CN109180755A - A method of extracting Rubusoside from sweet tea - Google Patents

A method of extracting Rubusoside from sweet tea Download PDF

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Publication number
CN109180755A
CN109180755A CN201811102849.4A CN201811102849A CN109180755A CN 109180755 A CN109180755 A CN 109180755A CN 201811102849 A CN201811102849 A CN 201811102849A CN 109180755 A CN109180755 A CN 109180755A
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sweet tea
rubusoside
reduced pressure
organic solvent
nanofiltration
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肖玉林
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Hubei Zhilin Agricultural Science And Technology Development Co Ltd
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Hubei Zhilin Agricultural Science And Technology Development Co Ltd
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    • C07ORGANIC CHEMISTRY
    • C07HSUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
    • C07H1/00Processes for the preparation of sugar derivatives
    • C07H1/06Separation; Purification
    • C07H1/08Separation; Purification from natural products
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07HSUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
    • C07H15/00Compounds containing hydrocarbon or substituted hydrocarbon radicals directly attached to hetero atoms of saccharide radicals
    • C07H15/20Carbocyclic rings
    • C07H15/24Condensed ring systems having three or more rings
    • C07H15/256Polyterpene radicals

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Abstract

A method of extracting Rubusoside from sweet tea, comprising the following steps: (1) sweet tea is crushed, be sieved, add water, Continuous Countercurrent Extraction, filtering;(2) enzyme preparation enzymatic hydrolysis is added, inactivates, it is cooling, it flocculates, filter residue is washed in filtering;(3) ultrafiltration, nanofiltration;(4) macroporous adsorption resin chromatography column adsorbs on, and washing, water lotion discards, organic solvent gradient elution, is concentrated under reduced pressure;(5) alumina chromatographic column adsorbs on, washes, and is concentrated under reduced pressure;(6) active carbon is added, stirs, filters, is concentrated under reduced pressure, spray drying;(7) organic solvent dissolves, and filters, and crystallizes, and filters, and is dried in vacuo, and crushes, obtains Sweet tea glycoside product.The extracted Sweet tea glycoside product of the method for the present invention is in pure white, purity >=99%, yield >=90.5%;The method of the present invention operating procedure is simple, and extraction time is short, energy consumption, at low cost, it can be achieved that continuous large-scale production.

Description

A method of extracting Rubusoside from sweet tea
Technical field
The present invention relates to a kind of methods for extracting Rubusoside, and in particular to a kind of side that Rubusoside is extracted from sweet tea Method.
Background technique
Sweet tea is the perennial machaka of rose family rubus, and main product is in the big precious jade area in Guangxi, main medicinal part Sweet tea, sweet tea main component are Rubusoside, sweet tea tannins, flavones and chlorophyll etc..
Rubusoside is a kind of high sugariness, natural sweetener low in calories, and sugariness is about 300 times of sucrose, and heat is only It is the 1% of sucrose, therefore, is suitable for diabetes, obesity and hyperlipemic patients, and be widely used in food, beverage etc., gathers around There is huge market value.But due to containing a large amount of sweet tea tannins and flavones in sweet tea, during isolating and purifying very Hardly possible is thoroughly removed, and thus will affect the quality of Sweet tea glucoside extract, being mainly manifested in Sweet tea glucoside extract has bitter taste and face Color is deeper.
Currently, the usual processing route of separating and purifying high-purity Sweet tea glycoside product is: extraction → filtering → macroporous absorption tree Rouge purifying → ion-exchange resin decolorization → crystallization and recrystallization, still, the technique is since flavones and polyphenol are easily by macroporous absorption Resin adsorption causes Rubusoside purification purity not high, while color is also relatively deep, and spent ion exchange resin decolourizes again, place Reason amount is smaller, and pigment processing is not thorough, and causes production cost higher.
