CN1951451A - Method for supercritical extraction of active ingredient of camellia - Google Patents
Method for supercritical extraction of active ingredient of camellia Download PDFInfo
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- CN1951451A CN1951451A CNA2006101225760A CN200610122576A CN1951451A CN 1951451 A CN1951451 A CN 1951451A CN A2006101225760 A CNA2006101225760 A CN A2006101225760A CN 200610122576 A CN200610122576 A CN 200610122576A CN 1951451 A CN1951451 A CN 1951451A
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- flos camelliae
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Abstract
The invention relates to a method for extracting the active components of camellia, which comprises that putting the dry camellia into extracting kettle; processing the CO2 gas into ultra-critical CO2 fluid, heating and pressurizing the connected extracting kettle, analysis kettle and separating post; circulated extracting, adding some clamping agent, adjusting the flux of CO2 fluid and controlling the time, keeping constant temperature and constant pressure; obtaining the active rough product from the outlet of analysis kettle. The invention has low temperature, without solvent to keep the active components most.
Description
Technical field
The present invention relates to Flos Camelliae Japonicae extraction of active ingredients technology, particularly a kind of supercritical fluid extraction separates the extraction process of the effective active composition in the Flos Camelliae Japonicae, belongs to the technical field of chemistry and chemical engineering of Chinese herbal medicine preparation.
Background technology
Flos Camelliae Japonicae active matter composition has excellent clearing away heat to stop bleeding function, be widely used in medical science in, disease treatments such as surgery, utilize the drug effect of Flos Camelliae Japonicae active matter composition to be applied to the oral cavity health nursing field and have positive effect, and being water, the extracting method of traditional Flos Camelliae Japonicae active matter composition carries or ethanol is carried crystallization process, these two kinds of methods all need to carry out the high temperature high cooking, therefore it is darker to exist impurity content polychrome pool in the Flos Camelliae Japonicae extract with above-mentioned technology extraction, low and the low problem of extraction ratio of active component content, the refining purification that both had been unfavorable for subsequent handling, and the composition of each batch extract is also uncertain, and also there is following shortcoming in this method: operation is many, the technology very complicated, required time is longer; And,, make finished color deepen poor stability when making active component decomposition, hydrolysis or oxidation deterioration easily with after adding in the toothpaste because these methods need repeatedly steaming and decocting or distillation, and heat time heating time is long; Active constituent content and extraction ratio are all lower.And might use some and have toxic solvent, environment is polluted.
Summary of the invention
The objective of the invention is existence at the problems referred to above, provide a kind of not only can effectively improve the purity and the extraction ratio of Flos Camelliae Japonicae activity extract and guarantee the active matter composition stable, but also can guarantee that it is with short production cycle, the method for the supercritical extraction Flos Camelliae Japonicae active component of easy reliable, the labor savings of technology.
The objective of the invention is to be achieved through the following technical solutions:
A kind of method of supercritical extraction Flos Camelliae Japonicae active component may further comprise the steps:
(1), the dry thing of will Flos Camelliae Japonicae is put in the extraction kettle;
(2), with CO
2The gas pressurized treatments of heating in storage tank makes it become supercritical CO
2Fluid, the temperature of handling of wherein heating is 30 ℃～32 ℃, the pressure of pressurized treatments is 7.0～7.2Mpa;
(3), respectively to processings of heating of the extraction kettle, extraction-container, the detached dowel that connect in regular turn, the temperature of the processing of wherein heating in each device is respectively extraction kettle: 35 ℃～60 ℃, extraction-container: 40 ℃～60 ℃;
(4), open storage tank and by high-pressure pump described supercritical CO 2 fluid joined respectively and carry out pressurized treatments in extraction kettle, extraction-container, the detached dowel, wherein the pressure of pressurized treatments is respectively extraction kettle in each device: 18～35Mpa, extraction-container: 3～14Mpa, detached dowel: 18～22Mpa;
(5), the beginning cycling extraction, and add an amount of entrainer, regulate supercritical CO
2Fluid each the device in flow and control cycling extraction time and make each the device in keep constant temperature and pressure, wherein each the device in supercritical CO
2Flow rate of fluid is: 12～20kg/h, and the time of described cycling extraction this moment is 60～180 minutes;
(6), when reaching selected cycling extraction after the time, from the discharging opening of extraction-container, obtain Flos Camelliae Japonicae active matter crude product.
