CN1047503A - The extracting method of Artemisinin and Artemisitene - Google Patents
The extracting method of Artemisinin and Artemisitene Download PDFInfo
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Abstract
The present invention relates to a kind of method of from the former plant of sweet wormwood, extracting Artemisinin and Artemisitene, wherein adopting lower boiling gasoline is solvent, lixiviate repeatedly, at least four times, separate Artemisinin and Artemisitene through the super short-thick type Filter column again, this method is separated soon, yield is high, solvent consumes few.
Description
The present invention relates to a kind of improving one's methods of its effective constituent Artemisinin of from the former plant of Chinese herbal artemisia, extracting, particularly relate to a kind of extracting method of new constituent Artemisitene.
Artemisinin is a kind of known new drug with anti-malarial effect, and this compound has following array structure:
Main extracting method is gasoline method and Ethanol Method in the prior art, the acetone method that particularly relates in the disclosed Chinese patent of the inventor (NC87101346A) extracts the method for Artemisinin, this method comprises that employing acetone is the effective constituent in the solvent lixiviate sweet wormwood, make sorbent material with silica gel, adopt industrial layers analysis apparatus and decompression dress post method, carry out the separation of Artemisinin.Silica gel with after carry out regeneration activating and handle repeatedly and use, thereby a kind of yield height is provided, cost is low, the crude drug that can be used for low levels extracts, and can be used for the extraction technology for artemisia annua element of suitability for industrialized production again.The weak point of this method is to adopt the industrial layers analysis apparatus that uses in the prior art to select for use common silica gel to make sorbent material, and disengaging time is long, and separating effect is relatively poor, and solvent load is big.
The objective of the invention is to avoid above-mentioned weak point of the prior art and provide a kind of Artemisinin is carried out sharp separation, high yield, the extracting method of low consumption solvent, and a kind of method of extracting another kind of new constituent Artemisitene is provided, it has following structural this compound:
Another object of the present invention is to separate the research that the new constituent Artemisitene obtain can utilize its double bond structure to open up the new series derivative to become possibility.
Another object of the present invention is can introduce deuterium on the non-swappable position of Artemisitene, to further investigate Artemisinin in the intravital metabolism of animal or human.
Purpose of the present invention can reach by following measure.A kind of method of extracting Artemisinin or another kind of new constituent Artemisitene from the former plant of Chinese herbal artemisia, this compound has following structural formula
A Artemisinin B Artemisitene
（Artemisinin） （Artemisitene）
It is characterized in that,
1) adopting lower boiling gasoline is solvent, and heat is returned and heated up in a steamer lixiviate sweet wormwood dry crushing leaf thing repeatedly, and heat is returned and heated up in a steamer at least 10 hours time;
2) with extracting solution by the proposition order directly by the super short wide column of spherical reaming silica gel is housed, carry out selective filter;
3) adopting Virahol or vinyl acetic monomer is eluent with the mixed solution of lower boiling gasoline, and whole filtrates are carried out wash-out by cylinder, concentrates effluent liquid then, promptly gets the Artemisinin crude product;
4) after the dissolve with ethanol Artemisinin purifying crude of employing 95% is handled, it is filtered;
5) above-mentioned filtrate is concentrated into two of original volume/for the moment, flow into crystallizer while hot, room temperature was placed 10-12 hour, and the crystallization of Artemisinin elaboration is just separated out lentamente; Filtrated stock then, and continue to be concentrated into 1/2nd of original volume, to place under the above-mentioned identical condition, concentrate four times so repeatedly, most Artemisinin finished product crystallizations is separated out;
6) mother liquor that will separate out Artemisinin carries out vapor distillation, tells the volatile component with special fragrance.An amount of sherwood oil of mother liquor adding makes its dissolving under warm then, under 5 ° of-10 ℃ of conditions, places 24-28 hour, separates out a small amount of Artemisinin crystallization again;
7) leach above-mentioned crystallization, mother liquor continues to be concentrated into small volume, admixes silica gel, carrying out silica gel column chromatography is solvent elution with Virahol with lower boiling gasoline, and concentrated filtrate is to there being needle crystal bunch to separate out, leach crystallization after, with ether-sherwood oil recrystallization, can get the pure product of Artemisitene again.
