CN106946836A - Process for extracting dracorhodin from Fibraurea recisa fruits - Google Patents
Process for extracting dracorhodin from Fibraurea recisa fruits Download PDFInfo
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- CN106946836A CN106946836A CN201710294522.0A CN201710294522A CN106946836A CN 106946836 A CN106946836 A CN 106946836A CN 201710294522 A CN201710294522 A CN 201710294522A CN 106946836 A CN106946836 A CN 106946836A
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- dracorhodin
- herba fibraureae
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D311/00—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings
- C07D311/02—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings ortho- or peri-condensed with carbocyclic rings or ring systems
- C07D311/04—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring
- C07D311/58—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4
- C07D311/60—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4 with aryl radicals attached in position 2
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Abstract
The invention discloses a method for extracting and purifying dracorhodin from Fibraurea recisa pierre fruits, which belongs to the technical field of extracting effective components from Fibraurea recisa pierre fruits, wherein the dracorhodin is prepared by the steps of crushing, primary decoloring, coarse crystallization, secondary decoloring, separation and purification by macroporous adsorption resin, concentration and crystallization, drying and the like. The extraction yield of the dracorhodin prepared by the method is more than 40.94 percent, the purity is more than 98.35 percent, and the purity meets the requirements of qualitative and quantitative reference substances.
Description
【Technical field】
The invention belongs to the technical field that herba fibraureae recisae fruit extracts effective ingredient, and in particular to one kind extracts dragon's blood from herba fibraureae recisae fruit
The technique of element.
【Background technology】
Dracorhodin is also known as dracorhodin, is one of important active component in herba fibraureae recisae fruit.According to the literature, dracorhodin
With antibacterial, antiviral isoreactivity.In recent years, the potential Anticancer Activities of dracorhodin are extensively concerned.Disclosed document is from Huang
The report of extraction purification dracorhodin is few in rattan fruit, and obtained dracorhodin purity is relatively low, does not reach as qualitative, quantitative pair
According to product requirement.
【The content of the invention】
The technique that dracorhodin is extracted in a kind of fruit from herba fibraureae recisae that the present invention is provided, to solve the extraction purification blood from herba fibraureae recisae fruit
Exhaust that plain purity is relatively low, the problem of not reaching as qualitative, quantitative reference substance requirement.
To solve above technical problem, the present invention uses following technical matters：
The technique that dracorhodin is extracted in a kind of fruit from herba fibraureae recisae, comprises the following steps：
S1：Herba fibraureae recisae fruit is crushed and sifted out, herba fibraureae recisae fruit powder end is made；
S2：Ethanol is added into herba fibraureae recisae fruit powder end made from step S1, the ultrasonic wave refluxing extraction 2-3 under water bath condition
Secondary, the frequency of each ultrasonic wave is 560-720W, and temperature is 42-50 DEG C, and the time is 12-15min, merges after extracting completely and extracts
Liquid, adjusts the pH value of extract solution to 4-4.3, temperature control is 42-50 DEG C, by decolorization and impurity removal by active carbon, and one is made after filtering
Secondary destainer；
S3：By a destainer concentrate drying made from step S2, extraction cream is made, extraction 5-6.2 times of body of cream is used in
50-55 DEG C long-pending of water is dissolved, and is carried out extraction 2-3 times using anhydrous ethyl acetate solvent, is continued to use anhydrous ethyl acetate
It is 1 to carry out solid-to-liquid ratio in 2-3 crystallization treatment, crystallization process:3.8-5 (W/V), is made crystal crude product；
S4：By ethanol dissolving of the coarse-grain made from step S3 through 70%-74%, the pH value of solution is adjusted to 4-4.3, temperature
Control as 42-50 DEG C, by decolorization and impurity removal by active carbon, secondary decolourization liquid is made after filtering；
S5：Secondary decolourization liquid made from step S4 is concentrated into 7%-19% containing dracorhodin in every milliliter, inhaled using macropore
The liquid of dracorhodin is made in attached resin separating-purifying, and condition is：The ethanol solution that agent is 50%-70% is parsed, its consumption is big
1.9-3.5 times of macroporous adsorbent resin volume, water wash zone is deionized water, and macroporous absorbent resin absorption regeneration solvent is 2.8%-
4.9% NaOH solution, adsorption zone flow velocity 8-10BV/h, desorption zone flow velocity 16-20BV/h, water wash zone flow velocity 22-26BV/h, then
Raw area flow velocity 6-9BV/h, switching time is 700-750s, and temperature is 43-50 DEG C, and pressure is 0.5-0.8MPa；
S6：Crystallized after dracorhodin liquid made from step S5 is concentrated, gained crystal is true in the case where temperature is 40-44 DEG C
Sky is dried, and dracorhodin is made.
