CN102838644B - Production method for extracting sweet tea glucoside from sweet tea leaves - Google Patents
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- 235000009508 confectionery Nutrition 0.000 title claims abstract description 30
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- 238000004519 manufacturing process Methods 0.000 title claims abstract description 16
- 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 19
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- 238000000605 extraction Methods 0.000 claims description 28
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- YWPVROCHNBYFTP-OSHKXICASA-N rubusoside Chemical compound O([C@]12C(=C)C[C@@]3(C1)CC[C@@H]1[C@@](C)(CCC[C@]1([C@@H]3CC2)C)C(=O)O[C@H]1[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O1)O)[C@@H]1O[C@H](CO)[C@@H](O)[C@H](O)[C@H]1O YWPVROCHNBYFTP-OSHKXICASA-N 0.000 claims description 24
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- HELXLJCILKEWJH-NCGAPWICSA-N rebaudioside A Chemical compound O([C@H]1[C@H](O)[C@@H](CO)O[C@H]([C@@H]1O[C@H]1[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O1)O)O[C@]12C(=C)C[C@@]3(C1)CC[C@@H]1[C@@](C)(CCC[C@]1([C@@H]3CC2)C)C(=O)O[C@H]1[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O1)O)[C@@H]1O[C@H](CO)[C@@H](O)[C@H](O)[C@H]1O HELXLJCILKEWJH-NCGAPWICSA-N 0.000 description 1
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- IKGXIBQEEMLURG-NVPNHPEKSA-N rutin Chemical compound O[C@@H]1[C@H](O)[C@@H](O)[C@H](C)O[C@H]1OC[C@@H]1[C@@H](O)[C@H](O)[C@@H](O)[C@H](OC=2C(C3=C(O)C=C(O)C=C3OC=2C=2C=C(O)C(O)=CC=2)=O)O1 IKGXIBQEEMLURG-NVPNHPEKSA-N 0.000 description 1
- QFVOYBUQQBFCRH-VQSWZGCSSA-N steviol Chemical compound C([C@@]1(O)C(=C)C[C@@]2(C1)CC1)C[C@H]2[C@@]2(C)[C@H]1[C@](C)(C(O)=O)CCC2 QFVOYBUQQBFCRH-VQSWZGCSSA-N 0.000 description 1
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Landscapes
- Saccharide Compounds (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
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 production method extracting Rubusoside from sweet tea.
Background technology
Sweet tea is the Rosaceae perennial rattan wood, is Guangxi distinctive a kind of nontoxic, low calorie, high sugariness and the wild rare sweet-tasting plant with nourishing function, the counties and cities such as the Yao Shan of main product in Guangxi, Jin Xiu, Yongfu and Cenxi.Because its taste is sweet, therefore named sweet tea.With Grosvenor Momordica, sweet Stevia be called the large sweet-tasting plant in Guangxi three, among the people in Guangxi have long applicating history, and local people are always when tea-drinking use for a long time, is also used for generation sugar processed food, also can be used as medicine.
The main component of sweet tea has Rubusoside, Vitamin P complex, tea-polyphenol, amino acid, inorganic salt etc.
The main sweet ingredient of sweet tea is Rubusoside, is the tetracyclic diterpene glycosides that steviol and glucose are combined into, molecular formula C
20h
50o
13, similar to stevioside glycosides (stevioside) in chemical structure.The sugariness of Rubusoside is about 300 times of sweetness of cane sugar, and calorific value is only 5% of sucrose.Through pharmacological evaluation, Rubusoside have 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 have high sugariness, low-calorie characteristic, not only can be used as medicinal, or a kind of colory foodstuff additive, can replace sucrose to be used in the food of the patients such as hypertension, diabetes, obesity and the elderly and children, healthcare products and medicine.
The aspects such as the domestic and international separation and Extraction to Rubusoside, test and pharmacology are studied, also report is had to the Rubusoside extracting higher degree on a small scale, but the Rubusoside suitability for industrialized production of high-content have not been reported, and in extraction and isolation process, adopt a large amount of toxic reagents to carry out separation and purification, being applied to food aspect to Rubusoside has obvious restriction.This illustrates, existing technical study is still in the junior stage, and really cannot reach industrialized production machine marketing level.For this reason, we take sweet tea as raw material, adopt the means such as macroporous resin separation and purification, column chromatography, crystallization and recrystallization to prepare Rubusoside sterling on a large scale, add as foodstuff additive, be widely used in the protective foods of the patients such as obesity, hypertension, diabetes and heart trouble.