Purpose of the present invention can also descend measure to reach: adopt lower boiling gasoline according to requirement of the present invention, as No. 6 or No. 120 gasoline, its carbon molecule is about about 6-120, be solvent, heat is returned the effective constituent of heating up in a steamer in the leaching sweet wormwood, leaching is at least four times repeatedly, and heat is returned the time of heating up in a steamer and was at least 10 hours, and the amount of wherein said solvent is mince 3 to 7 times of weight of sweet wormwood drying.Liquid is proposed in order, the central upper portion of inherent filtration cylinder drench into, carry out selective filter, treat after whole filtrate flows, use Virahol or the vinyl acetic monomer mixed solution wash-out with lower boiling gasoline instead, wherein Virahol or vinyl acetic monomer are 20-30: 80-70 with the part by weight of lower boiling gasoline; Effluent liquid carries out promptly obtaining the Artemisinin crude product after the concentration, and this crude product purity is more than 97%, and the solvent that obtains after wherein concentrating can also utilize again.
Selective filter post of the present invention, promptly a kind of novel industrialization chromatographic apparatus is the super short-thick type silicagel column, and the water absorbing properties of used silica gel is at the special reaming silica gel of ball-type of 0.9ml/ gram, and its granularity is the 100-200 order.The diameter of this silicagel column and post height ratio are 1: 1-2, filter plate about 200 orders is arranged down, for the filling gel level even, adopt disposable silica gel throw-in play, with the solvent identical with vat liquor, enter cylinder from the bottom, to get rid of the intravital air of post, can open the leach liquor valve this moment, allow leach liquor return the order that heats up in a steamer lixiviate by four heat, concentrate from central upper portion and quantitatively to drench cylinder, wherein, the flow through flow velocity of Filter column of vat liquor is 3.5-4.5 liter/minute kilogram, solution is not diffused into post jamb flowing to cylinder lower part outlet fashion like this, thereby eliminated " post jamb effect ", improved the charge capacity of cylinder, also played the effect of cylinder removal of contamination.Take cylinder of the present invention that the raising flow velocity is arranged, shorten disengaging time and be easy to fill advantages such as even.
According to the present invention, the consumption of described silica gel calculates by following formula:
(W-2.8)/the mince kilogram amount of required silica gel of per hundred kilograms of artemisia leafs of 0.7 * 6=
Wherein:
W: the dry weight of per hundred kilograms of sweet wormwood industrial naptha extracts
2.8: be rinsed the part dry measure
0.7: reaming silica gel adsorption constant, (weight that is the silica gel optimal adsorption solvent extract of water regain 1ml is 0.7 gram)
6: 6 times of silica gel adsorption amount
Around here, Zui Jia W value is 6-7.
For example: during W=7,
Then: (7-2.8)/0.7 * 6=4.2/0.7 * 6=36%
Be that per hundred kilograms of sweet wormwoods are in requisition for 36 kilograms in reaming silica gel
The present invention's method adopts and progressively concentrates primary crystallization method artemisinin purifying and can further obtain another kind of new constituent Artemisitene, to be the 60-80 of Artemisinin coarse crystallization weight 95% alcohol at normal temperature dissolving doubly, filter, and be concentrated into original volume two/for the moment, flow in the crystallizer while hot, room temperature was placed 10-12 hour, the crystallization of Artemisinin elaboration is slowly separated out, then mother liquor is filtered, and continue to be concentrated into 1/2 of original volume, the same with above-mentioned condition, concentrate at least four times so repeatedly, till separating out to most Artemisinin finished product crystallizations.Mother liquor stays the separation of doing compositions such as Artemisitene.
