CN105878323A - Method using ultrasonically-assisted supercritical extraction rectification to purify cynarin in globe artichoke - Google Patents

Method using ultrasonically-assisted supercritical extraction rectification to purify cynarin in globe artichoke Download PDF

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Publication number
CN105878323A
CN105878323A CN201610431892.XA CN201610431892A CN105878323A CN 105878323 A CN105878323 A CN 105878323A CN 201610431892 A CN201610431892 A CN 201610431892A CN 105878323 A CN105878323 A CN 105878323A
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extraction
cynarin
supercritical
leaf
ultrasonic
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CN201610431892.XA
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邓爱华
谢鹏
王云
谭小文
罗娟
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Hunan University of Arts and Science
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Hunan University of Arts and Science
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    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18—Magnoliophyta (angiosperms)
    • A61K36/185—Magnoliopsida (dicotyledons)
    • A61K36/28—Asteraceae or Compositae (Aster or Sunflower family), e.g. chamomile, feverfew, yarrow or echinacea
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K31/00—Medicinal preparations containing organic active ingredients
    • A61K31/21—Esters, e.g. nitroglycerine, selenocyanates
    • A61K31/215—Esters, e.g. nitroglycerine, selenocyanates of carboxylic acids
    • A61K31/216—Esters, e.g. nitroglycerine, selenocyanates of carboxylic acids of acids having aromatic rings, e.g. benactizyne, clofibrate
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C67/00—Preparation of carboxylic acid esters
    • C07C67/48—Separation; Purification; Stabilisation; Use of additives
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/30—Extraction of the material
    • A61K2236/37—Extraction at elevated pressure or temperature, e.g. pressurized solvent extraction [PSE], supercritical carbon dioxide extraction or subcritical water extraction
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/30—Extraction of the material
    • A61K2236/39—Complex extraction schemes, e.g. fractionation or repeated extraction steps
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/141—Feedstock
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/50—Improvements relating to the production of bulk chemicals
    • Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids

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  • Health & Medical Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Natural Medicines & Medicinal Plants (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Organic Chemistry (AREA)
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Abstract

The invention provides a method using ultrasonically-assisted supercritical extraction rectification to purify cynarin in globe artichoke. The method includes the steps of firstly, drying and crushing globe artichoke leaves, soaking with an ethanol aqueous solution, and loading into an ultrasonic extraction kettle; secondly, feeding supercritical CO2 into the ultrasonic extraction kettle, and soaking under certain pressure and temperature; thirdly, turning on an ultrasonic device, mixing the supercritical CO2 with 95% ethanol serving as the cosolvent for circulation extraction, and allowing the extracted supercritical solution to enter a rectifying tower for separation; fourthly, collecting a sample from the rectifying tower, and performing freeze drying to obtain reddish brown powder whose cynarin content can reach above 8.0%. The method has the advantages that the extraction process is assisted by ultrasonic, extraction efficiency can be increased, the supercritical CO2 extraction is combined with rectification, the products are separated according to the properties and boiling range during extraction, and the content of the cynarin in the extract can be increased greatly.