Preferably, the mesh number of sieve described in step S1 is 30-60.
Preferably, the end of herba fibraureae recisae fruit powder described in step S2 and the weight ratio of ethanol are 1:6-8.
Preferably, the volume fraction of the ethanol is 68%-78%.
Preferably, it is 0.8-1.4h by the time of decolorization and impurity removal by active carbon described in step S2.
Preferably, it is 0.6-1.2h by the time of decolorization and impurity removal by active carbon described in step S4.
Preferably, macroporous absorbent resin described in step S5 is AD-8 type macroporous absorbent resins.
Preferably, concentration described in step S6 is vacuum-concentrcted.
Preferably, crystallization described in step S6 is carried out in the case where temperature is 4-8 DEG C.
Preferably, crystal described in step S6 is dried under vacuum to moisture content≤0.7% in the case where temperature is 40-42 DEG C.
The invention has the advantages that：
The extraction yield of dracorhodin made from the method for the present invention is more than 62.05 and purity is more than 98.34%, purity
Reach as qualitative, quantitative reference substance requirement.
【Embodiment】
For ease of more fully understanding the present invention, it is illustrated by following examples, these embodiments belong to the present invention's
Protection domain, but do not limit the scope of the invention.
In embodiment, the technique that dracorhodin is extracted in the fruit from herba fibraureae recisae comprises the following steps：
S1：Herba fibraureae recisae fruit is crushed and 30-60 mesh sieve is crossed, herba fibraureae recisae fruit powder end is made；
S2：6-8 times of 68%-78% of its weight ethanol is added into herba fibraureae recisae fruit powder end made from step S1, in water-bath bar
Ultrasonic wave refluxing extraction 2-3 times under part, the frequency of each ultrasonic wave is 560-720W, and temperature is 42-50 DEG C, and the time is 12-
15min, merges extract solution after extracting completely, adjusts the pH value of extract solution to 4-4.3, temperature control is 42-50 DEG C, passes through activity
Carbon decoloring removal of impurities 0.8-1.4h, is made a destainer after filtering；
S3：By a destainer concentrate drying made from step S2, extraction cream is made, extraction 5-6.2 times of body of cream is used in
50-55 DEG C long-pending of water is dissolved, and is carried out extraction 2-3 times using anhydrous ethyl acetate solvent, is continued to use anhydrous ethyl acetate
It is 1 to carry out solid-to-liquid ratio in 2-3 crystallization treatment, crystallization process:3.8-5 (W/V), is made crystal crude product；
S4：By ethanol dissolving of the coarse-grain made from step S3 through 70%-74%, the pH value of solution is adjusted to 4-4.3, temperature
Control as 42-50 DEG C, by decolorization and impurity removal by active carbon 0.6-1.2h, secondary decolourization liquid is made after filtering；
S5：Secondary decolourization liquid made from step S4 is concentrated into 7%-19% containing dracorhodin in every milliliter, using AD-8 types
The liquid of dracorhodin is made in macroporous absorbent resin separating-purifying, and condition is：The ethanol solution that agent is 50%-70% is parsed, it is used
Amount is 1.9-3.5 times of macroporous absorbent resin volume, and water wash zone is deionized water, and macroporous absorbent resin absorption regeneration solvent is
2.8%-4.9% NaOH solution, adsorption zone flow velocity 8-10BV/h, desorption zone flow velocity 16-20BV/h, water wash zone flow velocity 22-
26BV/h, renewing zone flow velocity 6-9BV/h, switching time are 700-750s, and temperature is 43-50 DEG C, and pressure is 0.5-0.8MPa；
S6：Dracorhodin liquid made from step S5 is carried out after vacuum-concentrcted, crystallized in the case where temperature is 4-8 DEG C, institute
Obtain crystal and be dried under vacuum to moisture content≤0.7% in the case where temperature is 40-42 DEG C, dracorhodin is made.