Above-mentioned mother liquor is carried out vapor distillation, tell volatile component with special fragrance, down an amount of sherwood oil adding mother liquor is dissolved warm then, under 5 ° of-10 ℃ of conditions, placed 24-28 hour, leach a small amount of Artemisinin crystallization, after mother liquor concentrates and admixes silica gel, carry out silica gel column chromatography, with the mixed solvent wash-out of Virahol with No. 6 gasoline, this solvent Virahol is (weight) 20-30: 80-70 with the ratio of No. 6 gasoline, collects ultraviolet 210nm and checks that the absorption flow point is arranged, concentrating promptly has fine needle crystal bunch to separate out, after leaching crystallization, add diethyl ether again-the sherwood oil recrystallization, can obtain the pure product of 98.8% Artemisitene.
In order to reclaim the repeated use of residual solvent and silica gel, the selection Filter column that can adopt acetone rinsing to separate to finish is used distilled water flushing at last once more, and solvent not only can all reclaim like this, and can directly reuse after oven dry.The bake out temperature of reaming silica gel must not be higher than 110 ℃.Because too high very easily the causing of the reaming silica gel of suction heating bursts,, after moisture in the silica gel is removed substantially, temperature is increased to 110 ℃ again so be preferably in 80-95 ℃ when beginning to dry.The time of oven dry exceeds with the moisture required time in the basic removal reaming silica gel, is preferably in 60-80 minute.When the silica gel that uses this method to toast can be reused about 30 times, silica gel burst rate still less than 10%.Its specific practice is: filter post with acetone rinsing, at first effusive part mainly is the solvent of Virahol and 6# gasoline, when effluent liquid becomes when blackish green, for the acetone rinsing flow point, this is received respectively, to colourless.Use distilled water flushing then instead, each flow point of the acetone in the cylinder is distilled recovery respectively.Take out silica gel, oven dry then is in order to reusing.
With most preferred embodiment of the present invention aforesaid method is carried out the description of indefiniteness below.
Embodiment 1
The extraction of Artemisinin
Taking by weighing weight loss on drying is the sweet wormwood cured leaf powder 200kg of 8.5-9%, drops in the extractor, adds No. 6 industrial napthas of 5 times of weight of quite former medicine (1000kg), is heated to 60 ℃ and returns and heated up in a steamer 4 hours, suction filtration while hot, filtrate preservation; Add gasoline 850kg again No. 6 to extractor, carry out heat and return to heat up in a steamer and extracted 3 hours, suction filtration while hot, extracting solution is preserved in addition, and heat is returned to heat up in a steamer and is extracted four times so repeatedly, returns the times of heating up in a steamer for four times to be respectively 4 hours, and 3 hours, 2 hours, 1 hour mode is carried out.Proposing liquid preserves standby respectively.
Get the special reaming silica gel of ball-type 72kg, the super short-thick type Filter column of once packing into.Stud with one 200 purposes sieve in the bottom of Filter column, 50 centimetres of the diameters of this cylinder, height are 100 centimetres.Behind the leveling silica gel surface, directly above-mentioned proposition liquid is pressed the proposition order, directly, pass through cylinder with 16 liters/minute flow velocitys from the top at center, silica gel top layer, after the 4th proposition liquid has flowed, change the mixed solution wash-out of 6% Virahol or No. 6 industrial napthas of 10% vinyl acetic monomer.Ratio is: different third ferment: No. 6 industrial napthas (6: 94v/v) or vinyl acetic monomer: No. 6 industrial napthas (10: 90v/v).Flow velocity is the same, treats that effluent liquid becomes when colourless, begins to detect, and collects the outflow part that contains Artemisinin, concentrates effluent liquid, and room temperature is placed then, and when seeing that needle occurring in the postpone concentrated solution separates out, suction filtration is handled, and can get Artemisinin coarse crystallization 1.3kg.