Wherein for guaranteeing that further the present invention can directly obtain supercritical CO efficiently
2The crystallized product of extraction, thus common supercritical CO effectively solved
2Extract needs to carry out its active matter crude product numerous and diverse and the existing problem of the refining drying and other steps acquisition crystallized product of the centrifugal washing again of sucking filtration poor efficiency, said method also is included in device one crystallization kettle that is connected with the extraction-container discharging opening behind the extraction-container, and above-mentioned Flos Camelliae Japonicae active matter crude product enters into this crystallization kettle from the discharging opening of extraction-container carries out crystallization treatment and obtain Flos Camelliae Japonicae active matter crystalline solid.Crystallization treatment in the above-mentioned crystallization kettle is the Flos Camelliae Japonicae active matter crude product in this crystallization kettle to be carried out cooling decompression handle at this moment, and wherein the temperature in this crystallization kettle is 25 ℃～40 ℃, and the pressure of its reduced pressure treatment is 0.1Mpa～6Mpa.
The present invention is owing to adopt supercritical CO
2Abstraction technique extracts the method for the active component of Flos Camelliae Japonicae, makes full use of supercritical CO
2The temperature that extraction and separation technology had is low, without solvent, can separate and keep the characteristics of raw material active ingredient to greatest extent, supercritical carbon dioxide extraction method is used for the extraction of Flos Camelliae Japonicae, solve the defective of traditional Flos Camelliae Japonicae active matter extractive technique well, obtained the crystalline solid of the white and Flos Camelliae Japonicae active matter that composition is clear and definite of lighter color.The composition that had both fully guaranteed extract is determined, purity is high, the constant product quality of each batch.And when being applied to described extract in the toothpaste, can easily and reliably make Flos Camelliae Japonicae active matter content height, pure white, the clearing away heat to stop bleeding effect good health care toothpaste of color.
Describe realization of the present invention in detail below in conjunction with embodiment:
The specific embodiment
The method of supercritical extraction Flos Camelliae Japonicae active component of the present invention may further comprise the steps:
(1), the dry thing of the Flos Camelliae Japonicae behind the cool drying is put in the extraction kettle;
(2), with CO
2The gas pressurized treatments of heating in storage tank makes it become supercritical CO
2Fluid, the temperature of handling of wherein heating is 30 ℃～32 ℃, the pressure of pressurized treatments is 7.0～7.2Mpa;
(3), respectively to processings of heating of the extraction kettle, extraction-container, the detached dowel that connect in regular turn, the temperature of the processing of wherein heating in each device is respectively extraction kettle: 35 ℃～60 ℃, extraction-container: 40 ℃～60 ℃;
(4), open storage tank by high-pressure pump with described supercritical CO
2Fluid joins respectively and carries out pressurized treatments in extraction kettle, extraction-container, the detached dowel, and wherein the pressure of pressurized treatments is respectively extraction kettle in each device: 18～35Mpa, extraction-container: 3～14Mpa, detached dowel: 18～22Mpa;
(5), the beginning cycling extraction, and add an amount of entrainer, regulate the supercritical CO 2 fluid in each device flow and time of control cycling extraction and make in each device and keep constant temperature and pressure, the supercritical CO in each device wherein
2Flow rate of fluid is: 12～20kg/h, and the time of described cycling extraction this moment is 60～180 minutes;
(6), when reaching selected cycling extraction after the time, from the discharging opening of extraction-container, obtain Flos Camelliae Japonicae active matter crude product.
Wherein for guaranteeing that further the present invention can directly obtain supercritical CO efficiently
2The crystallized product of extraction, thus common supercritical CO effectively solved
2Extract needs to carry out its active matter crude product numerous and diverse and the existing problem of the refining drying and other steps acquisition crystallized product of the centrifugal washing again of sucking filtration poor efficiency, said method also is included in device one crystallization kettle that is connected with the extraction-container discharging opening behind the extraction-container, and above-mentioned Flos Camelliae Japonicae active matter crude product enters into this crystallization kettle from the discharging opening of extraction-container carries out crystallization treatment and obtain Flos Camelliae Japonicae active matter crystalline solid.The structure of the crystallization kettle described in the present invention is formed at extracting crystallized product and is designed, and is provided with multilayer insulating panel in it, and each wall and plate face are coarse, for the crystallization of active matter provides advantage, with the convenient crystallized product that obtains expeditiously.Crystallization treatment in the crystallization kettle is the Flos Camelliae Japonicae active matter crude product in this crystallization kettle to be carried out cooling decompression handle at this moment, and wherein the temperature that cooling is handled in this crystallization kettle is 25 ℃～40 ℃, and the pressure of its reduced pressure treatment is 0.1Mpa～6Mpa.
