CN104262427B - Method for extracting rubusoside from sweet tea leaves - Google Patents
Method for extracting rubusoside from sweet tea leaves Download PDFInfo
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- CN104262427B CN104262427B CN201410520899.XA CN201410520899A CN104262427B CN 104262427 B CN104262427 B CN 104262427B CN 201410520899 A CN201410520899 A CN 201410520899A CN 104262427 B CN104262427 B CN 104262427B
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- sweet tea
- extraction
- extract
- hydrangeae strigosae
- folium hydrangeae
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H15/00—Compounds containing hydrocarbon or substituted hydrocarbon radicals directly attached to hetero atoms of saccharide radicals
- C07H15/20—Carbocyclic rings
- C07H15/24—Condensed ring systems having three or more rings
- C07H15/256—Polyterpene radicals
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
- C07H1/06—Separation; Purification
- C07H1/08—Separation; Purification from natural products
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- 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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Abstract
The invention discloses a method for extracting rubusoside from sweet tea leaves. The method comprises the following steps: pretreatment, ultrasonic wave treatment, supercritical treatment, decolorization treatment, crystallization and recrystallization. By adopting the method disclosed by the invention, ultra-high-purity rubusoside products can be produced, the loss of materials is reduced, the production period is shortened and the yield is improved. The purity of rubusoside produced by the method is higher than 99.61% and the product has high purity and single component.
Description
Technical field
The present invention relates to extracting the technical field of active component from sweet tea, extract from sweet tea particularly to one kind
The method of Folium hydrangeae strigosae element.
Background technology
Folium hydrangeae strigosae is the perennial rattan wood of Rosaceae, is a kind of distinctive wild sweet-tasting plant in Guangxi, main product in my area Dayao Mountain,
Because its taste is sweet, therefore named Folium hydrangeae strigosae.With Fructus Momordicae, Folium Stevlae Rebaudianae and claim Guangxi three big sweet-tasting plant, my area among the people have long
Applicating history, for a long time local people always when tea-drinking is used, be also used for generation sugar processed food, also can be used as medicine.Guangxi in 1979
Analysis testing research center has carried out Chemical bath deposition with regard to Folium hydrangeae strigosae, determines that it contains the chemical constitution of sweet substance and stevioside
Unanimously, sugariness is 300 times of sucrose, and calorific value is only the 5% of sucrose.Identified, its Folium hydrangeae strigosae element (Folium hydrangeae strigosae glucoside) content is up to 6
～7%.Through pharmacological testing, there is blood sugar lowering, blood pressure lowering, the gastric acid inhibitory that enhances metabolism excessively, clearing heat and moistening lung, solution of promoting the production of body fluid
Yearningly and have high sugariness, low-calorie characteristic, the auxiliary treatment of diabetes, obesity can be made.Thermal sensation, heat syndrome cough are had preferably
Curative effect, has no toxic side effect through toxicological test, is a kind of new senior sweet taste health promoting beverage in the world.It is tasty and refreshing that mouthfeel is fresh and sweet, always
Few all suitable.Often drink, can building body.
Both at home and abroad the aspects such as the separation and Extraction of Folium hydrangeae strigosae element, test and pharmacology are studied, small-scale is extracted higher
The Folium hydrangeae strigosae element of purity also has been reported that, but carries out separating-purifying using substantial amounts of toxic reagent in extracting separation process, to sweet
Theine is applied to food aspect obvious restriction.For this reason, the present invention is with sweet tea as raw material, using supercritical co2Extraction, crystallization
Prepared Folium hydrangeae strigosae element sterling on a large scale with means such as recrystallization, be added as food additive, be widely used in fertilizer
The health food of the patient such as fat, hypertension, diabetes and heart disease.
Content of the invention
The technical problem to be solved is to provide a kind of method extracting Folium hydrangeae strigosae element from sweet tea, the method energy
Enough extract highly purified Folium hydrangeae strigosae element.
