CN102838644A - Production method for extracting sweet tea glucoside from sweet tea leaves - Google Patents
Production method for extracting sweet tea glucoside from sweet tea leaves Download PDFInfo
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- 235000009508 confectionery Nutrition 0.000 title claims abstract description 54
- 241001122767 Theaceae Species 0.000 title claims abstract description 51
- 238000004519 manufacturing process Methods 0.000 title abstract description 13
- 229930182478 glucoside Natural products 0.000 title abstract 6
- 150000008131 glucosides Chemical class 0.000 title abstract 6
- 238000000034 method Methods 0.000 claims abstract description 24
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 21
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- 238000001035 drying Methods 0.000 claims abstract description 8
- 239000000463 material Substances 0.000 claims abstract description 8
- 239000002904 solvent Substances 0.000 claims abstract description 8
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- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 15
- 239000000284 extract Substances 0.000 claims description 12
- 239000002994 raw material Substances 0.000 claims description 12
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- 239000004952 Polyamide Substances 0.000 claims description 4
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Images
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Abstract
The invention provides a production method for extracting sweet tea glucoside from sweet tea leaves. The method comprises the following process flows of: smashing a sweet tea crude drug; extracting a solvent; concentrating; precipitating with alcohol; purifying with macroporous resin; concentrating; carrying out chromatography with polyamide resin; concentrating; crystallizing and recrystallizing; drying; and obtaining a finished product. By using the method, a high-quality sweet tea glucoside product can be produced, and the method also has the advantages of reducing the material loss, shortening the production period, improving the product yield and reducing the production cost and is suitable for the industrial production; the purity of the sweet tea glucoside produced by utilizing the method is higher than 98 percent, so that the product purity is high, and the component is single; the color of the sweet tea glucoside is white and good; and meanwhile, the technical difficulty of industrially producing a high-content and high-quality sweet tea glucoside extractive is overcome, so that large-scale production is smoothly produced.
Description
Technical field
The present invention relates to a kind of working method of from sweet tea, extracting sweet tea glycosides.
Background technology
Sweet tea is the perennial rattan of Rosaceae wood, and for Guangxi distinctive a kind of nontoxic, low heat energy, high sugariness with have the wild rare sweet taste plant of nourishing function, main product is in the counties and cities such as Yao Shan, Jin Xiu, Yongfu and Cenxi in Guangxi.Because its flavor is sweet, so the sweet tea of name.With Grosvenor Momordica, sweet Stevia and be called Guangxi three big sweet taste plants, among the people in Guangxi have a long applicating history, and local people are always when tea-drinking usefulness for a long time, also is used for generation sugar processed food, also can be used as medicine.
The staple of sweet tea has sweet tea glycosides, Vitamin P complex, tea-polyphenol, amino acid, inorganic salt etc.
The main sweet ingredient of sweet tea is sweet tea glycosides, is the tetracyclic diterpene glycosides of steviol and glucose be combined into, molecular formula C
20H
50O
13, similar with stevioside glycosides (stevioside) on chemical structure.The sugariness of sweet tea glycosides is about 300 times of sweetness of cane sugar, and calorific value only is 5% of a sucrose.Through pharmacological evaluation; That sweet tea glycosides has is hypoglycemic, hypotensive, enhance metabolism, gastric acid inhibitory is too much; Clearing heat and moistening lung, promote the production of body fluid and quench one's thirst and high sugariness is arranged, low-calorie characteristic not only can be used as medicinal; Still a kind of colory foodstuff additive, but place of sucrose is used for patient such as hypertension, mellitus, obesity and the elderly and children's food, healthcare products and medicine.
Both at home and abroad the aspects such as separation and Extraction, test and pharmacology of sweet tea glycosides are studied; Sweet tea glycosides to extracting higher degree on a small scale also has report; But high-load sweet tea glycosides suitability for industrialized production is not also appeared in the newspapers; And in the extraction separation process, adopting a large amount of toxic reagents to carry out separation and purification, sweet tea glycosides is applied to the food aspect has significant limitation.This explanation, existing technical study still is in the junior stage, and can't really reach industrialized production machine marketing level.For this reason; We are raw material with the sweet tea; Adopt means such as macroporous resin separation and purification, column chromatography, crystallization and recrystallization to prepare the pure article of sweet tea glycosides on a large scale, add, be widely used in patients' such as obesity, hypertension, mellitus and heart trouble protective foods as foodstuff additive.
Summary of the invention
It is low to the purpose of this invention is to provide a kind of cost, simple to operate, and loss of material is few, with short production cycle, and the product yield is high, and low toxic and environment-friendly is suitable for industrialized production, and products obtained therefrom purity is high, the preparation method of the pure article of pure sweet tea glycosides.