CN102702284A discloses a kind of production technology of high-purity Rubusoside, be by sweet tea extracting in boiling water 3 times, Extracting solution is concentrated again, is flocculated and is clarified with water soluble chitosan, liquid centrifugal filtration of flocculating, with Macroporous Adsorption Resin, stripping liquid After having recycled ethyl alcohol, spent ion exchange resin decoloration, then taken off with desalination resin desalination finally with a kind of decoloration of composite decoloring agent The concentration of color liquid, spray drying obtain Rubusoside content >=98% product.Although this method can get 98% or more product of Rubusoside, It is, it cannot although the part macromolecular substances in extracting solution, such as protein and tannin can be removed with flocculate with chitosan Remove sweet tea tannins and flavones, cause purification with macroreticular resin effect poor, color is deeper, so as to cause subsequent ion exchange Resin decolorization effect is poor.
CN104193788A discloses a kind of extracting method of Rubusoside, and basic step is: extraction → filtering → concentration → Centrifugation → decolourize removes astringent taste, removal of impurities → drying, wherein decolourizing, remove astringent taste, cleaning is to pass sequentially through macroporous absorbent resin, ion exchange Resin, polyamide are realized.But this method is not only complex for operation step, and the purity of gained Rubusoside is relatively low.
CN101003552A discloses a kind of preparation method of high-purity Rubusoside, and basic step is: refluxing extraction → tree Rouge absorption → elution → column chromatographs removal of impurities → drying → ethyl alcohol dissolution → filtering → crystallization, wherein with macroporous resin adsorption, with gathering Amide, aluminium oxide or ion exchange resin carry out column chromatography removal of impurities.But this method only merely with polyamide, aluminium oxide or from One of sub-exchange resin mode carries out column chromatography removal of impurities, and treating capacity is smaller, and impurity removal is not thorough.
CN104262425A discloses a kind of new method for extracting Rubusoside, and basic technology is: raw material crushing → solvent mentions → film is concentrated → is taken to adjust pH value → macroporous resin purification → soda acid processing → elution → combination ion exchange resin chromatography → concentration → crystallization → drying.It is however a drawback of the method that after purification with macroreticular resin, then handled with soda acid, to water consumption requirement It is larger, and with combination ion exchange resin chromatographic decolorization, treating capacity is smaller.
CN102838644A discloses a kind of production method that Rubusoside is extracted from sweet tea, and process flow is: former Material is broken → and solvent extraction → concentration → ethanol precipitation → macroporous resin purification → concentration → polyamide chromatography → concentration → Crystallization and recrystallization → drying.It is however a drawback of the method that: using the mode of water extract-alcohol precipitation, although partial impurities can be removed, Such as protein, but depigmentation cannot be removed, and higher cost, the cost decolourized using polyamide is also higher.
CN105294790A discloses a kind of method that high-purity steviosides are extracted from STEVIA REBAUDIANA, and process flow is: Immersion → enzymatic hydrolysis → extraction → flocculation → macroreticular resin decoloration → silica gel column chromatography.It is however a drawback of the method that: use silica gel Organic solvent amount used in column chromatography is big, complicated for operation, and industrialization large-scale production is difficult.
CN106632540A discloses a kind of method of the extraction of Rubusoside, and basic technology is: Sweet tea crushes → digest water Propose → microwave alcohol extracting → macroporous resin column chromatography → polyamide column purification.It is however a drawback of the method that: extraction process is multiple Miscellaneous, more demanding to equipment and operation, the rate of recovery is relatively low.
CN105061526A discloses a kind of method of the extraction of high-purity Rubusoside, basic technology: pre-treatment-microwave is inverse Flow extraction-macroporous resin adsorption separation-Ultrafiltration-Concentration-crystallization and recrystallization.It is however a drawback of the method that: macroporous absorption point It is isolated and purified from rear gained Sweet tea crude extract without decoloration, product crystallization color is deeper, and yield is lower, quality stability Difference.
Summary of the invention
The technical problem to be solved by the present invention is to overcome drawbacks described above of the existing technology, provide a kind of gained production Quality is stablized, and purity, high income, operating procedure is simple, and extraction time is short, energy consumption, at low cost, it can be achieved that continuous extensive raw The method of Rubusoside is extracted in the slave sweet tea produced.