Embodiment 1
The technique that dracorhodin is extracted in a kind of fruit from herba fibraureae recisae, comprises the following steps：
S1：Herba fibraureae recisae fruit is crushed and 50 mesh sieve are crossed, herba fibraureae recisae fruit powder end is made；
S2：The ethanol of 7 times 72% of its weight is added into herba fibraureae recisae fruit powder end made from step S1, it is ultrasonic under water bath condition
Ripple refluxing extraction 2 times, the frequency of each ultrasonic wave is 620W, and temperature is 46 DEG C, and the time is 14min, merges after extracting completely and carries
Liquid is taken, the pH value of extract solution is adjusted to 4.2, temperature control is 46 DEG C, by decolorization and impurity removal by active carbon 1.2h, and one is made after filtering
Secondary destainer；
S3：By a destainer concentrate drying made from step S2, extraction cream is made, extraction 5.6 times of volumes of cream are used in
52 DEG C of water dissolved, using anhydrous ethyl acetate solvent carry out extraction 2 times, continuation is carried out 2 times with anhydrous ethyl acetate
Solid-to-liquid ratio is 1 in crystallization treatment, crystallization process:4.5 (W/V), are made crystal crude product；
S4：By ethanol dissolving of the coarse-grain made from step S3 through 70%-74%, the pH value of solution is adjusted to 4.2, temperature control
46 DEG C are made as, by decolorization and impurity removal by active carbon 0.9h, secondary decolourization liquid is made after filtering；
S5：Secondary decolourization liquid made from step S4 is concentrated into every milliliter and contains dracorhodin 12%, using AD-8 type macropores
The liquid of dracorhodin is made in polymeric adsorbent separating-purifying, and condition is：The ethanol solution that agent is 62% is parsed, its consumption is that macropore is inhaled
2.6 times of attached resin volume, water wash zone is deionized water, and macroporous absorbent resin absorption regeneration solvent is 4% NaOH solution, is inhaled
Attached area's flow velocity 9BV/h, desorption zone flow velocity 18BV/h, water wash zone flow velocity 24BV/h, renewing zone flow velocity 8BV/h, switching time is
730s, temperature is 47 DEG C, and pressure is 0.7MPa；
S6：Dracorhodin liquid made from step S5 is carried out after vacuum-concentrcted, crystallized in the case where temperature is 6 DEG C, gained
Crystal is that to be dried under vacuum to moisture content at 41 DEG C be 0.7% in temperature, and dracorhodin is made.
