CN102239983B - Method for extracting rubusoside from sweet tea leaves - Google Patents
Method for extracting rubusoside from sweet tea leaves Download PDFInfo
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- CN102239983B CN102239983B CN 201110124427 CN201110124427A CN102239983B CN 102239983 B CN102239983 B CN 102239983B CN 201110124427 CN201110124427 CN 201110124427 CN 201110124427 A CN201110124427 A CN 201110124427A CN 102239983 B CN102239983 B CN 102239983B
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Abstract
The invention provides a method for extracting rubusoside from sweet tea leaves, belonging to the technical field of natural product chemistry. The method comprises the following steps: drying the sweet tea leaves; extracting with ethanol solution, filtering, carrying out pressure reduced concentrating, then absorbing with resin, eluting with ethanol; carrying out pressure reduced concentrating on the elution solution, decoloring, crystallizing and recrystallizing to prepare into the pure rubusoside product. The processes for crystallizing, recrystallizing and purifying rubusoside are simple and easy to operate and ensure high purification degree.
Description
Technical field
The invention belongs to the technical field of natural product chemistry, and in particular to a kind of method that rubusoside is extracted from sweet tea.
Background technology
Sweet tea is the perennial rattan wood of the rose family, is a kind of distinctive wild sweet-tasting plant in Guangxi, main product is in my area Dayao Mountain, because its taste is sweet, therefore named Sweet tea.With Momordica grosvenori, STEVIA REBAUDIANA and claiming Guangxi three big sweet-tasting plant, there is long applicating history my area is among the people, local people, also for generation sugar processed food, can also be used as medicine always when tea-drinking is used for a long time.The analysis testing research center of Guangxi in 1979 has carried out Chemical bath deposition with regard to Sweet tea, determines that its chemical constitution containing sweet substance is consistent with rebaudioside, sugariness is 300 times of sucrose, and calorific value is only the 5% of sucrose.Identified, its rubusoside (Sweet tea glucoside) content is up to 6-7%.Through pharmacological testing, excessive with hypoglycemic, hypotensive, the gastric acid inhibitory that enhances metabolism, clearing heat and moistening lung, quench one's thirst of promoting the production of body fluid simultaneously have high sugariness, and the characteristic of low heat value can make diabetes, the auxiliary treatment of obesity.Thermal sensation, heat are coughed with preferable curative effect, had no toxic side effect through toxicological test, is a kind of new senior sweet taste health beverages in the world.It is tasty and refreshing that mouthfeel is fresh and sweet, suitable for people of all ages.Often drink, can physical fitness.
Both at home and abroad to being studied in terms of the separation and Extraction of rubusoside, test and pharmacology, the small-scale rubusoside for extracting higher degree is also had been reported that, but separating-purifying is carried out using substantial amounts of toxic reagent in separation process is extracted, there is obvious limitation in terms of being applied to food to rubusoside.Therefore, we are using sweet tea as raw material, carry out preparing rubusoside sterling on a large scale using means such as column chromatography, crystallization and recrystallizations, be added as food additives, be widely used in the health food of the patients such as obesity, hypertension, diabetes and heart disease.
The content of the invention
Present invention aim to provide, a kind of method is simple, low cost, industrialized production of being easy to, and products obtained therefrom purity is high, the preparation method of the rubusoside sterling of free from admixture.
The technical solution adopted by the present invention includes：Then sweet tea after dried concentrates through being extracted, being filtered with ethanol solution, be concentrated under reduced pressure with resin adsorption, ethanol elution, by eluent, decolourizes, and rubusoside sterling is made in crystallization and recrystallization.
Therefore, the present invention provides a kind of method that rubusoside is extracted from sweet tea, and step includes：
(1) crush and dry Sweet tea, and Sweet tea, 45% ethanol (kg)/volume ratio (V)=1: 1-3 by weight are mixed, heating and refluxing extraction；
(2) after filter cleaner, it is concentrated under reduced pressure into no ethanol flavor；
(3) macroporous absorbent resin LSA-40 (Xi'an Lanxiao Sci-Tech Co., Ltd.'s offer) carries out adsorbing separation on, and eluate is concentrated under reduced pressure drying, and wherein eluent is ethanol solution, and eluate is concentrated to dryness；
(4) add 70% ethanol and carry out heating for dissolving, then add activated carbon and decolourized, then carry out concentration until obtaining dried object；
(5) add 90% ethanol and carry out heating for dissolving, then add the hot water regulation final concentration of 40-50% of ethanol, ambient temperature overnight crystallization filters to obtain crystal, then carry out recrystallizing to obtain rubusoside sterling.
In one embodiment, in step 1 be 45% ethanol, preferably at 65 DEG C carry out heating stirring extraction.