The technical solution adopted by the present invention to solve the technical problems is as follows: a kind of side extracting Rubusoside from sweet tea Method, comprising the following steps:
(1) it crushes, extract: sweet tea is crushed, be sieved, add water, carry out Continuous Countercurrent Extraction, filtering obtains extracting solution;
(2) it digests, flocculate: enzyme preparation is added in the extracting solution obtained by step (1), is digested, enzymolysis liquid inactivation, cooling, wadding Solidifying, filtering washes filter residue to no sweet taste, obtains flocculation liquid;
(3) ultrafiltration, nanofiltration: flocculation liquid obtained by step (2) is subjected to ultrafiltration, nanofiltration obtains nanofiltration retentate fluid;
(4) macroporous absorbent resin adsorbs: macroporous adsorption resin chromatography column in nanofiltration retentate fluid obtained by step (3) being adsorbed, washing To no sweet taste, water lotion is discarded, then with organic solvent gradient elution, is concentrated under reduced pressure, is obtained concentrate;
(5) aluminium oxide refines: alumina chromatographic column on concentrate obtained by step (4) being adsorbed, efflux is collected, is washed to no sweet tea Taste collects water lotion, and efflux and water lotion are concentrated under reduced pressure, and obtains concentrate;
(6) it takes away the puckery taste, de- hardship: in the concentrate obtained by step (5), active carbon is added, stirs, filters, is concentrated under reduced pressure, it is spraying dry It is dry, obtain Rubusoside crude product;
(7) it crystallizes: Rubusoside crude product obtained by step (6) being dissolved with organic solvent, filters, crystallizes, filter, vacuum drying, powder It is broken, obtain Sweet tea glycoside product.
Preferably, in step (1), the mass content of the Rubusoside in Rubus suavissimus S. Lee by HPLC is 3~6%.
Preferably, in step (1), the mesh number of the sieving is 10~50 mesh.
Preferably, in step (1), total dosage of the water is 5~30 times (more preferable 10~25 times) of Sweet tea leaf quality.
Preferably, in step (1), the temperature of the Continuous Countercurrent Extraction is 80~100 DEG C, and the time extracted every time is 1 ~4h, number >=1 time of extraction.Since Rubusoside is highly soluble in hot water, extraction time is short, and leaching rate is high, so using hot water As Extraction solvent, not only save the cost, but also safety and environmental protection, and it can guarantee continuous industrial production using adverse current extraction.
Preferably, in step (1), with 100~300 mesh filter-cloth filterings.
Preferably, in step (2), the additive amount of the enzyme preparation is 0.01~0.5%(more preferable 0.1 of extracting solution quality ~0.3%).Due to that also can extract together part aqueous fiber and protein while hot water extracts sweet tea, if obstructed Enzymatic hydrolysis is crossed, it is poor to will lead to subsequent membrane separating and purifying effect.
Preferably, in step (2), the enzyme preparation be cellulase preparation, hemicellulase preparations, pectase preparation or One or more of protease preparation etc..
Preferably, in step (2), the temperature of the enzymatic hydrolysis is 40~60 DEG C, pH value be 2.0~9.0(more preferable 4.0~ 7.0), the time is 1~2h.
Preferably, in step (2), the temperature of the inactivation is 90~120 DEG C, and the time is 30~60s, and pressure is normal pressure.
Preferably, described to be cooled to board-like be cooled to room temperature in step (2).
Preferably, in step (2), the flocculation is: flocculant being added in enzymolysis liquid and is flocculated, during addition It is stirred continuously, until pH value is 2~6, is stirred for 0.5~1.5h, stands 0.5~1.5h, then adjust pH value >=8, be stirred for 0.5 ~1.5h stands 1~4h.
Preferably, the flocculant is one or more of FeCl3, FeSO4 or AlCl3 etc..Containing big in sweet tea Polyphenol, flavones and the tannic acid of amount, and these impurity can be precipitated rapidly and being complexed with metal flocculant, to realize impurity Removal, reduce the pressure of subsequent purification.
Preferably, pH value >=8 are adjusted with saturated limewater.Limewash primarily serves the effect of drainage.
Preferably, in step (2), the filter type is plate compression, and filter sizes are 0.4~30 μm (more preferable 0.5 ~5.0 μm).
Preferably, in step (2), the water consumption for washing filter residue is 1~2 times of sweet tea material quality.
Preferably, in step (3), the ultrafiltration membrane for ultrafiltration is ceramic membrane, and aperture is 0.3~1.0 μm.Only due to filtering Most of solid impurity can be removed, and the smaller impurity of fraction partial size can be removed using ultrafiltration, keeps feed clarification bright.