Embodiment 2
The technique that dracorhodin is extracted in a kind of fruit from herba fibraureae recisae, comprises the following steps：
S1：Herba fibraureae recisae fruit is crushed and 30 mesh sieve are crossed, herba fibraureae recisae fruit powder end is made；
S2：The ethanol of 6 times 68% of its weight is added into herba fibraureae recisae fruit powder end made from step S1, it is ultrasonic under water bath condition
Ripple refluxing extraction 2 times, the frequency of each ultrasonic wave is 560W, and temperature is 42 DEG C, and the time is 15min, merges after extracting completely and carries
Liquid is taken, the pH value of extract solution is adjusted to 4, temperature control is 42 DEG C, by decolorization and impurity removal by active carbon 1.4h, is made once after filtering
Destainer；
S3：By a destainer concentrate drying made from step S2, extraction cream is made, extraction 5 times of volumes of cream are used in
50 DEG C of water is dissolved, and extraction 2 times is carried out using anhydrous ethyl acetate solvent, and continuation carries out 2 knots with anhydrous ethyl acetate
Solid-to-liquid ratio is 1 in crystalline substance processing, crystallization process:3.8 (W/V), are made crystal crude product；
S4：Coarse-grain made from step S3 is dissolved through 70% ethanol, the pH value of solution is adjusted to 4, temperature control is 43
DEG C, by decolorization and impurity removal by active carbon 1.2h, secondary decolourization liquid is made after filtering；
S5：Secondary decolourization liquid made from step S4 is concentrated into every milliliter and contains dracorhodin 7%, is inhaled using AD-8 types macropore
The liquid of dracorhodin is made in attached resin separating-purifying, and condition is：The ethanol solution that agent is 50%-70% is parsed, its consumption is big
2 times of macroporous adsorbent resin volume, water wash zone is deionized water, and macroporous absorbent resin absorption regeneration solvent is molten for 2.8% NaOH
Liquid, adsorption zone flow velocity 8BV/h, desorption zone flow velocity 16BV/h, water wash zone flow velocity 22BV/h, renewing zone flow velocity 6BV/h, switching time
For 700s, temperature is 43 DEG C, and pressure is 0.5MPa；
S6：Dracorhodin liquid made from step S5 is carried out after vacuum-concentrcted, crystallized in the case where temperature is 4 DEG C, gained
Crystal is that to be dried under vacuum to moisture content at 40 DEG C be 0.6% in temperature, and dracorhodin is made.
Embodiment 3
The technique that dracorhodin is extracted in a kind of fruit from herba fibraureae recisae, comprises the following steps：
S1：Herba fibraureae recisae fruit is crushed and 60 mesh sieve are crossed, herba fibraureae recisae fruit powder end is made；
S2：The ethanol of 8 times 78% of its weight is added into herba fibraureae recisae fruit powder end made from step S1, it is ultrasonic under water bath condition
Ripple refluxing extraction 3 times, the frequency of each ultrasonic wave is 720W, and temperature is 50 DEG C, and the time is 12min, merges after extracting completely and carries
Liquid is taken, the pH value of extract solution is adjusted to 4.3, temperature control is 50 DEG C, by decolorization and impurity removal by active carbon 0.8h, and one is made after filtering
Secondary destainer；
S3：By a destainer concentrate drying made from step S2, extraction cream is made, extraction 6.2 times of volumes of cream are used in
55 DEG C of water dissolved, using anhydrous ethyl acetate solvent carry out extraction 3 times, continuation is carried out 3 times with anhydrous ethyl acetate
Solid-to-liquid ratio is 1 in crystallization treatment, crystallization process:5 (W/V), are made crystal crude product；
S4：Coarse-grain made from step S3 is dissolved through 74% ethanol, the pH value of solution is adjusted to 4.3, temperature control is
50 DEG C, by decolorization and impurity removal by active carbon 0.6h, secondary decolourization liquid is made after filtering；
S5：Secondary decolourization liquid made from step S4 is concentrated into every milliliter and contains dracorhodin 19%, using AD-8 type macropores
The liquid of dracorhodin is made in polymeric adsorbent separating-purifying, and condition is：The ethanol solution that agent is 70% is parsed, its consumption is that macropore is inhaled
3.5 times of attached resin volume, water wash zone is deionized water, and macroporous absorbent resin absorption regeneration solvent is molten for -4.9% NaOH
Liquid, adsorption zone flow velocity 10BV/h, desorption zone flow velocity 20BV/h, water wash zone flow velocity 26BV/h, renewing zone flow velocity 9BV/h, during switching
Between be 750s, temperature be 50 DEG C, pressure is 0.8MPa；
S6：Dracorhodin liquid made from step S5 is carried out after vacuum-concentrcted, crystallized in the case where temperature is 8 DEG C, gained
Crystal is that to be dried under vacuum to moisture content at 42 DEG C be 0.5% in temperature, and dracorhodin is made.
