CN105198956A - Method for extracting triptolide in tripterygium wilfordii by using subcritical method - Google Patents
Method for extracting triptolide in tripterygium wilfordii by using subcritical method Download PDFInfo
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- CN105198956A CN105198956A CN201510766447.4A CN201510766447A CN105198956A CN 105198956 A CN105198956 A CN 105198956A CN 201510766447 A CN201510766447 A CN 201510766447A CN 105198956 A CN105198956 A CN 105198956A
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Abstract
The invention discloses a method for extracting triptolide in tripterygium wilfordii by using subcritical method, and belongs to the field of extracting natural active ingredients. The method comprises the following steps: firstly, crushing tripterygium wilfordii roots, and then screening through a sieve of 20-80 meshes; secondly, putting into a subcritical water extraction device, and extracting for 30-90min for 1-3 times under the condition that the temperature is 100-150 DEG C, the pressure is 0.5-2.0MPa, and the liquid-solid ratio of subcritical water to tripterygium wilfordii powder is 10-40mL/g; thirdly, collecting an extract, standing, and then performing centrifugation to obtain a deposit namely a crude product; and finally, performing rotary evaporation concentration and column chromatography to obtain the triptolide. According to the method disclosed by the invention, the triptolide is extracted by adopting an advanced subcritical water extraction technology, the extraction time is short, and the extraction efficiency is high. The method is green and pollution-free, is low in equipment requirement, and is easy to realize industrial production.
Description
Technical field
The present invention relates to a kind of method utilizing Subcritical water chromotagraphy triptolide, belong to active skull cap components and extract field.
Background technology
Triptolide is also known as Triptolide, triptolide, it is a kind of Diterpenoid epoxide lactone compound extracted from the root of Celastraceae plant trypterygine, leaf, flower and fruit, the main active ingredient of Radix Tripterygii Wilfordii extract is constituted with alkaloids such as wilforine, Wilforine, wilforgine, wilfortrine, wilfozine and the bright alkali of trypterygine, be insoluble in water, be soluble in methyl alcohol, dimethyl sulfoxide (DMSO), dehydrated alcohol, ethyl acetate, chloroform etc.There is anti-inflammatory and immunosuppressive action.Triptolide is one and has multiple bioactive natural product, derives from the root of Chinese herb triperygium wilfordii, and to show that it has anti-oxidant in research, resisting rheumatoid disease, anti-senile dementia, the effect such as anticancer.
Mainly adopt the organic solvent extraction triptolides such as ethanol, chloroform or ethyl acetate both at home and abroad at present, extracting method mainly methyl alcohol or 95% ethanol is the reflux extraction of solvent, ultrasonic extraction etc.The people such as Yang Lei (Yang Lei, Li Tong, Zhang Lin, Lu Qi, Zu YuanGang. pressurized solvent method extracts triptolide and condition optimizing [J] thereof. and chemical industry is in progress, and 2010, (02): 323-327) adopt pressurized solvent method with 1,2-ethylene dichloride is solvent, and the actual extracting rate of triptolide can reach 0.173 ‰, and purity is 1.21%.The people such as Cheng Jingli (Cheng Jingli, Zhu Lie, Zhu Guonian, Xu Zhenyuan. the extraction process [J] of triptolide. agricultural chemicals, 2005, (07): 316-318.) extracting the triptolide in trypterygine leaf with 70% methanol eddy, extraction yield can reach 0.014%.The extracting method of traditional employing organic solvent will inevitably produce the problem such as dissolvent residual, environmental pollution, and the comparatively high temps in leaching process easily causes the decomposition of the determination system of thermal unstable material such as diterpenes, so in the urgent need to finding a kind of technique that can make up these deficiencies.
Subcritical water is also called high-pressure water heating, refers to when pressure is greater than 1MPa, water is heated to more than 100 DEG C, and critical temperature less than 374 DEG C, water body still keeps liquid state.When water reaches subcritical state, aqueous polar reduces, and is similar to organic solvent, can be used for extracting low-pole or nonpolar composition.Subcritical water can make the sex change such as protein, starch simultaneously, brings convenience to follow-up separation and purification, is highly suitable for the extraction of the scale operation of industry.This kind of method extracts that triptolide is inexpensive, pollution-free and extraction yield is high, is a kind of green abstraction technique, has not yet to see report.