Embodiment 1: a kind of method of supercritical extraction Flos Camelliae Japonicae active component may further comprise the steps:
(1), the dry thing of Flos Camelliae Japonicae is put in the extraction kettle;
(2), with CO
2The gas pressurized treatments of heating in storage tank makes it become supercritical CO
2Fluid, the temperature of handling of wherein heating is 30 ℃, the pressure of pressurized treatments is 7.2Mpa;
(3), respectively to processings of heating of the extraction kettle, extraction-container, the detached dowel that connect in regular turn, the temperature of the processing of wherein heating in each device is respectively extraction kettle: 60 ℃, extraction-container: 50 ℃;
(4), open storage tank by high-pressure pump with described supercritical CO
2Fluid joins respectively and carries out pressurized treatments in extraction kettle, extraction-container, the detached dowel, and wherein the pressure of pressurized treatments is respectively extraction kettle in each device: 32Mpa, extraction-container: 12Mpa, detached dowel: 21Mpa;
(5), the beginning cycling extraction, and add an amount of entrainer (it is 50～90% alcoholic solution that described entrainer adopts concentration), regulate supercritical CO
2Fluid each the device in flow and control cycling extraction time and make each the device in keep constant temperature and pressure, wherein each the device in supercritical CO
2Flow rate of fluid is: 18kg/h, and the time of described cycling extraction this moment is 60 minutes;
(6), when reaching selected cycling extraction after the time, from the discharging opening of extraction-container, obtain Flos Camelliae Japonicae active matter crude product,
(7), the Flos Camelliae Japonicae active matter crude product in the crystallization kettle carried out cooling decompression handle, wherein the temperature in the crystallization kettle is 30 ℃, its pressure is 2Mpa.
Embodiment 2: a kind of method of supercritical extraction Flos Camelliae Japonicae active component may further comprise the steps:
(1), the dry thing of Flos Camelliae Japonicae is put in the extraction kettle;
(2), with CO
2The gas pressurized treatments of heating in storage tank makes it become supercritical CO
2Fluid, the temperature of handling of wherein heating is 32 ℃, the pressure of pressurized treatments is 7.1Mpa;
(3), respectively to processings of heating of the extraction kettle, extraction-container, the detached dowel that connect in regular turn, the temperature of the processing of wherein heating in each device is respectively extraction kettle: 40 ℃, extraction-container: 60 ℃;
(4), open storage tank by high-pressure pump with described supercritical CO
2Fluid joins respectively and carries out pressurized treatments in extraction kettle, extraction-container, the detached dowel, and wherein the pressure of pressurized treatments is respectively extraction kettle in each device: 18Mpa, extraction-container: 14Mpa, detached dowel: 18Mpa;
(5), the beginning cycling extraction, and add an amount of entrainer (it is 50～90% alcoholic solution that described entrainer adopts concentration), regulate supercritical CO
2Fluid each the device in flow and control cycling extraction time and make each the device in keep constant temperature and pressure, wherein each the device in supercritical CO
2Flow rate of fluid is: 20kg/h, and the time of described cycling extraction this moment is 180 minutes;
(6), when reaching selected cycling extraction after the time, from the discharging opening of extraction-container, obtain Flos Camelliae Japonicae active matter crude product;
(7), the Flos Camelliae Japonicae active matter crude product in the crystallization kettle carried out cooling decompression handle, wherein the temperature in the crystallization kettle is 40 ℃, its pressure is 6Mpa.
Embodiment 3: a kind of method of supercritical extraction Flos Camelliae Japonicae active component may further comprise the steps:
(1), the dry thing of Flos Camelliae Japonicae is put in the extraction kettle;
(2), with CO
2The gas pressurized treatments of heating in storage tank makes it become supercritical CO
2Fluid, the temperature of handling of wherein heating is 31 ℃, the pressure of pressurized treatments is, 7.2Mpa;
(3), respectively to processings of heating of the extraction kettle, extraction-container, the detached dowel that connect in regular turn, the temperature of the processing of wherein heating in each device is respectively extraction kettle: 50 ℃, extraction-container: 45 ℃;
(4), open storage tank by high-pressure pump with described supercritical CO
2Fluid joins respectively and carries out pressurized treatments in extraction kettle, extraction-container, the detached dowel, and wherein the pressure of pressurized treatments is respectively extraction kettle in each device: 35Mpa, extraction-container: 3Mpa, detached dowel: 19Mpa;
(5), the beginning cycling extraction, and add an amount of entrainer (it is 50～90% alcoholic solution that described entrainer adopts concentration), regulate supercritical CO
2Fluid each the device in flow and control cycling extraction time and make each the device in keep constant temperature and pressure, wherein each the device in supercritical CO
2Flow rate of fluid is: 15kg/h, and the time of described cycling extraction this moment is 120 minutes;
(6), when reaching selected cycling extraction after the time, from the discharging opening of extraction-container, obtain Flos Camelliae Japonicae active matter crude product;
(7), the Flos Camelliae Japonicae active matter crude product in the crystallization kettle carried out cooling decompression handle, wherein the temperature in the crystallization kettle is 25 ℃, its pressure is 0.1Mpa.