For achieving the above object, the present invention adopts the following technical scheme that
A kind of method extracting Folium hydrangeae strigosae element from sweet tea, including following preparation process:
(1) pretreatment: remove the impurity in sweet tea, mechanical activation comminution, cross sieve classification, obtain sweet tea powder；
(2) ultrasonic Treatment: take sweet tea powder to put in ultrasonic unit and carry out ultrasonic Treatment, ultrasonic Treatment bar
Part: temperature is 50 DEG C～65 DEG C, power is 200w～350w, and the time is 3～6min, during supersound process, adds sweet tea grain weight
0.5%～1.1% vitamin e of amount；
(3) first supercritical processing: carry out supercritical co in the sweet tea powder loading extraction kettle that supersound process is crossed2Extraction, with
Supercritical co2Fluid be extractant, with volumetric concentration be 60～75% ethanol solution as entrainer, wherein, extracting pressure
For 25～35mpa, extraction temperature is 45～55 DEG C, co2Flow is 10～13l/h, collects extract every 20～30min, when
When no longer having extract to flow out, extraction finishes, and obtains extract；
(4) desolventing technology: add 60%～65% ethanol heating for dissolving in extract, add activated carbon and taken off
Color, then be vacuum dried under conditions of absolute pressure 4.0～4.5kpa, obtain dried object；
(5) crystallization and recrystallization: add 75%～85% ethanol heating for dissolving, low temperature crystallization in dried object, filter
Crystal, then carry out recrystallization, filter, be dried, obtain Folium hydrangeae strigosae element sterling.
The mesh number crossing sieve classification in step (1) of the present invention is 50～80 mesh.
Step (3) sweet tea powder of the present invention loads 20%～30% that volume is extraction kettle volume.
The temperature that step (5) of the present invention crystallizes is 4 DEG C～30 DEG C.
The temperature that step (5) of the present invention crystallizes is preferably 25 DEG C.
Compared with the prior art, the beneficial effects of the present invention is:
(1) present invention is by ultrasonic technology and supercritical co2Extraction phase combines, and reduces supercritical co2The extraction pressure of extraction
Power and temperature, shorten extraction time, and the Folium hydrangeae strigosae element purity obtaining are high, reaches more than 99.61%.During without ultrasonic Treatment,
The extracting pressure of supercritical extraction is 45～55mpa, and extraction temperature is 75 DEG C～80 DEG C, co2Flow is 20～30l/h, extraction
Time is 90min～150min.After being ultrasonically treated, extracting pressure is 25～35mpa, and extraction temperature is 45～55 DEG C,
co2Flow is 10～13l/h, and extraction time shorten to 50～70min hence it is evident that reducing extracting pressure and extraction temperature, reduces
Co2Flow, shortens extraction time.
(2) by supercritical co2The Folium hydrangeae strigosae extract being obtained by extraction is crystallized and recrystallization again, improves pure further
Degree, it is easy to operate, purification efficiency is high for process is simple.
Specific embodiment
The invention will be further described with reference to embodiments, but the invention is not limited in these embodiments.
Embodiment 1
A kind of method extracting Folium hydrangeae strigosae element from sweet tea, including following preparation process:
(1) pretreatment: remove the impurity in sweet tea, mechanical activation comminution, cross 50 mesh size, obtain sweet tea powder；
(2) ultrasonic Treatment: take sweet tea powder to put in ultrasonic unit and carry out ultrasonic Treatment, ultrasonic Treatment bar
Part: temperature is 50 DEG C, power is 200w, and the time is 3min, during supersound process, adds 0.5% vitamin of sweet tea grain weight amount
e；
(3) first supercritical processing: carry out supercritical co in the sweet tea powder loading extraction kettle that supersound process is crossed2Extraction, with
Supercritical co2Fluid be extractant, with volumetric concentration be 60% ethanol solution as entrainer, wherein, sweet tea powder load
Volume is the 20% of extraction kettle volume, and extracting pressure is 25mpa, and extraction temperature is 45 DEG C, co2Flow is 10l/h, every
20min collects extract, and when no longer there being extract to flow out, extraction finishes, and obtains extract；
(4) desolventing technology: add 60% ethanol heating for dissolving in extract, add activated carbon and decoloured, then
It is vacuum dried under conditions of absolute pressure 4.0kpa, obtained dried object；
(5) crystallization and recrystallization: add 75% ethanol heating for dissolving in dried object, crystallize at a temperature of 4 DEG C, filter
Crystal, then carry out recrystallization, filter, be dried, obtain Folium hydrangeae strigosae element sterling.
After testing, agilent1100 high performance liquid chromatograph, chromatographic column is hypersil ods (150mm × 4.6mm, 5 μ
M), mobile phase is the aqueous solution of 65% methanol, and Detection wavelength is 210nm, and flow velocity is 1ml/min, and sample size is 20 μ l, records sweet
The purity of theine sample is 99.61%.