Get sweet wormwood crude product 1.3kg, add 95% ethanol of 70 times of weight, this crude product of normal-temperature dissolution filters then, filtrate is concentrated into two of original volume/for the moment, concentrated solution flows in the crystallizer, and the crystallizer room temperature was placed 10 hours, and then seeing has crystallization to separate out in jar, extract mother liquor out, the reconcentration volume is placed as previously mentioned to half, and crystallization is separated out.So progressively concentrate quadruplication, collect crystallization, drain.Under 70-80 ℃ of temperature, the oven dry crystallization gets pure Artemisinin 1.16kg, and content is 99.65%, and it is 99.72% that its whole process is put forward yield.The Artemisinin product quality specifications that the inventive method is extracted and the material balance table of Artemisinin see Table 1 and table 2 respectively:
Table 1
This handicraft product of title specification country tentative specifications standard
Molecular formula C
15H
23O
5C
15H
22O
5
155 ℃ 153-155 ℃ of fusing point
Specific optical rotation [α] °
5+ 75.38(C=2 C
2H
5OH) [α] °
8+ 73-78 ° of (C=2 C
2H
5OH)
Residue on ignition 0.04% should not surpass 0.1%
Weight loss on drying 0.12% should not surpass 0.5%
Content 99.65% 97.0-103%
Annotate: test result is by the Yunnan Kunming pharmaceutical factory test in one's power of Sichuan drug inspection
Table 2
The material balance table of Artemisinin:
Sequence number name of material weight (kilogram) artemislnin content % remarks
1 sweet wormwood cured leaf meal 200 0.63
2 6# industrial napthas 3,550 0.01
The 3 sweet wormwood dregs of a decoction (drying) 187 0.0021
4 crude products 1.3 97
5 recrystallizations 1.16 99.65
6 crystalline mother solutions 0.1054 100
7 mother liquor yields 0.0791 99
8 Artemisitenes 0.0238 98.81
9 mother liquors remain following batch of 0.0036 0.28 mother liquors and apply mechanically
10 whole process are put forward yield 99.72
Annotate: 1. above result is 5 batches a mean value.
2. lab scale and pilot scale content get consistent results.
Embodiment 2
The separation of Artemisitene
Get the Artemisinin coarse-grain, progressively concentrate four times, tell the mother liquor behind the Artemisinin, continue to be concentrated into small volume (the ethanol quantity of distillate is degree of being reduced to obviously), carry out vapor distillation this moment with 95% ethanol.Tell volatile component, behind the moisture content, add 20 times of weight 6# industrial napthas in the removal mother liquor with special perfume (or spice), warm dissolving, filtered while hot, filtrate (best 5-10 ℃) under 10 ℃ was placed one, then had a small amount of needle (Artemisinin) to separate out.Leach filtrate continuation and be concentrated into 1/4 o'clock of original volume, room temperature is placed, and then has fine needle crystal bunch to form on the bottle wall.Leach haptophore, with cold 6# industrial naptha flushing, 80 ℃ of oven dry get coarse-grain.
With above coarse-grain, be dissolved in vinyl acetic monomer, adding 60 gram chromatographic silica gels mixes thoroughly, fling to solvent, after 80 ℃ of oven dry, carry out silica gel column chromatography, make eluent with sherwood oil (60-90 ℃)-actual use value of Virahol (94: 16), develop the color with 1% Vanillin sulfuric acid liquid, collect to merge developer is and become blue each flow point of tide (or at 210nm check with ultraviolet) behind the apricot again and reclaim solvent and get a colourless crystallization body, get the pure product 0.02381kg of Artemisitene with sherwood oil-ether recrystallization, promptly Artemisinin carry the amount 1.894%.