Embodiment 4: a kind of method of supercritical extraction Flos Camelliae Japonicae active component may further comprise the steps:
(1), the dry thing of Flos Camelliae Japonicae is put in the extraction kettle;
(2), with CO
2The gas pressurized treatments of heating in storage tank makes it become supercritical CO
2Fluid, the temperature of handling of wherein heating is 30 ℃, the pressure of pressurized treatments is 7.2Mpa;
(3), respectively to processings of heating of the extraction kettle, extraction-container, the detached dowel that connect in regular turn, the temperature of the processing of wherein heating in each device is respectively extraction kettle: 35 ℃, extraction-container: 40 ℃;
(4), open storage tank by high-pressure pump with described supercritical CO
2Fluid joins respectively and carries out pressurized treatments in extraction kettle, extraction-container, the detached dowel, and wherein the pressure of pressurized treatments is respectively extraction kettle in each device: 29Mpa, extraction-container: 10Mpa, detached dowel: 21Mpa;
(5), the beginning cycling extraction, and add an amount of entrainer (it is 50～90% alcoholic solution that described entrainer adopts concentration), regulate supercritical CO
2Fluid each the device in flow and control cycling extraction time and make each the device in keep constant temperature and pressure, wherein each the device in supercritical CO
2Flow rate of fluid is: 12kg/h, and the time of described cycling extraction this moment is 100 minutes;
(6), when reaching selected cycling extraction after the time, from the discharging opening of extraction-container, obtain Flos Camelliae Japonicae active matter crude product;
(7), the Flos Camelliae Japonicae active matter crude product in the crystallization kettle carried out cooling decompression handle, wherein the temperature in the crystallization kettle is 36 ℃, its pressure is 4Mpa.
Embodiment 5: a kind of method of supercritical extraction Flos Camelliae Japonicae active component may further comprise the steps:
(1), the dry thing of Flos Camelliae Japonicae is put in the extraction kettle;
(2), with CO
2The gas pressurized treatments of heating in storage tank makes it become supercritical CO
2Fluid, the temperature of handling of wherein heating is 32 ℃, the pressure of pressurized treatments is 7.0Mpa;
(3), respectively to processings of heating of the extraction kettle, extraction-container, the detached dowel that connect in regular turn, the temperature of the processing of wherein heating in each device is respectively extraction kettle: 56 ℃, extraction-container: 54 ℃;
(4), open storage tank by high-pressure pump with described supercritical CO
2Fluid joins respectively and carries out pressurized treatments in extraction kettle, extraction-container, the detached dowel, and wherein the pressure of pressurized treatments is respectively extraction kettle in each device: 29Mpa, extraction-container: 6Mpa, detached dowel: 22Mpa;
(5), the beginning cycling extraction, and add an amount of entrainer (it is 50～90% alcoholic solution that described entrainer adopts concentration), regulate supercritical CO
2Fluid each the device in flow and control cycling extraction time and make each the device in keep constant temperature and pressure, wherein each the device in supercritical CO
2Flow rate of fluid is: 12kg/h, and the time of described cycling extraction this moment is 90 minutes;
(6), when reaching selected cycling extraction after the time, from the discharging opening of extraction-container, obtain Flos Camelliae Japonicae active matter crude product;
(7), the Flos Camelliae Japonicae active matter crude product in the crystallization kettle carried out cooling decompression handle, wherein the temperature in the crystallization kettle is 32 ℃, its pressure is 5Mpa.