Summary of the invention
The object of the invention is to solve shortcomings and deficiencies of the prior art, provide a kind of pre-treatment simple, extract extraction yield high, the method for the industrial Subcritical water chromotagraphy triptolide of adaptation of constituent structure of simultaneously remaining valid again.
A kind of method utilizing Subcritical water chromotagraphy triptolide that the present invention proposes, specifically comprises the following steps:
(1) first trypterygine (root) pulverizer is pulverized, after 20 ~ 80 eye mesh screens, obtain Common Threewingnut Root.
(2) Common Threewingnut Root that a certain amount of step (1) obtains is taken in Subcritical water chromotagraphy device, Extracting temperature 100 ~ 150 DEG C, extraction time 30 ~ 90min, extract pressure 0.5 ~ 2.0MPa, solid-liquid ratio 1:10 ~ the 1:40g/mL of Common Threewingnut Root and solvent, in solvent, ethanol contend per-cent 20 ~ 80%, obtains mixed liquor A.
(3) mixed liquor A is put into the centrifuge tube of whizzer, under rotating speed 4000 ~ 6000r/min after centrifugal 5 ~ 10min, take off centrifuge tube, obtain supernatant liquor B and sediment B.
(4) adopt rotary evaporation to be concentrated by supernatant liquor B, obtain triptolide crude product C.Be that the crude product C of 0.25 ~ 2g/mL admixes in macroporous adsorbent resin by concentration, loading quality and macroporous resin volume ratio are 1:10 ~ 1:20g/L, then be placed in chromatography column and carry out wash-out separation, collect elutriant stage by stage, detect triptolide content in elutriant, merge each and contain triptolide elutriant, rotary evaporation concentrates, crystallization, obtains triptolide sterling.
Wherein, the Subcritical water chromotagraphy device described in step (2) is TGYF-A type stainless steel high pressure extract device.Macroporous adsorbent resin described in step (4) is any one in D101, D4020, AB-8.
A kind of method utilizing Subcritical water chromotagraphy triptolide that the present invention proposes, the triptolide extraction yield obtained is 0.02 ~ 0.06 ‰.
Advantage of the present invention is as follows:
(1) a kind of method utilizing Subcritical water chromotagraphy triptolide of the present invention's proposition, adopt Subcritical water chromotagraphy triptolide, extraction time is short, and extraction efficiency is high.
(2) a kind of method utilizing Subcritical water chromotagraphy triptolide of the present invention's proposition, this technical process is simple, with short production cycle, green non-pollution, and equipment requirements is low, easily realizes industrial application.
Accompanying drawing explanation
Fig. 1: a kind of process flow sheet utilizing the method for Subcritical water chromotagraphy triptolide that the present invention proposes.
Embodiment
Below in conjunction with drawings and Examples, the present invention is described in further detail.
A kind of method utilizing Subcritical water chromotagraphy triptolide that the present invention proposes, as shown in Figure 1, specifically comprises the following steps:
(1) pre-treatment of trypterygine.First medicinal trypterygine (root) pulverizer is pulverized, after 20 ~ 80 eye mesh screens, obtain Common Threewingnut Root.
(2) Common Threewingnut Root that a certain amount of step (1) obtains is taken in Subcritical water chromotagraphy device, Extracting temperature 100 ~ 150 DEG C, extraction time 30 ~ 90min, extract pressure 0.5 ~ 2.0MPa, solid-liquid ratio 1:10 ~ the 1:40 of Common Threewingnut Root and solvent, in solvent, ethanol contend per-cent 20 ~ 80%, obtains mixed liquor A.
(3) mixed liquor A is put into the centrifuge tube of whizzer, under rotating speed 4000 ~ 6000r/min after centrifugal 5 ~ 10min, take off centrifuge tube, obtain supernatant liquor B and sediment B.
(4) adopt rotary evaporation to be concentrated by supernatant liquor B, obtain triptolide crude product C.Be that the crude product C of 0.25 ~ 2g/mL admixes in macroporous adsorbent resin by concentration, loading quality and macroporous resin volume ratio are 1:10 ~ 1:20g/L, then be placed in chromatography column and carry out wash-out separation, collect elutriant stage by stage, detect triptolide content in elutriant, merge each and contain triptolide elutriant, rotary evaporation concentrates, crystallization, obtains triptolide sterling.