Summary of the invention
The object of this invention is to provide a kind of cost low, simple to operate, loss of material is few, with short production cycle, and product yield is high, and low toxic and environment-friendly is suitable for industrialized production, the preparation method of high, the pure Rubusoside sterling of products obtained therefrom purity.
The technical solution used in the present invention comprises the following steps:
1) bulk drug extracts
Be raw material with sweet tea, add water after fragmentation, by heating and refluxing extraction 2 ~ 3 times or normal pressure ultrasonic extraction; During heating and refluxing extraction, Extracting temperature 60 ~ 80 DEG C, first time hot water extraction, the volumetric usage of water is 8 ~ 12 times of raw material, extraction time 50 ~ 70min, in each hot water extraction afterwards, volume of water consumption is 0.7 ~ 1 times of raw material, extraction time 20 ~ 40min; When adopting normal pressure supersound extraction, ultrasonic power output 250 ~ 350W, temperature 60 ~ 80 DEG C, water consumption is at least 10 times of raw material, at least extracts 2 times, each extraction time 5 ~ 8min;
2) said extracted liquid concentrating under reduced pressure is merged; Concentrated condition: vacuum ranges 0.7 ~ 1MPa, temperature is not higher than 90 DEG C, and concentrated material liquid volume is to 1:1 ~ 3; Finally be concentrated into often liter containing 0.8 ~ 1.2Kg crude drug;
3) add alcohol settling after concentrating and go out insolubles, filter;
4) macroporous resin purification: filtrate by resin column, is washed till effluent liquid with purified water (i.e. distilled water) colourless, be then that 50% ~ 70% ethanolic soln carries out wash-out with concentration of volume percent, collection elutriant, concentrates, until obtain dry matter sample; Resin: sample quality is than being 1:8 ~ 12;
5) polyamide resin chromatography: aqueous solution sample being configured to 10% ~ 20% mass percent concentration crosses polyamide column, collects post flow liquid, and with water wash to without sweet taste, merges post flow liquid and water elution liquid, concentrated, dry, obtains crude product;
6) crystallization-recrystallization: add solvent in crude product, is placed in 75 ~ 85 DEG C of water-baths and is heated to whole dissolving, filtered while hot, places and separates out, and filters, then recrystallization, and spraying dry, obtains Rubusoside fine work.
Of the present inventionly also can to process in the following ways, when namely wherein adopting reflux 3 times in step 1), third time extracting solution extract water as lower batch of first time and use.
When the present invention adopts hot water extraction, particularly preferably being extraction time first time is 60min; Each extraction time of hot water extraction is afterwards 30min.In normal pressure supersound extraction, each extraction time is 6min.
Macroporous resin in the present invention in step 4) particularly preferably is D-101 macroporous resin.
2 ~ 3 times of column volume elutriants are collected in described step 4).
Polyamide resin specification in step 5) of the present invention is 100 ~ 200 orders.
In step 6) of the present invention the solvent of crystallization-recrystallization comprise methyl alcohol, ethanol, acetone, ethyl acetate, chloroform or sherwood oil one or more.
Crystallization in step 6 of the present invention-recrystallization temperature scope: be advisable for 60 ~ 80 DEG C.Particularly preferably crude product is placed in 80 DEG C of water-bath heating for dissolving.
The present invention is by by the sweet tea after dried, pulverize and sieve, hot water return extract or ultrasonic-assisted extraction, come, concentrating under reduced pressure, alcohol settling impurity, then with resin absorption, ethanol elution, elutriant is concentrated, cross polyamide resin chromatography, concentrate, crystallization and recrystallization obtain the Rubusoside sterling that purity is not less than 98%.There is relative to prior art the advantage of following technique effect:
1) material equipment cost advantage: the raw material used in the inventive method, equipment are common common raw material, equipment, to avoid in commercial process for expensive raw materials, dependence together, greatly reduces production cost.
2) on extracting mode, adopt hot water extraction's refluxing extraction or ultrasonic extraction, effectively can improve product yield, the leaching being conducive to activeconstituents be separated, be conducive to the phenomenon of bubbling and running material in production control process simultaneously.Adopt extracting solution solvent cover formulation, reduce solvent consumption.