The technical scheme that the present invention adopts may further comprise the steps:
1) bulk drug extracts
With the sweet tea is raw material, adds water after the fragmentation, through heating and refluxing extraction 2～3 times or normal pressure ultrasonic extraction; During heating and refluxing extraction, extract 60～80 ℃ of temperature, for the first time the hot water lixiviate; The volumetric usage of water is 8～12 times of raw material, and extraction time 50～70min is in each hot water lixiviate afterwards; The volume of water consumption is 0.7～1 times of raw material, extraction time 20～40min; When adopting the normal pressure supersound extraction, ultrasonic power output 250～350W, 60～80 ℃ of temperature, water consumption is 10 times of raw material at least, extracts at least 2 times, each extraction time 5～8min;
2) merge said extracted liquid concentrating under reduced pressure; The condition of concentrating: vacuum ranges 0.7～1MPa, temperature is not higher than 90 ℃, concentrates material liquid volume to 1:1～3; Be concentrated into every liter at last and contain 0.8～1.2Kg crude drug;
3) concentrate back adding ethanol sedimentation and go out insolubles, filter;
4) macroporous resin purification: filtrating is through resin column, and it is colourless to be washed till effluent with purified water (being zero(ppm) water), and using concentration of volume percent then is that 50%～70% ethanolic soln carries out wash-out, collects elutriant, concentrates, until obtaining dry matter sample; Resin: sample quality is than being 1:8～12;
5) polyamide resin chromatography: the aqueous solution that sample ligand is set to 10%～20% mass percent concentration is crossed polyamide column, collects the post flow liquid, and with water wash to there not being sweet taste, merge post flow liquid and water elution liquid, concentrate, drying must bullion;
6) crystallization-recrystallization: add solvent in the bullion, place 75～85 ℃ of water-baths to be heated to whole dissolvings, filtered while hot, placement is separated out, filters, recrystallization again, spraying drying obtains sweet tea glycosides elaboration.
Of the present inventionly also can adopt following mode to handle, when promptly wherein adopting reflux 3 times in the step 1), extracting solution is as extracting the water use the following batch first time for the third time.
When the present invention adopted the hot water lixiviate, particularly preferably being the extraction time first time was 60min; Each extraction time of hot water lixiviate afterwards is 30min.Each extraction time is 6min in the normal pressure supersound extraction.
Macroporous resin among the present invention in the step 4) particularly preferably is the D-101 macroporous resin.
Collect 2～3 times of column volume elutriants in the said step 4).
Polyamide resin specification in the step 5) of the present invention is 100～200 orders.
In the step 6) of the present invention the solvent of crystallization-recrystallization comprise methyl alcohol, ethanol, acetone, ETHYLE ACETATE, chloroform or sherwood oil one or more.
Crystallization in the step 6 of the present invention-recrystallization temperature scope: be advisable for 60～80 ℃.Especially preferably bullion is placed 80 ℃ of water-bath heating for dissolving.
The present invention passes through drying sweet tea later; Crushing screening; Hot water refluxing extraction or ultrasonic-assisted extraction, come, concentrating under reduced pressure, ethanol sedimentation impurity is then with resin absorption, ethanol elution, concentrate elutriant; Cross the polyamide resin chromatography, concentrate, crystallization and recrystallization obtain purity and are not less than 98% pure article of sweet tea glycosides.The advantage that has following technique effect with respect to prior art:
1) material equipment cost advantage: the raw material that uses in the inventive method, equipment are common common raw material, equipment, have avoided in the commercial process having reduced production cost widely for expensive raw materials, together dependence.
2) on extracting mode, adopt hot water lixiviate refluxing extraction or ultrasonic extraction, can effectively improve product yield, the leaching that helps activeconstituents with separate, help controlling the phenomenon of bubbling and running material in the production process simultaneously.Adopt extracting solution solvent cover formulation, reduce solvent consumption.
3) extracting solution adding ethanolic soln is settled out insolubles, can effectively insolubless such as amino acid be removed, and improves product purity.
4) among the present invention; What adopt is nonpolar macroporous resin, because this resin has sizable specific surface area and suitable aperture, the glycoside material is had special selected property; Can with the Flavonoid substances in the sweet tea, phenolic substance, amino acid etc. separately guarantee product purity; Also adopted the polyamide resin chromatography among the present invention, the further sweet tea glycosides of separation and purification, its lock out operation is simple, and is easy to control.