Wherein, the Subcritical water chromotagraphy device described in step (2) is TGYF-A type stainless steel high pressure extract device.Macroporous adsorbent resin described in step (4) is any one in D101, D4020, AB-8.
A kind of method utilizing Subcritical water chromotagraphy triptolide that the present invention proposes, the triptolide extraction yield obtained is 0.02 ~ 0.06 ‰.
embodiment 1:
(1) pre-treatment of trypterygine.First medicinal trypterygine (root) pulverizer is pulverized, after 20 eye mesh screens, obtain Common Threewingnut Root.
(2) Common Threewingnut Root that a certain amount of step (1) obtains is taken in Subcritical water chromotagraphy device, Extracting temperature 100 DEG C, extraction time 30min, extract pressure 1.0MPa, the solid-liquid ratio 1:15 of Common Threewingnut Root and solvent, in solvent, ethanol contend per-cent 20%, obtains mixed liquor A.
(3) mixed liquor A is put into the centrifuge tube of whizzer, under rotating speed 5000r/min after centrifugal 10min, take off centrifuge tube, obtain supernatant liquor B and sediment B.
(4) adopt rotary evaporation to be concentrated by supernatant liquor B, obtain triptolide crude product C.Be that the crude product C of 0.1g/mL admixes in macroporous adsorbent resin by concentration, loading quality and macroporous resin volume ratio are 1:20g/L, then be placed in chromatography column and carry out wash-out separation, collect elutriant stage by stage, detect triptolide content in elutriant, merge each and contain triptolide elutriant, rotary evaporation concentrates, crystallization, obtains triptolide sterling.
Wherein, the Subcritical water chromotagraphy device described in step (2) is TGYF-A type stainless steel high pressure extract device.Macroporous adsorbent resin described in step (4) is D101.
A kind of method utilizing Subcritical water chromotagraphy triptolide that the present invention proposes, the triptolide extraction yield obtained is 0.06 ‰.
embodiment 2:
(1) pre-treatment of trypterygine.First medicinal trypterygine (root) pulverizer is pulverized, after 60 eye mesh screens, obtain Common Threewingnut Root.
(2) Common Threewingnut Root that a certain amount of step (1) obtains is taken in Subcritical water chromotagraphy device, Extracting temperature 110 DEG C, extraction time 50min, extract pressure 1.5MPa, the solid-liquid ratio 1:15 of Common Threewingnut Root and solvent, in solvent, ethanol contend per-cent 40%, obtains mixed liquor A.
(3) mixed liquor A is put into the centrifuge tube of whizzer, under rotating speed 4000r/min after centrifugal 15min, take off centrifuge tube, obtain supernatant liquor B and sediment B.
(4) adopt rotary evaporation to be concentrated by supernatant liquor B, obtain triptolide crude product C.Be that the crude product C of 0.5g/mL admixes in macroporous adsorbent resin by concentration, loading quality and macroporous resin volume ratio are 1:15g/L, then be placed in chromatography column and carry out wash-out separation, collect elutriant stage by stage, detect triptolide content in elutriant, merge each and contain triptolide elutriant, rotary evaporation concentrates, crystallization, obtains triptolide sterling.
Wherein, the Subcritical water chromotagraphy device described in step (2) is TGYF-A type stainless steel high pressure extract device.Macroporous adsorbent resin described in step (4) is D4020.
A kind of method utilizing Subcritical water chromotagraphy triptolide that the present invention proposes, the triptolide extraction yield obtained is 0.04 ‰.
embodiment 3:
(1) pre-treatment of trypterygine.First medicinal trypterygine (root) pulverizer is pulverized, after 60 eye mesh screens, obtain Common Threewingnut Root.
(2) Common Threewingnut Root that a certain amount of step (1) obtains is taken in Subcritical water chromotagraphy device, Extracting temperature 120 DEG C, extraction time 70min, extract pressure 2.0MPa, the solid-liquid ratio 1:15 of Common Threewingnut Root and solvent, in solvent, ethanol contend per-cent 60%, obtains mixed liquor A.
(3) mixed liquor A is put into the centrifuge tube of whizzer, under rotating speed 6000r/min after centrifugal 5min, take off centrifuge tube, obtain supernatant liquor B and sediment B.