Embodiment 3
Heat up in a steamer the selection of extraction time and see Table 3 for hot time
Table 3
6# solvent Artemisinin heat is returned and is heated up in a steamer the artemisin Artemisinin of at every turn turning green
Gasoline is carried to such an extent that amount is put forward yield with the content of starting materials input amount total content number of times time of heating up in a steamer
(kg) (kg) (kg) (hour) (kg) (%)
5 1.0836 86
4 1.0829 85.9
1000 leaves, bud 200 1.26 13 1.0141 80.5
2 0.9872 78.3
1 0.6311 50
Embodiment 4
Heat is returned the selection of heating up in a steamer number of times and is seen Table 4
Table 4
Blue heat returns to slip and carries each heat artemisin Artemisinin of turning green and always carry in the 6# solvent raw material
Gasoline contains with content of starting materials input amount artemisin measures the number of times slide time amount of getting and must measure yield
(kg) (kg) (kg) (hour) (kg) (kg) (%)
1 4 1.0829 85.94
Leaf 23 0.1388 1.2217 96.96
1000 buds 200 1.26 32 0.0279 1.2508 99.26
4 1 0.0061 1.2569 99.76
5 1 0.0021 1.2590 99.92
Embodiment 5
The 6# industrial naptha leaves standstill extraction and heat and returns and to heat up in a steamer the extraction Artemisinin and carry this taking technique stability observing that relatively reaches of yield and see Table 5 and table 6 respectively
Table 5
The lixiviate mode leaves standstill hot the returning of lixiviate and heats up in a steamer lixiviate
Test sequence number 123 average 456 is average
Sweet wormwood throws 100 100 100 100 100 100 100 100
Go into amount (kg)
Artemisinin real 0.63 0.63 0.63 0.63 0.63 0.63 0.63 0.63
Border content (kg)
Actually soak 0.6098 0.6106 0.6102 0.6102 0.6298 0.6297
Output (kg)
When lixiviate is total 72 72 72 72 10 10 10 10
Between (hour)
Total proposition 96.86 99.96
Rate %
Embodiment 6
Get 200 kilograms in sweet wormwood cured leaf powder, the method described in the embodiment 1 of pressing is extracted Artemisinin, and wherein solvent uses balance to see Table 7:
Table 7
Operation number technology title input amount yield waste wastage rate
（kg） （kg） （kg） %
1 6# gasoline extracts 1,000 860 for the first time
2 6# gasoline extract 850 852 for the second time
3 6# gasoline extract 850 864 for the third time
4 6# gasoline extract 850 873 the 4th time
5 dregs of a decoction dash and steam 98 13 0.37
6 acetone rinsing cylinders 254 248 6 2.36
7 6% Virahol 6# fluid 521 511 10 1.90
8 95% ethanol 91 90.30 0.8 0.87
Amount to 4,416 29.8 0.675
Annotate: 1. above numerical value is the mean value of five experiments,
2. the total solvent waste is 29.8kg; Account for 0.675% of the total usage quantity of solvent, account for 14.9% of survival dose
Embodiment 7
Implementing the inventive method process, in order to strengthen the monitoring of Artemisinin effluent liquid, and adapt to change solvent, adopt colour-change to the Filter column effluent liquid to detect Artemisinin and whether exists, this detection means has been created condition to full scale production technology realization automated operation.Following three qualitative checking methods will be applicable to the Artemisinin that monitoring is extracted through technology of the present invention.
A proves that when effluent liquid has special fragrance this effluent liquid contains Artemisinin;
B, the silica gel thin-layer detection method;
Get one of little silica gel thin-layer plate, on thin plate, drip a stream of droplets fluid, it is diffusing to allow solvent wave voluntarily, drip sherwood oil liquid in former dot center then, treat stone gasoline ether wave loose after, with 10% Vanillin sulfuric acid liquid, the spraying demonstration, if the mottle center shows apricot and becomes damp blue look gradually, then prove and contain Artemisinin in the effluent liquid;
C gets effluent liquid 50ml, and solvent is reclaimed in water-bath, concentrates this solution then, places a moment 30 ℃ of temperature, if see that having needle to separate out proves that then this effluent liquid contains Artemisinin.