In one embodiment, the filter process of step 2 is filtered through gauze, ceramic membrane filter.Wherein, preferably three layers filtered through gauze 2 times, ceramic membrane filter 1 time.
In one embodiment, wherein in step 3, the eluent of LSA-40 chromatographic columns is 30-80% ethanol solution.
In one embodiment, the ethanol of step 5 final concentration of 45%.
In another embodiment, 70% ethanol that is added in step 4, activated carbon, its volume (V)/weight (kg) ratio=16-10: 1.
In another embodiment, the crystallization of step 6 and recrystallization temperature are 4 DEG C until room temperature.
Technique effect：
1st, raw material used in the inventive method, equipment are common common raw material, equipment, it is to avoid for expensive raw materials, the dependence of instrument in commercial process, greatly reduce production cost；
2nd, the separation material used in this purge process is macroporous absorbent resin LSA-40, and its separation operation process is simple, is easy to get cheap, easy to control.
3rd, purified using crystallization and recrystallization, technique is simple, it is easy to operate, purification efficiency is high.
4th, the reagent used by the present invention is the routine techniques reclaimed in nontoxic, cheap, volume production chemical reagent, whole process using ripe reagent, and this greatly reduces to environmental emission discarded object.
5th, by long-felt, present invention determine that being crystallized at ambient temperature using 40-50% (preferably 45%) ethanol final concentration, the purity of rubusoside is highest, can reach 98.57-99.53%.
Brief description of the drawings
Fig. 1：The purity HPLC curve maps of rubusoside are extracted from Sweet tea, wherein ordinate represents peak area, and abscissa represents disengaging time.
Fig. 2：The HPLC curve maps of rubusoside standard items, wherein ordinate represent peak area, and abscissa represents disengaging time.
Embodiment
Below, the present invention will be further detailed with embodiment, but it is not limited to any one or similar example of these embodiments.
Embodiment 1：Crush and dry Sweet tea 100kg, add 45% ethanol 300L, 65 DEG C of heating and refluxing extraction 2h, three layers of filtered through gauze twice, ceramic membrane filter, it is concentrated under reduced pressure into 50L (no ethanol flavor), then macroporous absorbent resin LSA-40 posts on concentrate, obtain eluate with 70% ethanol elution, eluate are concentrated to dryness.Again with 70% ethanol 80L heating for dissolving, plus 5kg grain active carbons carry out decolouring 30min, are further concentrated to dry; after 90% ethanol 2L heating for dissolving, reheat water and mix, until ethanol final concentration 50%; then crystallizing at room temperature 24h, filters to obtain crystal, then carries out being recrystallized to give rubusoside sample.
After testing, Agilent1100 high performance liquid chromatographs, chromatographic column is Hypersil ODS (150mm × 4.6mm, 5 μm), and mobile phase is the aqueous solution of 65% methanol；Detection wavelength is 210nm；Flow velocity is 1ml/min；Sample size is 20 μ L.The purity of rubusoside sample is 97.27%, as a result as shown in table 1 and Fig. 1.
Embodiment 2：
Crush and dry Sweet tea 500kg, add 45% ethanol 600L, 65 DEG C of heating and refluxing extraction 2h, three layers of filtered through gauze twice, ceramic membrane filter, it is concentrated under reduced pressure into 100L (no ethanol flavor), then macroporous absorbent resin LSA-40 posts on concentrate, obtain eluate with 70% ethanol elution, eluate are concentrated to dryness.Again with 70% ethanol 150L heating for dissolving, plus 15kg activated carbon carries out decolouring 30min, is further concentrated to dry, after 90% ethanol 6L heating for dissolving, water is reheated until ethanol final concentration 47%, crystallizing at room temperature 24h, crystal is filtered to obtain, then carries out being recrystallized to give rubusoside sample.Purity detecting is carried out according to the method for embodiment 1, purity is 97.82%, as a result as shown in table 1.
Embodiment 3：
Crush and dry Sweet tea 200kg, add 45% ethanol 200L, 65 DEG C of heating and refluxing extraction 2h, three layers of filtered through gauze twice, ceramic membrane filter, it is concentrated under reduced pressure into 50L (no ethanol flavor), then macroporous absorbent resin LSA-40 posts on concentrate, obtain eluate with 70% ethanol elution, eluate are concentrated to dryness.Again with 70% ethanol 100L heating for dissolving, plus 8kg activated carbon carries out decolouring 30min, is further concentrated to dry, after 90% ethanol 3L heating for dissolving, water is reheated until ethanol final concentration 40%, crystallizing at room temperature 24h, crystal is filtered to obtain, then carries out being recrystallized to give rubusoside sample.Purity detecting is carried out according to the method for embodiment 1, purity is 98.95%, as a result as shown in table 1.