3) extracting solution adds ethanolic soln and is settled out insolubles, effectively by insolubles removings such as amino acid, can improve product purity.
4) in the present invention, what adopt is non-polar macroporous resin, because this resin has sizable specific surface area and suitable aperture, has special selectivity to glycoside material, by the Flavonoid substances in sweet tea, phenolic substance, amino acid etc. separately, product purity can be ensure that; Additionally use polyamide resin chromatography in the present invention, further separation and purification Rubusoside, its lock out operation is simple, easy to control.
5) technological line of low toxic and environment-friendly economical and efficient: the technological line of a kind of environmental protection economy that what the present invention taked is, the extraction adopted in this technological line, concentrated, the production units such as purification devices all can adopt airtight system, in the process of operation, can operator be avoided to greatest extent to touch reagent, effectively ensure the health of human body.The solvent adopted in the method, resin etc. can recycle, and can reduce loss of material, carry high product yield.This technological line echoes mutually in the pattern of China's Sustainable development, has good social benefit.
6) produce market advantage: the present invention passes through the assurance of several key technology parameters in whole technique and provides, and the purity of the Rubusoside of present invention process gained can be made to be not less than 98%, is pure white crystallization, is high-content high-quality sweet tea extract; And energy industrialized mass production, become the sweet tea extract product that added value of product is in the market the highest, meet the needs of problems of market to high-quality Rubusoside product.
7) drive agriculture industrialization, the large-scale development of the sweet tea of China, improve farmers' income; Improve the added value of sweet tea extract, promote plant milk extract industry development; Meet downstream industry to high-content high-quality Rubusoside demand, promote the common development of every profession and trade, and be the economic benefit and social benefit that social creativity is good.
Accompanying drawing explanation
Fig. 1 is concrete process flow sheet of the present invention.
Embodiment
Below, the present invention will be further described by embodiment, but it is not limited to any one or similar example of these examples.
Embodiment 1
Get sweet tea 500Kg (content is 5.2% after testing), 40 mesh sieves are crossed after broken, drop in extractor, add distilled water 5000L, be heated to 80 DEG C, refluxing extraction 60min, suction filtration while hot, respectively adds 4000L distilled water again and carries out second time, third time extraction, reflux 30min/ time with under condition in the dregs of a decoction, merge first time, for the second time extracting solution and be concentrated into 500L, lower batch of first time of third time extracting solution work extracts and does water use.Concentrated solution adds 350L alcohol settling and goes out insolubles, and filter, filtrate adds in the good 50KgD101 resin column of pre-treatment, flow velocity 5BV/h, after upper prop, be washed till effluent liquid with purified water colourless, finally use 70% ethanol elution, flow velocity 1BV/h, collects this elutriant of 150L, is concentrated into dry.Sample is configured to the aqueous solution of 20% concentration, crosses polyamide column, collect post flow liquid, and with distilled water drip washing to without sweet taste, merge post flow liquid and water elution liquid, be concentrated into dry, obtain crude product Rubusoside (content 81.2%).Add methyl alcohol, be placed in 80 DEG C of water-bath reflux to all dissolving, suction filtration while hot, placement washes out, the crystallisate of filtration, then carries out recrystallization, and spraying dry obtains pure white crystal 18.65Kg, after testing, and Shimadzu high performance liquid chromatograph, chromatographic column C
18(4.6mm × 250mm, 5um), moving phase is methyl alcohol: water=80:20; Determined wavelength is 210nm; Flow velocity is 1mL/min; Sample size is that below 10uL(implementation issue is same), purity is 98.15%, yield 3.73%, and the rate of recovery of whole process Rubusoside reaches 70.4%.