Embodiment 8
Can adopt low temperature roller formula desiccating method to the reaming silica gel after using, removing moisture, after oven dry again.Storing time is 60-80 minute, and bake out temperature is no more than 110 ℃.The method of taking elevated temperature gradually is to avoid the described silica gel that contains large quantity of moisture owing to bursting that the fierceness vaporization of moisture causes.As seen following table toasts silica gel the most nearly 48 times the time repeatedly with high-temperature smelting pot, the observations of the fried rate that it uses repeatedly.(seeing Table 8)
Table 8
After testing each use of sweet wormwood silica gel oven dry oven dry, dry the remarks that sieve
Numbering consumption consumption temperature-time
(gram) (gram) (℃) (hour)＞200 order persons accumulative total gram
1 100 41 90 4
2 100 40.9801 90 4
Use for 3 100 40.9654 90 4 0.1211 10 times
4 100 41.0081 90 4
Use accumulative total 5 100 41.1584 90 4 0.1734 28 times
6 100 41.3421 90 4 0.2144 38 accumulative totals
7 100 41.9563 90 4 0.2810 48 accumulative totals
This experiment used silica gel is the special reaming silica gel of 100-200 order ball-type, sifts out fine powder with 200 mesh sieves before using.Use up oven dry back in addition crosses 200 sieve fine powders and preserves and weigh at every turn.Silica gel consumption weight increases system and filters badly because of proposing liquid, has due to silt in a small amount of raw material sneaks into.Experiment 6 experiments 7 all are 90 ℃ fully took out by 600 ℃ of high temperature after the oven dry more while hot in two minutes, slowly after the cooling, crossed the result that 200 mesh sieves are weighed and obtained then.
According to above test:
Silica gel uses 48 times continuously, and silica gel leads to 200 mesh sieve hole persons, cumulative weight 0.2810 gram, and it bursts rate is 0.685%.Behind the continuous use silica gel 28 times, 90 ℃ of fully oven dry, it bursts rate is 0.42%.Use 29 to 48 times continuously, 90 ℃ of fully oven dry were passed through 600 ℃ of high temperature two minutes more while hot, and it bursts rate 0.26%.
So draw according to above-mentioned experiment: as long as the thorough drying post-heating, even high temperature there is no and bursts phenomenon.
Using infrared drying to measure also obtains and above-mentioned same result.
The present invention has following advantage compared to existing technology:
1, adopts low boiling gasoline heat to return and heat up in a steamer active ingredient in the extraction sweet wormwood, directly filter fast by ultrashort thick silica gel cylinder proposing liquid, saved and concentrated the oven dry of mix silica gel; Numerous and diverse technology such as upper prop has reduced the post jamb effect, has improved post effect and carrying capacity.
2, the reaming silica gel that uses in the selective filter post need not activation process, directly repeats to make after the oven dry With, save operation sequence.
3, adopt the primary crystallization method that progressively concentrates in purification process technology, greatly improved the purity of qinghaosu, make it to reach the 99.65%(national regulation more than 97%). And can separate and obtain a kind of newfound composition-Artemisitene.
4, the monitoring method of qinghaosu leaching process provided by the present invention is all industrialization of technology, and automation provides condition. Because technology characteristics of the present invention and effect so that the production cycle shortened to 4 days by original about 10 days.
5, solvent-oil ratio reduces greatly. Wherein by former consumption agent (such as acetone) amount 55%, be down to 14.9%. Be 0.675% of the total use amount of solvent, and omnidistance raise rate and reached 99.72% of crude drug total content.
Be below the comparison sheet of several main production leading indicators for your guidance.
Main production indices comparison sheet
Consist of method of the present invention, being described by above-described embodiment, can infer simultaneously, only otherwise depart from the present invention's essence and scope, can carry out some change to it.
Claims (11)
1, a kind of method of extracting Artemisinin and Artemisitene, this compound has following structural formula:
It is characterized in that:
1) adopting lower boiling gasoline is solvent, and heat is returned to heat up in a steamer and extracted sweet wormwood dry crushing leaf thing, at least 10 hours extraction times repeatedly.
2) with extracting solution by carry the order directly by spherical special reaming silica gel super short-thick type selective filter post is housed;
3) adopting the mixed solution of Virahol or vinyl acetic monomer and lower boiling gasoline is eluent, and whole cylinders are carried out wash-out, concentrates effluent liquid, promptly gets the Artemisinin crude product;
4) behind the dissolve with ethanol Artemisinin crude product of employing 95%, it is filtered.