5) technological line of low toxic and environment-friendly economical and efficient: what the present invention taked is a kind of technological line of environmental protection economy; The extraction of adopting in this technological line; Concentrate, production units such as purification devices all can adopt airtight system, in the process of operation; Can avoid operator to touch reagent to greatest extent, ensure the health of human body effectively.The solvent that adopts in this method, resin etc. can both recycle, and can reduce loss of material, improve the product yield.This technological line echoes in the pattern of China's Sustainable development mutually, and good social benefit is arranged.
6) produce market advantage: the present invention is through with the assurance of several key technology parameters in the whole technology with provide, and can make the purity of sweet tea glycosides of technology gained of the present invention be not less than 98%, is the pure white crystallization, is the high-quality sweet tea extract of high-content; And the ability industrialized mass production, become the sweet tea extract product that added value of product is the highest in the market, satisfied the needs of problems of market to high-quality sweet tea glycoside product.
7) agriculture industrialization, the large-scale development of the sweet tea of drive China improve farmers' income; Improve the added value of sweet tea extract, promote the plant milk extract industry development; Satisfy downstream industry to the high-quality sweet tea glycosides demand of high-content, promote the common development of every profession and trade, and be that society creates good economic benefit and social benefit.
Description of drawings
Fig. 1 is a concrete process flow sheet of the present invention.
Embodiment
Below, the present invention will further specify with embodiment, but it is not limited to any or similar instance of these instances.
Embodiment 1
Get sweet tea 500Kg (is 5.2% through detection level), 40 mesh sieves are crossed in broken back, drop in the extractor; Add zero(ppm) water 5000L, be heated to 80 ℃, refluxing extraction 60min; Suction filtration while hot respectively adds 4000L zero(ppm) water again and carries out for the second time, extracts for the third time in the dregs of a decoction, with condition refluxed 30min/ time; Merging for the first time, extracting solution is concentrated into 500L for the second time, and following batch of extraction for the first time of extracting solution do for the third time made water and used.Liquid concentrator adds the 350L ethanol sedimentation and goes out insolubles, filters, and filtrating adds in the good 50KgD101 resin column of pre-treatment, flow velocity 5BV/h; After upper prop finished, it was colourless to be washed till effluent with purified water, used 70% ethanol elution at last; Flow velocity 1BV/h collects this elutriant of 150L, is concentrated into dried.Sample ligand is set to the aqueous solution of 20% concentration, crosses polyamide column, collect the post flow liquid, and with zero(ppm) water drip washing to there not being sweet taste, merging post flow liquid and water elution liquid are concentrated into driedly, obtain the sweet tea glycosides of bullion (content 81.2%).Add methyl alcohol, place 80 ℃ of water-bath reflux to all dissolvings, suction filtration while hot, placement washes out, and filtering crystallisate carries out recrystallization again, and spraying drying gets pure white crystal 18.65Kg, through detecting Tianjin, island high performance liquid chromatograph, chromatographic column C
18(4.6mm * 250mm, 5um), moving phase is methyl alcohol: water=80:20; The detection wavelength is 210nm; Flow velocity is 1mL/min; Sample size is 10uL (following implementation issue is together), and purity is 98.15%, yield 3.73%, and the recovery of the sweet tea glycosides of whole process reaches 70.4%.
Embodiment 2
Get sweet tea 500Kg (is 5.4% through detection level),, be crushed to and drop into behind 40 orders in the ultrasonic extraction jar; Add 5000L zero(ppm) water, ultrasonic power output 800W, 80 ℃ of supersound extraction 6min; Filter, add 4000L zero(ppm) water in the dregs of a decoction once more and carry out for the second time, extract for the third time, after extracting 6min under the condition; Merging for the first time, extracting solution is concentrated into 500L for the second time, and extracting solution is done down and done water treatment batch first time for the third time.Liquid concentrator adds the 350L ethanol sedimentation and goes out insolubles, filters, and filtrating adds in the good 50KgD101 resin column of pre-treatment, flow velocity 5BV/h; After upper prop finished, it was colourless to be washed till effluent with purified water, used 70% ethanol elution at last; Flow velocity 1BV/h collects this elutriant of 150L, is concentrated into dried.Sample ligand is set to the aqueous solution of 20% concentration, crosses polyamide column, collect the post flow liquid, and with zero(ppm) water drip washing to there not being sweet taste, merging post flow liquid and water elution liquid are concentrated into driedly, obtain the sweet tea glycosides of bullion (content 81.2%).Add methyl alcohol, place 80 ℃ of water-bath reflux to all dissolvings, suction filtration while hot, placement washes out; Filtering crystallisate carries out recrystallization again, and spraying drying gets pure white crystal 19.48Kg, through detecting; Purity is 98.24%, yield 3.90%, and the recovery of the sweet tea glycosides of whole process reaches 70.95%.