Embodiment 4：
Crush and dry Sweet tea 300kg, add 45% ethanol 300L, 65 DEG C of heating and refluxing extraction 2h, three layers of filtered through gauze twice, ceramic membrane filter, it is concentrated under reduced pressure into 80L (no ethanol flavor), then macroporous absorbent resin LSA-40 posts on concentrate, obtain eluate with 70% ethanol elution, eluate are concentrated to dryness.Again with 70% ethanol 120L heating for dissolving, plus 10kg activated carbon carries out decolouring 30min, is further concentrated to dry, after 90% ethanol 2L heating for dissolving, reheat water and mix until ethanol final concentration 45%, crystallizing at room temperature 24h, crystal is filtered to obtain, then carries out being recrystallized to give rubusoside sterling.Purity detecting is carried out according to the method for embodiment 1, purity is 99.45%, as a result as shown in table 1.
Table 1
With reference to above example, the present invention has advantages below compared with current art：
1. being prepared using conventional method, required equipment is simple, easy to operate, safety.
2. technology is not carried using the essence such as ultrasonic operation or Enzymatic Extraction, chromatography, therefore organic solvent loss is small, and environment is not polluted.
Claims (1)
1. a kind of method that rubusoside is extracted from Sweet tea, step is as follows：
(1) crush dry Sweet tea, and by Sweet tea and 45% ethanol by weight/volume ratio 1:1-3 is mixed, 65 DEG C of heating and refluxing extractions；
(2) after filter cleaner, it is concentrated under reduced pressure into no ethanol flavor；
(3) macroporous absorbent resin LSA-40 carries out adsorbing separation on, and eluate is concentrated under reduced pressure until obtaining dried object：Wherein eluent is 70% ethanol solution, and macroporous absorbent resin provides for Xi'an Lanxiao Sci-Tech Co., Ltd.；
(4) add 70% ethanol and carry out heating for dissolving, then add activated carbon and decolourized, then concentrated, until obtaining dried object；
(5) add 90% ethanol and carry out heating for dissolving, then add the hot water regulation final concentration of 40-50% of ethanol, ambient temperature overnight crystallization filters to obtain crystal, then carry out recrystallizing to obtain rubusoside sterling.
2. method according to claim 1, wherein step（2）In filter process be three layers of filtered through gauze 2 times and ceramic membrane filter 1 time.
3. method according to claim 1, wherein step（4）70% ethanol and the volume/weight ratio of activated carbon added is 16-10:1.
4. method according to claim 1, wherein step（5）Middle ethanol final concentration of 45%.
5. method according to claim 1, wherein step（6）Middle crystallization and recrystallization temperature are 4 DEG C until room temperature.
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| CN 201110124427 CN102239983B (en) | 2011-05-16 | 2011-05-16 | Method for extracting rubusoside from sweet tea leaves |
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Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102838644B (en) * | 2012-08-23 | 2015-06-03 | 湖南绿蔓生物科技股份有限公司 | Production method for extracting sweet tea glucoside from sweet tea leaves |
| CN104370981B (en) * | 2014-09-30 | 2016-08-24 | 桂林市一峰食品有限公司 | A kind of method extracting Folium hydrangeae strigosae element from Folium hydrangeae strigosae |
| CN104262427B (en) * | 2014-09-30 | 2017-02-01 | 桂林三宝药业有限公司 | Method for extracting rubusoside from sweet tea leaves |
| CN104483424B (en) * | 2014-12-18 | 2017-01-18 | 广西壮族自治区中医药研究院 | Rubusoside quality control method |
| 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 |
| CN106924304A (en) * | 2017-03-29 | 2017-07-07 | 桂林实力科技有限公司 | The extracting method of Sweet tea active ingredient |
| CN108541948A (en) * | 2018-07-16 | 2018-09-18 | 怀化学院 | A kind of lithocarpus litseifolius lozenge and preparation method thereof |
| CN109503675B (en) * | 2018-12-07 | 2021-10-12 | 湖南食品药品职业学院 | Method for extracting rubusoside and ursolic acid from sweet tea |
| CN109717445B (en) | 2019-01-30 | 2022-10-18 | 湖南绿蔓生物科技股份有限公司 | Sweet taste composition and preparation method and application thereof |
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| CN1122447C (en) * | 2001-01-05 | 2003-10-01 | 云南省农业科学院生物技术研究所 | Sweet tea extract and its preparing process and application |
| CN101003552A (en) * | 2006-01-18 | 2007-07-25 | 广西师范大学 | Method for preparing glycosides in high purity |
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