When 5) above-mentioned filtrate being concentrated into original volume 1/2, flow into crystallizer while hot, room temperature was placed 10-12 hour, the crystallization of Artemisinin finished product is separated out, leach mother liquor then, and continue to be concentrated into 1/2 of original volume, with placing under the above-mentioned condition, concentration is at least four times so repeatedly.The crystallization of most Artemisinin finished product is all separated out;
6) will separate out Artemisinin crystalline mother liquor and carry out vapor distillation, place 24-28 hour 5-10 ℃ of condition down with an amount of sherwood oil adding mother liquor dissolving, leach a small amount of Artemisinin crystallization warm;
7) mother liquor that leaches after the above-mentioned crystallization concentrates, concentrated solution carries out silica gel column chromatography, with Virahol and No. 6 gasoline is solvent elution, and at 210nm effluent liquid is detected (or check with the spraying colour developing of 1% Vanillin sulfuric acid liquid) collection positive reaction flow point with ultraviolet ray, being concentrated into a fine acicular bunch crystallization separates out, after leaching crystallization, again with ether--the sherwood oil recrystallization can get the pure product of Artemisitene.
2, by the described method of claim 1, the amount that it is characterized in that described solvent for the Artemisinin drying mince weight 3-7 doubly.
3, by claim 1 or 2 described methods, it is characterized in that heat is returned repeatedly heats up in a steamer extraction at least four times.Heat is returned at least 10 hours time.
4, it is characterized in that by the described method of claim 1, is 20-30: 80-70 as the Virahol of eluent or vinyl acetic monomer with the ratio of lower boiling gasoline weight.
5, by the described method of claim 1, it is characterized in that the diameter of described Filter column and the ratio of cylinder height are 1: 1-2.
6, by the described method of claim 1, it is characterized in that described silica gel is to have water absorbing properties to restrain at 0.9ml/ at least; The special reaming silicon particle of 100-200 purpose ball-type.
7, by claim 1 or 6 described methods, it is characterized in that the consumption of described silica gel calculates by following formula:
(W-2.8)/0.7 kilogram required silica gel kilogram of artemisia leaf amount *=per hundred.
Wherein, The dry weight of the thing of per hundred kilograms of Artemisinin solvent extraction of W.
8, by claim 4 or 5 described methods, it is characterized in that, vat liquor flow through the flow velocity of Filter column be the 3.4-4.5 liter/minute. kilogram.
9,, it is characterized in that described purifying is 60-80 times of Artemisinin coarse crystallization weight with 95% alcoholic acid amount by the described method of claim 1.
10, by the described method of claim 7, it is characterized in that described special reaming silica gel is carried out baking processing, the temperature of anhydrating must not be greater than 1100 ℃, and storing time is 60-80 minute.
11, by the described method of claim 1, it is characterized in that the Filter column Artemisinin can adopt following method in the monitoring stream fluid.
A. when having special fragrance, effluent liquid proves that this effluent liquid contains Artemisinin.
B. silica gel thin-layer detection method;
Get one of little silica gel thin-layer plate, on thin plate, drip a stream of droplets fluid, it is diffusing to allow solvent wave voluntarily, drip sherwood oil liquid in former dot center then, treat stone gasoline ether wave loose after, with 10% Vanillin sulfuric acid liquid, spraying shows, then proves and contains Artemisinin in the effluent liquid if the mottle center shows apricot and becomes damp blue look gradually.