Embodiment 2
Get sweet tea 500Kg(after testing content be 5.4%), drop into after being crushed to 40 orders in ultrasonic extraction tank, add 5000L distilled water, ultrasonic power output 800W, 80 DEG C of supersound extraction 6min, filter, again add 4000L distilled water in the dregs of a decoction and carry out second time, third time extraction, after extracting 6min under condition, merge first time, second time extracting solution is concentrated into 500L, extracting solution does down batch first time and does water treatment for the third time.Concentrated solution adds 350L alcohol settling and goes out insolubles, and filter, filtrate adds in the good 50KgD101 resin column of pre-treatment, flow velocity 5BV/h, after upper prop, be washed till effluent liquid with purified water colourless, finally use 70% ethanol elution, flow velocity 1BV/h, collects this elutriant of 150L, is concentrated into dry.Sample is configured to the aqueous solution of 20% concentration, crosses polyamide column, collect post flow liquid, and with distilled water drip washing to without sweet taste, merge post flow liquid and water elution liquid, be concentrated into dry, obtain crude product Rubusoside (content 81.2%).Add methyl alcohol, be placed in 80 DEG C of water-bath reflux to all dissolving, suction filtration while hot, placement washes out, the crystallisate filtered, then carry out recrystallization, spraying dry obtains pure white crystal 19.48Kg, after testing, purity is 98.24%, yield 3.90%, and the rate of recovery of whole process Rubusoside reaches 70.95%.
Claims (2)
1. from sweet tea, extract a production method for Rubusoside, it is characterized in that, comprise the following steps:
1) bulk drug extracts
Be raw material with sweet tea, add water after fragmentation, by heating and refluxing extraction 3 times or normal pressure ultrasonic extraction; During heating and refluxing extraction, Extracting temperature 60 ~ 80 DEG C, first time hot water extraction, the volumetric usage of water is 8 ~ 12 times of raw material, extraction time 50 ~ 70min, in each hot water extraction afterwards, volume of water consumption is 0.7 ~ 1 times of raw material, extraction time 20 ~ 40min; When adopting normal pressure supersound extraction, ultrasonic power output 250 ~ 350W, temperature 60 ~ 80 DEG C, water consumption is at least 10 times of raw material, at least extracts 2 times, each extraction time 5 ~ 8min;
2) said extracted liquid concentrating under reduced pressure is merged; Concentrated condition: vacuum ranges 0.7 ~ 1MPa, temperature is not higher than 90 DEG C, and concentrated material liquid volume is to 1:1 ~ 3; Finally be concentrated into often liter containing 0.8 ~ 1.2Kg crude drug;
3) add alcohol settling after concentrating and go out insolubles, filter;
4) macroporous resin purification: filtrate by resin column, is washed till effluent liquid with purified water colourless, is then that 50% ~ 70% ethanolic soln carries out wash-out with concentration of volume percent, collects elutriant, concentrate, until obtain dry matter sample; Resin: sample quality is than being 1:8 ~ 12;
5) polyamide resin chromatography: aqueous solution sample being configured to 10% ~ 20% mass percent concentration crosses polyamide column, collects post flow liquid, and with water wash to without sweet taste, merges post flow liquid and water elution liquid, concentrated, dry, obtains crude product;
6) crystallization-recrystallization: add solvent in crude product, is placed in 75 ~ 85 DEG C of water-baths and is heated to whole dissolving, filtered while hot, places and separates out, and filters, then recrystallization, and spraying dry, obtains Rubusoside fine work;
When wherein adopting reflux 3 times in step 1), third time extracting solution extract water as lower batch of first time and use;
Wherein in step 4), macroporous resin is D-101 macroporous resin; 2 ~ 3 times of column volume elutriants are collected in described step 4);
Wherein in step 5), polyamide resin specification is 100 ~ 200 orders.
2. method according to claim 1, when adopting hot water extraction, extraction time first time is 60min; Each extraction time of hot water extraction is afterwards 30min; In normal pressure supersound extraction, each extraction time is 6min.
3. method according to claim 1, wherein in step 6), the solvent of crystallization-recrystallization is one or more in methyl alcohol, ethanol, acetone, ethyl acetate, chloroform or sherwood oil.
Priority Applications (1)
| 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 |
Applications Claiming Priority (1)
| 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 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102838644A CN102838644A (en) | 2012-12-26 |
| CN102838644B true CN102838644B (en) | 2015-06-03 |
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| 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 |
| CN104926892A (en) * | 2015-06-04 | 2015-09-23 | 广西大学 | Method for extracting rubusoside from sweet tea |
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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 |
| CN107915768B (en) * | 2017-12-14 | 2021-05-04 | 中南大学 | Method for separating and purifying friedelin from old sweet tea leaves |
| 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 |
| CN110615819B (en) * | 2019-10-10 | 2020-11-06 | 合肥极世茗香生物科技有限公司 | Method for rapidly extracting rubusoside |
| CN113429444B (en) * | 2021-04-25 | 2022-08-09 | 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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