Claims (10)
1. a working method of from sweet tea, extracting sweet tea glycosides is characterized in that, may further comprise the steps:
1) bulk drug extracts
With the sweet tea is raw material, adds water after the fragmentation, through heating and refluxing extraction 2～3 times or normal pressure ultrasonic extraction; During heating and refluxing extraction, extract 60～80 ℃ of temperature, for the first time the hot water lixiviate; The volumetric usage of water is 8～12 times of raw material, and extraction time 50～70min is in each hot water lixiviate afterwards; The volume of water consumption is 0.7～1 times of raw material, extraction time 20～40min; When adopting the normal pressure supersound extraction, ultrasonic power output 250～350W, 60～80 ℃ of temperature, water consumption is 10 times of raw material at least, extracts at least 2 times, each extraction time 5～8min;
2) merge said extracted liquid concentrating under reduced pressure; The condition of concentrating: vacuum ranges 0.7～1MPa, temperature is not higher than 90 ℃, concentrates material liquid volume to 1:1～3; Be concentrated into every liter at last and contain 0.8～1.2Kg crude drug;
3) concentrate back adding ethanol sedimentation and go out insolubles, filter;
4) macroporous resin purification: filtrating is through resin column, and it is colourless to be washed till effluent with purified water, and using concentration of volume percent then is that 50%～70% ethanolic soln carries out wash-out, collects elutriant, concentrates, until obtaining dry matter sample; Resin: sample quality is than being 1:8～12;
5) polyamide resin chromatography: the aqueous solution that sample ligand is set to 10%～20% mass percent concentration is crossed polyamide column, collects the post flow liquid, and with water wash to there not being sweet taste, merge post flow liquid and water elution liquid, concentrate, drying must bullion;
6) crystallization-recrystallization: add solvent in the bullion, place 75～85 ℃ of water-baths to be heated to whole dissolvings, filtered while hot, placement is separated out, filters, recrystallization again, spraying drying obtains sweet tea glycosides elaboration.
2. according to the process of claim 1 wherein that when adopting reflux 3 times in the step 1), extracting solution is as extracting the water use the following batch first time for the third time.
3. according to the method for claim 1, when adopting the hot water lixiviate, extraction time is 60min for the first time; Each extraction time of hot water lixiviate afterwards is 30min.
4. according to the method for claim 1, each extraction time is 6min in the normal pressure supersound extraction.
5. according to the process of claim 1 wherein that macroporous resin is the D-101 macroporous resin in the step 4).
6. according to the method for claim 1 or 5, collect 2～3 times of column volume elutriants in the said step 4).
7. according to the process of claim 1 wherein that the polyamide resin specification in the step 5) is 100～200 orders.
8. according to the process of claim 1 wherein that the solvent of crystallization-recrystallization in the step 6) is one or more in methyl alcohol, ethanol, acetone, ETHYLE ACETATE, chloroform or the sherwood oil.
9. according to the process of claim 1 wherein crystallization-recrystallization temperature scope in the step 6): 60～80 ℃.
10. place 80 ℃ of water-bath heating for dissolving according to the process of claim 1 wherein in the step 6).
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210302985.4A CN102838644B (en) | 2012-08-23 | 2012-08-23 | Production method for extracting sweet tea glucoside from sweet tea leaves |
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| CN104193788A (en) * | 2014-09-05 | 2014-12-10 | 广西大学 | Extraction method of rubusoside |
| CN104262427A (en) * | 2014-09-30 | 2015-01-07 | 桂林三宝药业有限公司 | Method for extracting rubusoside from sweet tea leaves |
| CN104370981A (en) * | 2014-09-30 | 2015-02-25 | 桂林市一峰食品有限公司 | Method for extraction of rubusoside from sweet tea |
| CN104926892A (en) * | 2015-06-04 | 2015-09-23 | 广西大学 | Method for extracting rubusoside from sweet tea |
| CN105061526A (en) * | 2015-07-23 | 2015-11-18 | 湖南华诚生物资源有限公司 | Extraction method for high purity rubusoside |
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| CN107556350A (en) * | 2017-10-12 | 2018-01-09 | 江南大学 | Rubusoside crystal, its preparation method, food compositions and application with crystal formation A forms |
| CN107915768A (en) * | 2017-12-14 | 2018-04-17 | 中南大学 | A kind of method of separating-purifying suberone in old leaf from Sweet tea |
| CN109717445A (en) * | 2019-01-30 | 2019-05-07 | 湖南绿蔓生物科技股份有限公司 | Sweetener composition and its preparation method and application |
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| CN113429444A (en) * | 2021-04-25 | 2021-09-24 | 杭州天草科技有限公司 | Method for separating and purifying rubusoside from stevia rebaudiana mother liquor sugar |
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