C. get effluent liquid 50ml, solvent is reclaimed in water-bath, concentrates this solution then, places a moment 30 ℃ of temperature, if see that having needle to separate out proves that then this effluent liquid contains Artemisinin.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 89103384 CN1030080C (en) | 1989-05-25 | 1989-05-25 | Method for extracting arteannuin and methenylarteannuin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 89103384 CN1030080C (en) | 1989-05-25 | 1989-05-25 | Method for extracting arteannuin and methenylarteannuin |
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| Publication Number | Publication Date |
|---|---|
| CN1047503A true CN1047503A (en) | 1990-12-05 |
| CN1030080C CN1030080C (en) | 1995-10-18 |
Family
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 89103384 Expired - Fee Related CN1030080C (en) | 1989-05-25 | 1989-05-25 | Method for extracting arteannuin and methenylarteannuin |
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| CN (1) | CN1030080C (en) |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2706166A1 (en) * | 1993-06-08 | 1994-12-16 | Archimex Ass | Process for the extraction of artemisinin |
| CN100341877C (en) * | 2005-12-08 | 2007-10-10 | 侯金荣 | Artemisinin extracting method |
| CN101130548B (en) * | 2006-08-25 | 2010-11-03 | 上海诺德生物实业有限公司 | Method for extracting and producing high content arteannuin |
| CN102219790A (en) * | 2011-05-05 | 2011-10-19 | 广西仙草堂制药有限责任公司 | Green extraction process for artemisinin |
| CN102617591A (en) * | 2012-03-07 | 2012-08-01 | 广州牌牌生物科技有限公司 | Method for producing artemisinin from artemisia annua serving as Chinese herbal medicine |
| CN103694249A (en) * | 2013-12-28 | 2014-04-02 | 湘西自治州奥瑞克医药化工有限责任公司 | Production technology for extracting artemisinin from artemisia annua |
| CN105779129A (en) * | 2016-04-22 | 2016-07-20 | 四川蓝伯特生物科技有限责任公司 | Method for preparing Artemisia apiacea volatile oil from Artemisia apiacea waste mother liquor, method for preparing byproduct and obtained byproduct |
| CN107235988A (en) * | 2017-06-21 | 2017-10-10 | 禹州市天源生物科技有限公司 | A kind of extracting method of qinghaosu and Artemisitene |
| CN108299460A (en) * | 2018-03-21 | 2018-07-20 | 李文彩 | The environment-friendly high-efficiency extracting method of qinghaosu and Artemisitene |
| CN112129721A (en) * | 2020-10-23 | 2020-12-25 | 湖南星辰生物科技股份有限公司 | Ultraviolet visible light rapid detection method for artemisinin |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102285995A (en) * | 2011-06-24 | 2011-12-21 | 成都恩威投资（集团）有限公司 | Method for extracting artemisinin |
-
1989
- 1989-05-25 CN CN 89103384 patent/CN1030080C/en not_active Expired - Fee Related
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2706166A1 (en) * | 1993-06-08 | 1994-12-16 | Archimex Ass | Process for the extraction of artemisinin |
| CN100341877C (en) * | 2005-12-08 | 2007-10-10 | 侯金荣 | Artemisinin extracting method |
| CN101130548B (en) * | 2006-08-25 | 2010-11-03 | 上海诺德生物实业有限公司 | Method for extracting and producing high content arteannuin |
| CN102219790A (en) * | 2011-05-05 | 2011-10-19 | 广西仙草堂制药有限责任公司 | Green extraction process for artemisinin |
| CN102617591A (en) * | 2012-03-07 | 2012-08-01 | 广州牌牌生物科技有限公司 | Method for producing artemisinin from artemisia annua serving as Chinese herbal medicine |
| CN103694249A (en) * | 2013-12-28 | 2014-04-02 | 湘西自治州奥瑞克医药化工有限责任公司 | Production technology for extracting artemisinin from artemisia annua |
| CN105779129A (en) * | 2016-04-22 | 2016-07-20 | 四川蓝伯特生物科技有限责任公司 | Method for preparing Artemisia apiacea volatile oil from Artemisia apiacea waste mother liquor, method for preparing byproduct and obtained byproduct |
| CN107235988A (en) * | 2017-06-21 | 2017-10-10 | 禹州市天源生物科技有限公司 | A kind of extracting method of qinghaosu and Artemisitene |
| CN108299460A (en) * | 2018-03-21 | 2018-07-20 | 李文彩 | The environment-friendly high-efficiency extracting method of qinghaosu and Artemisitene |
| 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 |
| CN112129721A (en) * | 2020-10-23 | 2020-12-25 | 湖南星辰生物科技股份有限公司 | Ultraviolet visible light rapid detection method for artemisinin |
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