(4) adopt rotary evaporation to be concentrated by supernatant liquor B, obtain triptolide crude product C.Be that the crude product C of 2g/mL admixes in macroporous adsorbent resin by concentration, loading quality and macroporous resin volume ratio are 1:10g/L, then be placed in chromatography column and carry out wash-out separation, collect elutriant stage by stage, detect triptolide content in elutriant, merge each and contain triptolide elutriant, rotary evaporation concentrates, crystallization, obtains triptolide sterling.
Wherein, the Subcritical water chromotagraphy device described in step (2) is TGYF-A type stainless steel high pressure extract device.Macroporous adsorbent resin described in step (4) is AB-8.
A kind of method utilizing Subcritical water chromotagraphy triptolide that the present invention proposes, the triptolide extraction yield obtained is 0.02 ‰.
Claims (4)
1. utilize a method for Subcritical water chromotagraphy triptolide, it is characterized in that the method specifically comprises the following steps:
(1) first trypterygine (root) pulverizer is pulverized, after 20 ~ 80 eye mesh screens, obtain Common Threewingnut Root;
(2) Common Threewingnut Root that a certain amount of step (1) obtains is taken in Subcritical water chromotagraphy device, Extracting temperature 100 ~ 150 DEG C, extraction time 30 ~ 90min, extract pressure 0.5 ~ 2.0MPa, solid-liquid ratio 1:10 ~ the 1:40 of Common Threewingnut Root and solvent, in solvent, ethanol contend per-cent 20 ~ 80%, obtains mixed liquor A;
(3) mixed liquor A is put into the centrifuge tube of whizzer, under rotating speed 4000 ~ 6000r/min after centrifugal 5 ~ 10min, take off centrifuge tube, obtain supernatant liquor B and sediment B;
(4) adopt rotary evaporation to be concentrated by supernatant liquor B, obtain triptolide crude product C;
Be that the crude product C of 0.25 ~ 2g/mL admixes in macroporous adsorbent resin by concentration, loading quality and macroporous resin volume ratio are 1:10 ~ 1:20g/L, then be placed in chromatography column and carry out wash-out separation, collect elutriant stage by stage, detect triptolide content in elutriant, merge each and contain triptolide elutriant, rotary evaporation concentrates, crystallization, obtains triptolide sterling.
2. a kind of method utilizing Subcritical water chromotagraphy triptolide according to claim 1, is characterized in that described Subcritical water chromotagraphy device is TGYF-A type stainless steel high pressure extract device.
3. a kind of method utilizing Subcritical water chromotagraphy triptolide according to claim 1, is characterized in that described macroporous adsorbent resin is any one in D101, D4020, AB-8.
4. a kind of method utilizing Subcritical water chromotagraphy triptolide according to claim 1, is characterized in that the triptolide extraction yield obtained is 0.02 ~ 0.06 ‰.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108129545A (en) * | 2018-02-06 | 2018-06-08 | 赖旭宇 | A kind of method for preparing triptolide |
| CN108929201A (en) * | 2018-08-20 | 2018-12-04 | 凤阳县小岗村永和营养保健品有限公司 | A kind of method that Subcritical Water Extraction technology extracts cannabidiol |
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| CN104861081A (en) * | 2015-06-02 | 2015-08-26 | 北京林业大学 | Method for extracting dendrobium polysaccharides through subcritical water |
| CN104876999A (en) * | 2015-06-02 | 2015-09-02 | 北京林业大学 | Method for extracting betulinic acid by subcritical water |
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- 2015-11-11 CN CN201510766447.4A patent/CN105198956A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104861081A (en) * | 2015-06-02 | 2015-08-26 | 北京林业大学 | Method for extracting dendrobium polysaccharides through subcritical water |
| CN104876999A (en) * | 2015-06-02 | 2015-09-02 | 北京林业大学 | Method for extracting betulinic acid by subcritical water |
Non-Patent Citations (1)
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| 韦玮等: "二萜类化合物的提取与纯化工艺研究进展", 《中国实验方剂学杂志》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108129545A (en) * | 2018-02-06 | 2018-06-08 | 赖旭宇 | A kind of method for preparing triptolide |
| CN108929201A (en) * | 2018-08-20 | 2018-12-04 | 凤阳县小岗村永和营养保健品有限公司 | A kind of method that Subcritical Water Extraction technology extracts cannabidiol |
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Application publication date: 20151230 |