Extraction yield and purity to dracorhodin made from embodiment 1-3 are detected, as a result as shown in the table.
| Experimental project | Extract yield (%) | Purity (%) |
| Embodiment 1 | 45.68 | 98.35 |
| Embodiment 2 | 40.94 | 98.76 |
| Embodiment 3 | 43.11 | 98.91 |
From with upper table, the extraction yield of dracorhodin made from the method for the present invention exists more than 40.94 with purity
More than 98.35%, purity has been reached as qualitative, quantitative reference substance requirement.
Above content is to combine specific preferred embodiment further description made for the present invention, it is impossible to assert
The specific implementation of the present invention is confined to these explanations, for person of an ordinary skill in the technical field, is not departing from
On the premise of present inventive concept, some simple deduction or replace can also be made, the present invention should be all considered as belonging to by being submitted
Claims determine scope of patent protection.
Claims (10)
1. the technique of dracorhodin is extracted in a kind of fruit from herba fibraureae recisae, it is characterised in that comprise the following steps：
S1：Herba fibraureae recisae fruit is crushed and sifted out, herba fibraureae recisae fruit powder end is made；
S2：Ethanol is added into herba fibraureae recisae fruit powder end made from step S1, ultrasonic wave refluxing extraction 2-3 times under water bath condition, often
The frequency of secondary ultrasonic wave is 560-720W, and temperature is 42-50 DEG C, and the time is 12-15min, merges extract solution after extracting completely, adjusts
The pH value of extract solution is saved to 4-4.3, temperature control is 42-50 DEG C, by decolorization and impurity removal by active carbon, is made and once decolourizes after filtering
Liquid；
S3：By a destainer concentrate drying made from step S2, extraction cream is made, extraction 5-6.2 times of volume of cream is used in
50-55 DEG C of water is dissolved, and carries out extraction 2-3 times using anhydrous ethyl acetate solvent, continuation is carried out with anhydrous ethyl acetate
Solid-to-liquid ratio is 1 in 2-3 crystallization treatment, crystallization process:3.8-5 (W/V), is made crystal crude product；
S4：By ethanol dissolving of the coarse-grain made from step S3 through 70%-74%, the pH value of solution is adjusted to 4-4.3, temperature control
For 42-50 DEG C, by decolorization and impurity removal by active carbon, secondary decolourization liquid is made after filtering；
S5：Secondary decolourization liquid made from step S4 is concentrated into 7%-19% containing dracorhodin in every milliliter, using macroporous absorption tree
The liquid of dracorhodin is made in fat separating-purifying, and condition is：The ethanol solution that agent is 50%-70% is parsed, its consumption is that macropore is inhaled
1.9-3.5 times of attached resin volume, water wash zone is deionized water, and macroporous absorbent resin absorption regeneration solvent is 2.8%-4.9%
NaOH solution, adsorption zone flow velocity 8-10BV/h, desorption zone flow velocity 16-20BV/h, water wash zone flow velocity 22-26BV/h, renewing zone
Flow velocity 6-9BV/h, switching time is 700-750s, and temperature is 43-50 DEG C, and pressure is 0.5-0.8MPa；
S6：Crystallized after dracorhodin liquid made from step S5 is concentrated, gained crystal vacuum in the case where temperature is 40-44 DEG C is done
It is dry, dracorhodin is made.
2. the technique of dracorhodin is extracted in the fruit according to claim 1 from herba fibraureae recisae, it is characterised in that：Sieved described in step S1
The mesh number of son is 30-60.
3. the technique of dracorhodin is extracted in the fruit according to claim 1 from herba fibraureae recisae, it is characterised in that：It is yellow described in step S2
Rattan fruit powder end is 1 with the weight ratio of ethanol:6-8.