Embodiment 2
A kind of method extracting Folium hydrangeae strigosae element from sweet tea, including following preparation process:
(1) pretreatment: remove the impurity in sweet tea, mechanical activation comminution, cross 60 mesh size, obtain sweet tea powder；
(2) ultrasonic Treatment: take sweet tea powder to put in ultrasonic unit and carry out ultrasonic Treatment, ultrasonic Treatment bar
Part: temperature is 55 DEG C, power is 250w, and the time is 4min, during supersound process, adds 0.7% vitamin of sweet tea grain weight amount
e；
(3) first supercritical processing: carry out supercritical co in the sweet tea powder loading extraction kettle that supersound process is crossed2Extraction, with
Supercritical co2Fluid be extractant, with volumetric concentration be 65% ethanol solution as entrainer, wherein, sweet tea powder load
Volume is the 25% of extraction kettle volume, and extracting pressure is 28mpa, and extraction temperature is 48 DEG C, co2Flow is 11l/h, every
25min collects extract, and when no longer there being extract to flow out, extraction finishes, and obtains extract；
(4) desolventing technology: add 65% ethanol heating for dissolving in extract, add activated carbon and decoloured, then
It is vacuum dried under conditions of absolute pressure 4.2kpa, obtained dried object；
(5) crystallization and recrystallization: add 80% ethanol heating for dissolving in dried object, crystallize at a temperature of 15 DEG C, filter
Obtain crystal, then carry out recrystallization, filter, be dried, obtain Folium hydrangeae strigosae element sterling.
After testing, agilent1100 high performance liquid chromatograph, chromatographic column is hypersil ods (150mm × 4.6mm, 5 μ
M), mobile phase is the aqueous solution of 65% methanol, and Detection wavelength is 210nm, and flow velocity is 1ml/min, and sample size is 20 μ l, records sweet
The purity of theine sample is 99.91%.
Embodiment 3
A kind of method extracting Folium hydrangeae strigosae element from sweet tea, including following preparation process:
(1) pretreatment: remove the impurity in sweet tea, mechanical activation comminution, cross 70 mesh size, obtain sweet tea powder；
(2) ultrasonic Treatment: take sweet tea powder to put in ultrasonic unit and carry out ultrasonic Treatment, ultrasonic Treatment bar
Part: temperature is 55 DEG C, power is 300w, and the time is 5min, during supersound process, adds 0.9% vitamin of sweet tea grain weight amount
e；
(3) first supercritical processing: carry out supercritical co in the sweet tea powder loading extraction kettle that supersound process is crossed2Extraction, with
Supercritical co2Fluid be extractant, with volumetric concentration be 70% ethanol solution as entrainer, wherein, sweet tea powder load
Volume is the 25% of extraction kettle volume, and extracting pressure is 30pa, and extraction temperature is 50 DEG C, co2Flow is 12l/h, every 25min
Collect extract, when no longer there being extract to flow out, extraction finishes, and obtains extract；
(4) desolventing technology: add 60% ethanol heating for dissolving in extract, add activated carbon and decoloured, then
It is vacuum dried under conditions of absolute pressure 4.3kpa, obtained dried object；
(5) crystallization and recrystallization: add 80% ethanol heating for dissolving in dried object, crystallize at a temperature of 25 DEG C, filter
Obtain crystal, then carry out recrystallization, filter, be dried, obtain Folium hydrangeae strigosae element sterling.
After testing, agilent1100 high performance liquid chromatograph, chromatographic column is hypersil ods (150mm × 4.6mm, 5 μ
M), mobile phase is the aqueous solution of 65% methanol, and Detection wavelength is 210nm, and flow velocity is 1ml/min, and sample size is 20 μ l, records sweet
The purity of theine sample is 99.99%.