Preferably, in step (3), the nanofiltration is that ultrafiltrate is first passed through to molecular cut off for 800~5000 dalton Nanofiltration membrane, water catches up with film to permeate without sweet taste, and permeate passes through the nanofiltration membrane that molecular cut off is 100~500 dalton again, Until water catches up with film to hundred benefit degree >=20% of trapped fluid, nanofiltration retentate fluid is obtained.Nanofiltration first passes through the big nanofiltration membrane of molecular cut off, Big molecular impurity and most of pigment can be removed and can remove small molecular weight impurity and desalination after the small nanofiltration membrane of molecular cut off.
Preferably, in step (4), the macroporous adsorption resin chromatography column is made of >=2 chromatographic columns, and nanofiltration retentate fluid is first Upper 1st chromatographic column, after its efflux is pleasantly sweet, the 2nd chromatographic column concatenated on efflux, while nanofiltration retentate fluid starts Upper 2nd chromatographic column, and so on, after the completion of upper prop, the 1st is connected in series to 1 chromatographic column of most end and is washed, washed Liquid discards, then carries out gradient elution to every chromatographic column respectively with organic solvent.When the efflux is pleasantly sweet, sweet tea in efflux Mass percent >=0.05% of tea glycosides.This upper prop mode advantage is: it both can ensure that every chromatographic column is attained by adsorption saturation, It to utilize resin to the greatest extent, and can guarantee the continuity of production, improve production efficiency, meanwhile, be connected in series progress The mode of washing improves Sweet tea so that can be adsorbed again in rear chromatographic column in the Rubusoside that preceding chromatographic column is washed away again The yield of glycosides.
Preferably, in step (4), the diameter height of the macroporous adsorption resin chromatography column than for 1:2~8(it is 1:4 more preferable~ 6).
Preferably, in step (4), the volume mass ratio (L/kg) of the macroporous absorbent resin and Sweet tea leaf raw material is 1:5 ~10.
Preferably, in step (4), the flow velocity of the upper prop is 1~4BV/h.
Preferably, in step (4), model D-101, AB-8, LX-T28, DM-130 or X- of the macroporous absorbent resin One or more of 5 etc..Under alkaline condition, Rubusoside is easily adsorbed by macroporous absorbent resin, and most of polyphenol and flavones It is then not easy to be adsorbed, to reach good purification effect.Macroporous resin adsorption is mainly used for being enriched with Rubusoside, but also has simultaneously A small amount of polyphenol and flavones are enriched with together, later by alumina chromatographic column, then can adsorb this part polyphenol and flavones, and Sweet tea Glycosides is not adsorbed, and is flowed out with efflux, to improve Rubusoside purity.
Preferably, in step (4), the flow velocity of the washing is 1.0~3.0BV/h.
Preferably, in step (4), the flow velocity of the organic solvent gradient elution is 0.5~2.0BV/h.
Preferably, in step (4), the gradient elution refers to: first with the organic solvent of 1~3BV volume fraction 10~30% Elution discards eluent, then is eluted with the organic solvent of more preferable 65~80%) 1~3BV volume fraction, 60~95%(, and collection is washed De- liquid.The biggish impurity of small part polarity mainly can remove using the organic solvent elution of volume fraction 10~30%, for example remain A small amount of polyphenol and flavones in resin etc., and then mainly elution is enriched on resin the organic solvent of volume fraction 60~95% Rubusoside, can make in product that Rubusoside purity is higher using gradient elution, and color is more shallow, and quality stability is more preferable.
Preferably, in step (4), the organic solvent is edible ethanol solution.
Preferably, in step (4), the temperature of the reduced pressure is 60~90 DEG C, and pressure is -0.09~-0.07MPa, Being concentrated under reduced pressure into solid content is 10~30%.
Preferably, in step (5), the flow velocity of the upper prop is 0.5~2.0BV/h.
Preferably, in step (5), the diameter height of the alumina chromatographic column compares for 1:2~8.
Preferably, in step (5), the volume mass ratio (L/kg) of the aluminium oxide and Sweet tea leaf raw material is 1:40~100 (more preferable 1:50~80).The effect of aluminium oxide is mainly remaining a small amount of coloured in adsorbing and removing macroporous absorbent resin eluent Substance, such as polyphenol and flavones;And aluminium oxide has decoloration at low cost compared with ion exchange resin or polyamide, and effect is good etc. Advantage.