Description

A kind of method of cynarin in ultrasonic wave added super critical extracting and rectifying purification Carlina acaulis
Technical field
The present invention relates to extraction and the purification process of cynarin in Carlina acaulis, be specifically related to a kind of method of cynarin in ultrasonic wave added super critical extracting and rectifying purification Carlina acaulis.
Background technology
Leaf of Cynara scolymus L include abundant phenolic acid such as cynarin (1,5-dicaffeoylquinic acid), chlorogenic acid, 1,3-dicaffeoylquinic acid etc..It has protect the liver, hepatoprotective, effect for the treatment of dyspepsia etc..Therefore the exploitation to leaf of Cynara scolymus L can improve Carlina acaulis value-added content of product, can be that medicines and health protection field provides a kind of new raw material simultaneously.Artichoke leaf extract on international market typically requires that cynarin content is higher than 2.5% at present.
Current supercritical CO2Fluid extraction process there is problems in that 1 during cynarin in extraction and rectification purification leaf of Cynara scolymus L, extracting power is low, inefficient；2, the temperature of extracting system is high, can be destroyed heat sensitive cynarin；3, the cynarin quality of purification by liquid extraction is the highest.
Summary of the invention
For solving the problems referred to above, present invention aim at providing a kind of method of cynarin in ultrasonic wave added super critical extracting and rectifying purification Carlina acaulis.
The purpose of the present invention is achieved through the following technical solutions:
In a kind of ultrasonic wave added super critical extracting and rectifying purification Carlina acaulis, the method for cynarin, comprises the steps:
(1) the fresh blade of Carlina acaulis removes disease leaf, Huang Ye after gathering, and rinsing removes cold drying after the impurity such as earth, puts in disintegrating apparatus and pulverizes, and crosses 50 ~ 60 mesh sieves, prepares leaf of Cynara scolymus L coarse powder；
(2) it is 1:1 ~ 1:10 by prepared leaf of Cynara scolymus L coarse powder with 75% ~ 95% alcohol solution dipping, solid-liquid ratio, soaks 3 ~ 8 hours under room temperature；
(3) the leaf of Cynara scolymus L coarse powder after soaking puts in ultrasonic extraction still, carries out CO2Supercritical extraction；Extraction kettle temperature is 35 ~ 65 DEG C, extraction kettle pressure is 10 ~ 30MPa, CO2Flow is 10 ~ 50L/h, and ultrasonic wave added power is 200 ~ 800W, and entrainer is 95% ethanol solution, and extraction time is 0.5 ~ 3h；Extract is passed directly in rectifying column carry out rectification, and in rectifying column, pressure is 8 ~ 15Mpa, and in rectifying column, the temperature in four regions is respectively 45 DEG C, 60 DEG C, 75 DEG C, 85 DEG C from top to bottom；
(4) after rectification terminates, the fraction in the superiors region, lyophilization in collection rectifying column, obtains cynarin dry powder, and after testing, wherein cynarin content is not less than 8.0%.
Compared with prior art, the invention has the beneficial effects as follows: cynarin preparation method in a kind of Carlina acaulis of the present invention, at supercritical CO2Use ultrasonic wave added strengthening on the basis of extraction, and be combined with distillation technology, add supercritical CO2The extracting power of fluid, and reduce the temperature of extracting system so that heat sensitive cynarin can at utmost be retained.Additionally, invention also reduces the pressure of extracting system, entrainer consumption and extraction required time, substantially increase extraction efficiency.Supercritical CO2Extraction is combined with rectification, while extraction, by its character and boiling range, product is divided into some different products, can effectively ensure that and improve the content of cynarin.Simultaneously during whole, contamination-free is got rid of, without chemical residual, pure natural, nonhazardous, safety and environmental friendliness.
Detailed description of the invention
The following examples can illustrate in greater detail the present invention, but limits the present invention the most in any form.
Embodiment 1:
(1) the fresh blade of Carlina acaulis removes disease leaf, Huang Ye after gathering, and rinsing removes cold drying after the impurity such as earth, puts in disintegrating apparatus and pulverizes, and crosses 50 mesh sieves, prepares leaf of Cynara scolymus L coarse powder；
(2) by prepared leaf of Cynara scolymus L coarse powder 75% alcohol solution dipping, solid-liquid ratio is 1:1, soaks 3 hours under room temperature；
(3) the leaf of Cynara scolymus L coarse powder after soaking puts in ultrasonic extraction still, carries out CO2Supercritical extraction；Extraction kettle temperature is 35 DEG C, extraction kettle pressure is 10MPa, CO2Flow is 10L/h, and ultrasonic wave added power is 200W, and entrainer is 95% ethanol solution, and extraction time is 0.5h；Extract is passed directly in rectifying column carry out rectification, and in rectifying column, pressure is 8Mpa, and in rectifying column, the temperature in four regions is respectively 45 DEG C, 60 DEG C, 75 DEG C, 85 DEG C from top to bottom；
(4) after rectification terminates, the fraction in the superiors region, lyophilization in collection rectifying column, obtains cynarin dry powder, and after testing, wherein cynarin content is 8.3%.
Embodiment 2:
(1) the fresh blade of Carlina acaulis removes disease leaf, Huang Ye after gathering, and rinsing removes cold drying after the impurity such as earth, puts in disintegrating apparatus and pulverizes, and crosses 55 mesh sieves, prepares leaf of Cynara scolymus L coarse powder；
(2) by prepared leaf of Cynara scolymus L coarse powder 85% alcohol solution dipping, solid-liquid ratio is 1:5, soaks 6 hours under room temperature；
(3) the leaf of Cynara scolymus L coarse powder after soaking puts in ultrasonic extraction still, carries out CO2Supercritical extraction；Extraction kettle temperature is 50 DEG C, extraction kettle pressure is 20MPa, CO2Flow is 30L/h, and ultrasonic wave added power is 600W, and entrainer is 95% ethanol solution, and extraction time is 2h；Extract is passed directly in rectifying column carry out rectification, and in rectifying column, pressure is 12Mpa, and in rectifying column, the temperature in four regions is respectively 45 DEG C, 60 DEG C, 75 DEG C, 85 DEG C from top to bottom；
(4) after rectification terminates, the fraction in the superiors region, lyophilization in collection rectifying column, obtains cynarin dry powder, and after testing, wherein cynarin content is 9.3%.
Embodiment 3:
(1) the fresh blade of Carlina acaulis removes disease leaf, Huang Ye after gathering, and rinsing removes cold drying after the impurity such as earth, puts in disintegrating apparatus and pulverizes, and crosses 60 mesh sieves, prepares leaf of Cynara scolymus L coarse powder；
(2) by prepared leaf of Cynara scolymus L coarse powder 95% alcohol solution dipping, solid-liquid ratio is 1:10, soaks 8 hours under room temperature；
(3) the leaf of Cynara scolymus L coarse powder after soaking puts in ultrasonic extraction still, carries out CO2Supercritical extraction；Extraction kettle temperature is 65 DEG C, extraction kettle pressure is 30MPa, CO2Flow is 50L/h, and ultrasonic wave added power is 800W, and entrainer is 95% ethanol solution, and extraction time is 3h；Extract is passed directly in rectifying column carry out rectification, and in rectifying column, pressure is 15Mpa, and in rectifying column, the temperature in four regions is respectively 45 DEG C, 60 DEG C, 75 DEG C, 85 DEG C from top to bottom；
(4) after rectification terminates, the fraction in the superiors region, lyophilization in collection rectifying column, obtains cynarin dry powder, and after testing, wherein cynarin content is 10.3%
The above; it is only the present invention preferably detailed description of the invention; but protection scope of the present invention is not limited thereto; any those familiar with the art is in the technical scope of present disclosure; according to technical scheme and inventive concept equivalent or change in addition thereof, all should contain within protection scope of the present invention.