Embodiment 4
A kind of method extracting Folium hydrangeae strigosae element from sweet tea, including following preparation process:
(1) pretreatment: remove the impurity in sweet tea, mechanical activation comminution, cross 80 mesh size, obtain sweet tea powder；
(2) ultrasonic Treatment: take sweet tea powder to put in ultrasonic unit and carry out ultrasonic Treatment, ultrasonic Treatment bar
Part: temperature is 65 DEG C, power is 350w, and the time is 6min, during supersound process, adds 1.1% vitamin of sweet tea grain weight amount
e；
(3) first supercritical processing: carry out supercritical co in the sweet tea powder loading extraction kettle that supersound process is crossed2Extraction, with
Supercritical co2Fluid be extractant, with volumetric concentration be 75% ethanol solution as entrainer, wherein, sweet tea powder load
Volume is the 30% of extraction kettle volume, and extracting pressure is 35mpa, and extraction temperature is 55 DEG C, co2Flow is 13l/h, every
30min collects extract, and when no longer there being extract to flow out, extraction finishes, and obtains extract；
(4) desolventing technology: add 65% ethanol heating for dissolving, add activated carbon and decoloured, then in absolute pressure
It is vacuum dried under conditions of 4.5kpa, obtained dried object；
(5) crystallization and recrystallization: add 85% ethanol heating for dissolving in dried object, crystallize at a temperature of 30 DEG C, filter
Obtain crystal, then carry out recrystallization, filter, be dried, obtain Folium hydrangeae strigosae element sterling.
After testing, agilent1100 high performance liquid chromatograph, chromatographic column is hypersil ods (150mm × 4.6mm, 5 μ
M), mobile phase is the aqueous solution of 65% methanol, and Detection wavelength is 210nm, and flow velocity is 1ml/min, and sample size is 20 μ l, records sweet
The purity of theine sample is 99.87%.
Claims (4)
1. a kind of method extracting Folium hydrangeae strigosae element from sweet tea is it is characterised in that include following preparation process:
(1) pretreatment: remove the impurity in sweet tea, mechanical activation comminution, cross sieve classification, obtain sweet tea powder；
(2) ultrasonic Treatment: take sweet tea powder to put in ultrasonic unit and carry out ultrasonic Treatment, ultrasonic Treatment condition: temperature
Spend for 50 DEG C～65 DEG C, power is 200w～350w, and the time is 3～6min, during supersound process, add sweet tea grain weight amount
0.5%～1.1% vitamin e；
(3) first supercritical processing: carry out supercritical co in the sweet tea powder loading extraction kettle that supersound process is crossed2Extraction, with supercritical
co2Fluid be extractant, with volumetric concentration be 60～75% ethanol solution as entrainer, wherein, extracting pressure be 25～
35mpa, extraction temperature is 45～55 DEG C, co2Flow is 10～13l/h, collects extract every 20～30min, when no longer having
When extract flows out, extraction finishes, and obtains extract；
(4) desolventing technology: add 60%～65% ethanol heating for dissolving in extract, add activated carbon and decoloured, then
It is vacuum dried under conditions of absolute pressure 4.0～4.5kpa, obtained dried object；
(5) crystallization and recrystallization: add 75%～85% ethanol heating for dissolving, low temperature crystallization in dried object, filter and must crystallize
Thing, then carry out recrystallization, filter, be dried, obtain Folium hydrangeae strigosae element sterling；
The mesh number crossing sieve classification in described step (1) is 50～80 mesh.
2. according to claim 1 from sweet tea extract Folium hydrangeae strigosae element method it is characterised in that: described step (3)
Sweet tea powder loads 20%～30% that volume is extraction kettle volume.
3. the method extracting Folium hydrangeae strigosae element from sweet tea according to claim 1 it is characterised in that: described step (5) knot
Brilliant temperature is 4 DEG C～30 DEG C.
4. the method extracting Folium hydrangeae strigosae element from sweet tea according to claim 3 it is characterised in that: described step (5) knot
Brilliant temperature is 25 DEG C.
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| CN201410520899.XA CN104262427B (en) | 2014-09-30 | 2014-09-30 | Method for extracting rubusoside from sweet tea leaves |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| KR101734857B1 (en) | 2015-02-17 | 2017-05-15 | 서울대학교산학협력단 | A composition for inhibiting glut1, glut5, or glut1 and glut5 activities |
| JP6633833B2 (en) * | 2015-03-23 | 2020-01-22 | 株式会社ヤクルト本社 | Sweet tea extract essence and its use |
| CN105166198A (en) * | 2015-09-29 | 2015-12-23 | 重庆骄王天然产物股份有限公司 | Preparation method of high-purity rubusoside |
| CN105153252A (en) * | 2015-09-30 | 2015-12-16 | 桂林益元素生物科技有限公司 | Method for extracting rubusoside from strigose hydrangea leaves |
| CN113831374B (en) * | 2021-11-08 | 2023-03-31 | 湖南华诚生物资源股份有限公司 | Method for crystallizing rubusoside |
| CN115212263A (en) * | 2022-08-15 | 2022-10-21 | 邓冰言 | Ampelopsis grossedentata dropping pill and preparation method thereof |
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