Preferably, in step (5), the aluminium oxide is acidic alumina or neutral alumina.
Preferably, in step (5), the aluminium oxide is first activated using preceding: first by aluminium oxide at 500~600 DEG C Hot conditions under, activate 10~20h after, then with volume fraction be 85~98% ethanol solution clean it is colourless to efflux It is bright, and in addition to ethanol flavor without other smells until, be finally washed to no ethanol flavor.
Preferably, in step (5), the mesh number of the aluminium oxide is 80~300 mesh.
Preferably, in step (5), the flow velocity of the washing is 0.5~1.0BV/h.
Preferably, in step (5), the temperature of the reduced pressure is 60~90 DEG C, and pressure is -0.09~-0.07MPa, Being concentrated under reduced pressure into solid content is 40~60%.
Preferably, in step (6), the dosage of the active carbon is the 0.1~0.5% of concentrate quality.
Preferably, in step (6), the mesh number of the active carbon is 60~200 mesh.
Preferably, in step (6), the temperature of the stirring is 80~100 DEG C, and the time is 0.5~1.5h.
Preferably, in step (6), described be filtered into first uses plate compression, then uses ceramic membrane filter.
Preferably, the aperture of board-like filter membrane used in the plate compression is 0.4~30 μm (more preferable 0.5~5.0 μm), institute The aperture for stating ceramic membrane is 0.3~1.0 μm.
Preferably, in step (6), the temperature of the reduced pressure is 60~90 DEG C, and pressure is -0.09~-0.07MPa, Being concentrated under reduced pressure into solid content is 40~60%.
Preferably, in step (6), the inlet air temperature of the spray drying is 180~220 DEG C, and leaving air temp is 70~90 ℃。
Preferably, in step (7), the mass ratio of the Rubusoside crude product and organic solvent is the more preferable 1:6 of 1:5~15( ~10).
Preferably, in step (7), the volume fraction of the organic solvent is 60~95%.
Preferably, in step (7), the temperature of the dissolution is 60~90 DEG C.
Preferably, in step (7), the temperature of the crystallization is -5~10 DEG C, the time is 2~for 24 hours.
Preferably, in step (7), the organic solvent is one or more of methanol, ethyl alcohol, propyl alcohol or isopropanol.
Preferably, in step (7), the vacuum drying temperature be 60~90 DEG C, vacuum degree be -0.01~- 0.09MPa, the time be 2~for 24 hours.
The method of the present invention has the beneficial effect that:
(1) the extracted Sweet tea glycoside product of the method for the present invention is in pure white, purity >=99%, yield >=90.5%;
(2) the method for the present invention removes polyphenol, flavones and the tannin in Sweet tea extracting solution using flocculated mode after first digesting, and goes It is more at low cost than other way except significant effect;The method of the present invention is realized using ultrafiltration, nanofiltration to be isolated and purified and desalination bleaching, It is equally at low cost compared to traditional ion exchange resin desalination bleaching, simple process;Enzymatic hydrolysis+flocculated mode can remove most of Pigment, ultrafiltration+nanofiltration mode can remove most of impurity, after most of pigment and impurity all remove, then with macroporous absorption tree Rouge adsorbs the mode of Rubusoside, compared to the directly upper macroporous resin adsorption of extracting solution, not only large amount of adsorption, and macroporous resin adsorption Afterwards, product purity is higher, up to 90% or more, then is refined by way of aluminium oxide+active carbon, decolourizes, takes away the puckery taste, de- hardship, knot Crystalline substance, treating capacity is big, and effect is more preferable, and product quality is more stable;
(3) the method for the present invention operating procedure is simple, and extraction time is short, energy consumption, at low cost, it can be achieved that continuous large-scale production.
Specific embodiment
Below with reference to embodiment, the invention will be further described.
