of obtained dry crude crystalline in step 6 is dissolved, Filtering, is concentrated into 8%-the 10% of original volume, and reclaim ethanol by filtered fluid；Step 8：It is high-purity crystallized to produce；Concentrate in step 7 is stood under 25 DEG C -28 DEG C normal temperature, naturally cooled to Crystallization, leaching crystallize and collect mother liquor；Crystallization is carried out 2-3 times using high concentration ethanol, natural air drying, at 25 DEG C-28 DEG C It is dried under lower normal temperature, that is, high-purity qinghaosu is made.
- A kind of 2. preparation method of high-purity extraction qinghaosu as claimed in claim 1, it is characterised in that：Described step 3 In low temperature be 25 DEG C -30 DEG C.
- A kind of 3. preparation method of high-purity extraction qinghaosu as claimed in claim 1, it is characterised in that：Described step 2 In cellulase and pectase mass ratio be 0.7：1—1：0.7.
- A kind of 4. preparation method of high-purity extraction qinghaosu as claimed in claim 1, it is characterised in that：Described step 7 In high concentration ethanol concentration be 80% -95%.
- A kind of 5. preparation method of high-purity extraction qinghaosu as claimed in claim 1, it is characterised in that：Described step 4 In stirring use silica gel product.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108299460A (en) * | 2018-03-21 | 2018-07-20 | 李文彩 | The environment-friendly high-efficiency extracting method of qinghaosu and Artemisitene |
| CN108299461A (en) * | 2018-03-21 | 2018-07-20 | 李文彩 | A kind of qinghaosu extracting method of environment-friendly high-efficiency |
| CN108770885A (en) * | 2018-06-04 | 2018-11-09 | 福建亚森农业综合开发股份公司 | Poultry nontoxic insectifuge |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101962386A (en) * | 2010-10-15 | 2011-02-02 | 肖文中 | Process for extracting arteannuin by biological compound enzymes |
-
2017
- 2017-06-30 CN CN201710520829.8A patent/CN107522713A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101962386A (en) * | 2010-10-15 | 2011-02-02 | 肖文中 | Process for extracting arteannuin by biological compound enzymes |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108299460A (en) * | 2018-03-21 | 2018-07-20 | 李文彩 | The environment-friendly high-efficiency extracting method of qinghaosu and Artemisitene |
| CN108299461A (en) * | 2018-03-21 | 2018-07-20 | 李文彩 | A kind of qinghaosu extracting method of environment-friendly high-efficiency |
| CN108299461B (en) * | 2018-03-21 | 2019-09-27 | 黑龙江赛美生物科技开发有限公司 | A kind of qinghaosu extracting method |
| CN108299460B (en) * | 2018-03-21 | 2019-11-01 | 四川协力制药股份有限公司 | The extracting method of qinghaosu and Artemisitene |
| CN108770885A (en) * | 2018-06-04 | 2018-11-09 | 福建亚森农业综合开发股份公司 | Poultry nontoxic insectifuge |
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Application publication date: 20171229 |