4. the technique of dracorhodin is extracted in the fruit according to claim 3 from herba fibraureae recisae, it is characterised in that：The volume of the ethanol
Fraction is 68%-78%.
5. the technique of dracorhodin is extracted in the fruit according to claim 1 from herba fibraureae recisae, it is characterised in that：Lead to described in step S2
The time for crossing decolorization and impurity removal by active carbon is 0.8-1.4h.
6. the technique of dracorhodin is extracted in the fruit according to claim 1 from herba fibraureae recisae, it is characterised in that：Lead to described in step S4
The time for crossing decolorization and impurity removal by active carbon is 0.6-1.2h.
7. the technique of dracorhodin is extracted in the fruit according to claim 1 from herba fibraureae recisae, it is characterised in that：It is big described in step S5
Macroporous adsorbent resin is AD-8 type macroporous absorbent resins.
8. the technique of dracorhodin is extracted in the fruit according to claim 1 from herba fibraureae recisae, it is characterised in that：It is dense described in step S6
It is condensed to vacuum-concentrcted.
9. the technique of dracorhodin is extracted in the fruit according to claim 1 from herba fibraureae recisae, it is characterised in that：Tied described in step S6
Crystalline substance is carried out in the case where temperature is 4-8 DEG C.
10. the technique of dracorhodin is extracted in the fruit according to claim 1 from herba fibraureae recisae, it is characterised in that：Described in step S6
Crystal is dried under vacuum to moisture content≤0.7% in the case where temperature is 40-42 DEG C.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107266308A (en) * | 2017-07-20 | 2017-10-20 | 广西南宁桂知科技有限公司 | The technique that a kind of utilization longan pericarp prepares protocatechuic acid |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5063244A (en) * | 1990-07-30 | 1991-11-05 | Development Center For Biotechnology | Process for the isolation of antifungal agents (5-methoxy-7-hydroxyflavan) from dragon's blood resin and its use in agriculture |
-
2017
- 2017-04-28 CN CN201710294522.0A patent/CN106946836B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5063244A (en) * | 1990-07-30 | 1991-11-05 | Development Center For Biotechnology | Process for the isolation of antifungal agents (5-methoxy-7-hydroxyflavan) from dragon's blood resin and its use in agriculture |
Non-Patent Citations (3)
| Title |
|---|
| 尹光天等: "黄藤果实血竭成分的提取和鉴别", 《中南林学院学报》 * |
| 梁伟玲等: "正交试验优化麒麟血竭中血竭素的超声提取工艺", 《中国生化药物杂志》 * |
| 郑道君等: "中国血竭基源植物的研究与利用", 《中国野生植物资源》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107266308A (en) * | 2017-07-20 | 2017-10-20 | 广西南宁桂知科技有限公司 | The technique that a kind of utilization longan pericarp prepares protocatechuic acid |
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Effective date of registration: 20190820 Address after: 530199 Room 202, Building 1, Fengqi Oriental Building, Xiangshan Avenue, Wuming County, Nanning City, Guangxi Zhuang Autonomous Region Applicant after: Wuming Xin Yi Rong Niu vigorously Chinese herbal medicine planting professional cooperatives Address before: 530100 No. 22, Dingluo District, Biaoying Community, Wuming County, Nanning City, Guangxi Zhuang Autonomous Region Applicant before: Nanning Xin Rong Rong Biological Technology Co., Ltd. |
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Effective date of registration: 20210909 Address after: 530100 No. 22, District D, dingluo District, biaoying community, Wuming District, Nanning City, Guangxi Zhuang Autonomous Region Patentee after: Nanning Chengtai Biotechnology Co.,Ltd. Address before: 530199 Room 202, unit 1, building 1, Fengqi Dongfang, Xiangshan Avenue, Wuming County, Nanning City, Guangxi Zhuang Autonomous Region Patentee before: WUMING XINYI RONGNIU DALI TRADITIONAL HERBAL MEDICINE PLANTING PROFESSIONAL COOPERATIVE |