Claims (1)

1. the method for cynarin in a ultrasonic wave added super critical extracting and rectifying purification Carlina acaulis, it is characterised in that comprise the steps:
(1) the fresh blade of Carlina acaulis removes disease leaf, Huang Ye after gathering, and rinsing removes cold drying after the impurity such as earth, puts in disintegrating apparatus and pulverizes, and crosses 50 ~ 60 mesh sieves, prepares leaf of Cynara scolymus L coarse powder；
(2) it is 1:1 ~ 1:10 by prepared leaf of Cynara scolymus L coarse powder with 75% ~ 95% alcohol solution dipping, solid-liquid ratio, soaks 3 ~ 8 hours under room temperature；
(3) the leaf of Cynara scolymus L coarse powder after soaking puts in ultrasonic extraction still, carries out CO2Supercritical extraction；Extraction kettle temperature is 35 ~ 65 DEG C, extraction kettle pressure is 10 ~ 30MPa, CO2Flow is 10 ~ 50L/h, and ultrasonic wave added power is 200 ~ 800W, and entrainer is 95% ethanol solution, and extraction time is 0.5 ~ 3h；Extract is passed directly in rectifying column carry out rectification, and in rectifying column, pressure is 8 ~ 15Mpa, and in rectifying column, the temperature in four regions is respectively 45 DEG C, 60 DEG C, 75 DEG C, 85 DEG C from top to bottom；
(4) after rectification terminates, the fraction in the superiors region, lyophilization in collection rectifying column, obtains cynarin dry powder, and after testing, wherein cynarin content is not less than 8.0%.
CN201610431892.XA 2016-06-17 2016-06-17 Method using ultrasonically-assisted supercritical extraction rectification to purify cynarin in globe artichoke Pending CN105878323A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108484402A (en) * 2018-06-13 2018-09-04 爱可道生物科技有限公司 The purifying technique of cynarin in a kind of globe artichoke
CN110042000A (en) * 2019-03-27 2019-07-23 湖南文理学院 A kind of method of essential oil in ultrasonic wave added supercritical fluid extraction cape jasmine leaf
CN110465040A (en) * 2019-09-05 2019-11-19 刘长美 A kind of degradation agent and its preparation and application of farm-forestry crop pesticide residue of degrading
CN113651804A (en) * 2021-09-18 2021-11-16 陕西嘉禾生物科技股份有限公司 Industrialized preparation method of cynaropicrin

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100998626A (en) * 2006-12-20 2007-07-18 浙江大学 Method for preparing extract of korea thistle leaf
CN105543013A (en) * 2015-11-23 2016-05-04 郑汉洙 Makeup removing soap with plant botanical component extracting solution and manufacturing method for same

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100998626A (en) * 2006-12-20 2007-07-18 浙江大学 Method for preparing extract of korea thistle leaf
CN105543013A (en) * 2015-11-23 2016-05-04 郑汉洙 Makeup removing soap with plant botanical component extracting solution and manufacturing method for same

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
雷颂 等: "朝鲜蓟叶片多酚提取条件的工艺优化", 《农产品加工》 *

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108484402A (en) * 2018-06-13 2018-09-04 爱可道生物科技有限公司 The purifying technique of cynarin in a kind of globe artichoke
CN110042000A (en) * 2019-03-27 2019-07-23 湖南文理学院 A kind of method of essential oil in ultrasonic wave added supercritical fluid extraction cape jasmine leaf
CN110465040A (en) * 2019-09-05 2019-11-19 刘长美 A kind of degradation agent and its preparation and application of farm-forestry crop pesticide residue of degrading
CN113651804A (en) * 2021-09-18 2021-11-16 陕西嘉禾生物科技股份有限公司 Industrialized preparation method of cynaropicrin

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