Sweet tea used in the embodiment of the present invention originates in Dayaoshan, Guangxi, and the mass content of Rubusoside is 4.5%;This hair Cellulase preparation used in bright embodiment, hemicellulase preparations, pectase preparation and protease preparation are purchased from Shandong Long Kete enzyme preparation Co., Ltd;NF8040-800D, NF8040-300D, NF8040- used in the embodiment of the present invention 5000D, NF8040-500D, NF8040-1000D type high molecular material organic nanofiltration membrane are purchased from Jiangsu my high-tech share long Co., Ltd;It is new to be purchased from Xi'an indigo plant dawn science and technology for D-101 type used in the embodiment of the present invention, AB-8 type macroporous absorbent resin Material limited liability company;X-5 type resin, is purchased from Tianjin Nankai Hecheng S&T Co., Ltd. used in the embodiment of the present invention; The used acidic alumina of the embodiment of the present invention, mesh number are 200 mesh, are purchased from Qingdao Marine Chemical Co., Ltd.;The present invention is implemented Ethanol solution used in example is food-grade;Active carbon used in the embodiment of the present invention is purchased from Tianjin Ke Miou chemical reagent Co., Ltd;Raw material and chemical reagent used in the embodiment of the present invention are obtained by routine business approach unless otherwise specified ?.
Reference example 1
Acidic alumina used in the embodiment of the present invention is first activated using preceding: first by acidic alumina at 550 DEG C Under hot conditions, activate 18h after, then with volume fraction be 95% ethanol solution clean it is colorless and transparent to efflux, and remove ethyl alcohol Taste it is outer without other smells until, be finally washed to no ethanol flavor.
Embodiment 1
(1) it crushes, extract: 5t sweet tea is crushed, cross 20 meshes, 50t water is added, at 85 DEG C, carry out Continuous Countercurrent Extraction 1h obtains 35t extracting solution with 100 mesh filter-cloth filterings;
(2) it digests, flocculate: 35kg cellulase preparation and 35kg protease system being added in the 35t extracting solution obtained by step (1) Agent under pH value is 5, carries out enzymatic hydrolysis 1h at 50 DEG C, and enzymolysis liquid is at 110 DEG C, under normal pressure, inactivates 60s, board-like to be cooled to room temperature, then FeCl3 is added in enzymolysis liquid and is flocculated, is stirred continuously during addition, until pH value is 3,0.8h is stirred for, stands 1.2h adjusts pH value to 8 with saturated limewater, is stirred for 1.2h, stands 1h, with filter sizes be 2.0 μm board-like filter membrane into Row plate compression, then with 6t water washes filter residue to no sweet taste, obtains 41t and flocculates liquid;
(3) ultrafiltration, nanofiltration: the ceramic membrane in 0.5 μm of aperture of the flocculation liquid of 41t obtained by step (2) is subjected to ultrafiltration, then ultrafiltrate The NF8040-800D type nanofiltration membrane that molecular cut off is 800 dalton is first passed through, water catches up with film to permeate without sweet taste, permeate It is again the NF8040-300D type nanofiltration membrane of 300 dalton by molecular cut off, water catches up with film to hundred benefit degree >=20% of trapped fluid Until, obtain 10t nanofiltration retentate fluid;
(4) macroporous absorbent resin adsorbs: macroporous adsorption resin chromatography column is by 2 D-101 type macroporous adsorption resin chromatographies (every, column The diameter height of chromatographic column compares for 1:6, and total resin volume is 700L) composition, first by 10t nanofiltration retentate fluid obtained by step (3) with flow velocity 2BV/h, upper 1st chromatographic column, after mass percent >=0.05% of Rubusoside in its efflux, concatenated on efflux the 2nd Root chromatographic column, while nanofiltration retentate fluid starts with flow velocity 2BV/h, upper 2nd chromatographic column, after the completion of upper prop, by the 1st and the 2nd Root chromatographic column is connected in series, and is washed to no sweet taste with flow velocity 2.5BV/h, and water lotion discards, then with 0.5BV/h flow velocity, first with total Volume 2100L(, that is, 3BV), volume fraction be 10% edible ethanol solution 2 chromatographic columns are eluted respectively, discard elution Liquid, then 2 chromatographic columns are eluted respectively with total volume 2100L(, that is, 3BV), the edible ethanol solution that volume fraction is 65%, Eluent is collected, at 70 DEG C, under -0.08MPa, being concentrated under reduced pressure into solid content is 15%, obtains 1.6t concentrate;