Claims (3)
1, a kind of method of supercritical extraction Flos Camelliae Japonicae active component is characterized in that said method comprising the steps of:
(1), the dry thing of Flos Camelliae Japonicae is put in the extraction kettle;
(2), with CO
2The gas pressurized treatments of heating in storage tank makes it become supercritical CO
2Fluid, the temperature of handling of wherein heating is 30 ℃～32 ℃, the pressure of pressurized treatments is 7.0～7.2Mpa;
(3), respectively to processings of heating of the extraction kettle, extraction-container, the detached dowel that connect in regular turn, the temperature of the processing of wherein heating in each device is respectively extraction kettle: 35 ℃～60 ℃, extraction-container: 40 ℃～60 ℃;
(4), open storage tank by high-pressure pump with described supercritical CO
2Fluid joins respectively and carries out pressurized treatments in extraction kettle, extraction-container, the detached dowel, and wherein the pressure of pressurized treatments is respectively extraction kettle in each device: 18～35Mpa, extraction-container: 3～14Mpa, detached dowel: 18～22Mpa;
(5), the beginning cycling extraction, and add an amount of entrainer, regulate supercritical CO
2Fluid each the device in flow and control cycling extraction time and make each the device in keep constant temperature and pressure, wherein each the device in supercritical CO
2Flow rate of fluid is: 12～20kg/h, and the time of described cycling extraction this moment is 60～180 minutes;
(6), when reaching selected cycling extraction after the time, from the discharging opening of extraction-container, obtain Flos Camelliae Japonicae active matter crude product.
2, according to the method for the described supercritical extraction Flos Camelliae Japonicae of claim 1 active component, it is characterized in that said method also is included in device one crystallization kettle that is connected with the extraction-container discharging opening behind the extraction-container, above-mentioned Flos Camelliae Japonicae active matter crude product enters into this crystallization kettle from the discharging opening of extraction-container carries out crystallization treatment and obtains Flos Camelliae Japonicae active matter crystalline solid.
3, the method for supercritical extraction Flos Camelliae Japonicae active component according to claim 2, it is characterized in that the crystallization treatment in the above-mentioned crystallization kettle is the Flos Camelliae Japonicae active matter crude product in this crystallization kettle to be carried out cooling decompression handle, wherein the temperature in this crystallization kettle is 25 ℃～40 ℃, and its pressure is 0.1Mpa～6Mpa.
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| CNA2006101225760A CN1951451A (en) | 2006-09-30 | 2006-09-30 | Method for supercritical extraction of active ingredient of camellia |
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| CNA2006101225760A CN1951451A (en) | 2006-09-30 | 2006-09-30 | Method for supercritical extraction of active ingredient of camellia |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101928643A (en) * | 2010-09-03 | 2010-12-29 | 河南工业大学 | Preparation method for compound with flavor of Xinyang maojian tea |
| CN103705647A (en) * | 2014-01-02 | 2014-04-09 | 青岛农业大学 | Process method for extracting general flavone of golden camellia leaves by CO2 supercritical method |
| CN106727024A (en) * | 2017-01-13 | 2017-05-31 | 华南理工大学 | A kind of oil tea gargle and preparation method thereof |
| CN107568362A (en) * | 2017-09-25 | 2018-01-12 | 广西金秀县圣昌生态种植专业合作社 | A kind of preparation method of wild black tea |
| CN107823008A (en) * | 2017-12-12 | 2018-03-23 | 国妆汉美（广州）化妆品有限公司 | A kind of essence additive extracted from natural plants and preparation method thereof |
-
2006
- 2006-09-30 CN CNA2006101225760A patent/CN1951451A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101928643A (en) * | 2010-09-03 | 2010-12-29 | 河南工业大学 | Preparation method for compound with flavor of Xinyang maojian tea |
| CN101928643B (en) * | 2010-09-03 | 2012-10-03 | 河南工业大学 | Preparation method for compound with flavor of Xinyang maojian tea |
| CN103705647A (en) * | 2014-01-02 | 2014-04-09 | 青岛农业大学 | Process method for extracting general flavone of golden camellia leaves by CO2 supercritical method |
| CN103705647B (en) * | 2014-01-02 | 2016-08-24 | 青岛农业大学 | A kind of CO2the process of supercritical methanol technology extracting gold jasmine tea leaf flavonoids |
| CN106727024A (en) * | 2017-01-13 | 2017-05-31 | 华南理工大学 | A kind of oil tea gargle and preparation method thereof |
| CN107568362A (en) * | 2017-09-25 | 2018-01-12 | 广西金秀县圣昌生态种植专业合作社 | A kind of preparation method of wild black tea |
| CN107823008A (en) * | 2017-12-12 | 2018-03-23 | 国妆汉美（广州）化妆品有限公司 | A kind of essence additive extracted from natural plants and preparation method thereof |
| CN107823008B (en) * | 2017-12-12 | 2021-06-11 | 无锡容颜美医学科技有限公司 | Essence additive extracted from natural plant and preparation method thereof |
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Open date: 20070425 |