(5) aluminium oxide refines: by 1.6t concentrate obtained by step (4) with flow velocity 1.5BV/h, upper acidic alumina chromatographic column (diameter For height than being 1:3, aluminium oxide volume is 100L) it is adsorbed, efflux is collected, no sweet taste is washed to speed 1BV/h, collects water Washing lotion, efflux and water lotion are at 70 DEG C, and under -0.08MPa, being concentrated under reduced pressure into solid content is 50%, obtain 510.74kg concentrate;
(6) it takes away the puckery taste, de- hardship: in the 501.74kg concentrate obtained by step (5), the active carbon of addition 2.5kg, 80 mesh, 100 DEG C Under, 0.5h is stirred, then first carries out plate compression, then the ceramic membrane for being 1.0 μm with aperture with the board-like filter membrane that aperture is 2.0 μm It is filtered, at 60 DEG C, under -0.08MPa, being concentrated under reduced pressure into solid content is 40%, and concentrate is 180 DEG C in inlet air temperature, outlet air Temperature is to be spray-dried at 70 DEG C, obtain 250.87kg Rubusoside crude product;
(7) it crystallizes: by the methanol solution of 250.87kg Rubusoside crude product 2.5t volume fraction 85% obtained by step (6) at 80 DEG C Lower dissolution, filtering, then at 5 DEG C, 20h is crystallized, crystal is filtered, finally at 70 DEG C, under -0.09MPa, is dried in vacuo 20h, powder It is broken, obtain 205.68kg Sweet tea glycoside product.
Through detecting, gained Sweet tea glycoside product is pure white, purity 99.0%, yield 90.5%.
Embodiment 2
(1) it crushes, extract: 5t sweet tea is crushed, cross 30 meshes, 100t water is added, at 95 DEG C, carry out Continuous Countercurrent Extraction 3h obtains 95t extracting solution with 300 mesh filter-cloth filterings;
(2) it digests, flocculate: 47.5kg hemicellulase preparations and 47.5kg pectin being added in the 95t extracting solution obtained by step (1) Enzyme preparation under pH value is 4, carries out enzymatic hydrolysis 2h at 55 DEG C, and enzymolysis liquid is at 100 DEG C, under normal pressure, inactivates 40s, board-like to be cooled to often Temperature, then FeSO4 is added in enzymolysis liquid and is flocculated, it is stirred continuously during addition, until pH value is 5, is stirred for 1.2h, it is quiet 0.8h is set, pH value is adjusted to 9 with saturated limewater, is stirred for 0.8h, standing 3h, the board-like filter membrane for being 1.0 μm with filter sizes Plate compression is carried out, then uses 8t water, washing filter residue obtains 103t and flocculates liquid to no sweet taste;
(3) ultrafiltration, nanofiltration: the ceramic membrane in 0.5 μm of aperture of the flocculation liquid of 103t obtained by step (2) is subjected to ultrafiltration, then ultrafiltration Liquid first passes through the NF8040-5000D type nanofiltration membrane that molecular cut off is 5000 dalton, and water catches up with film to permeate without sweet taste, thoroughly Cross liquid pass through again molecular cut off be 500 dalton NF8040-500D type nanofiltration membrane, water catch up with film to trapped fluid hundred benefit degree >= Until 20%, 15t nanofiltration retentate fluid is obtained;
(4) macroporous absorbent resin adsorbs: macroporous adsorption resin chromatography column is by 3 AB-8 type macroporous adsorption resin chromatographies (every, column The diameter height of chromatographic column compares for 1:5, and total resin volume is 800L) composition, first by 15t nanofiltration retentate fluid obtained by step (3) with flow velocity 1.5BV/h, upper 1st chromatographic column concatenate on efflux after mass percent >=0.05% of Rubusoside in its efflux 2nd chromatographic column, while nanofiltration retentate fluid starts with flow velocity 1.5BV/h, upper 2nd chromatographic column, to Rubusoside in its efflux Mass percent >=0.05% after, the 3rd chromatographic column concatenated on efflux, while nanofiltration retentate fluid starts with flow velocity After the completion of upper prop, the 1st and the 3rd chromatographic column are connected in series for 1.5BV/h, upper 3rd chromatographic column, with flow velocity 2BV/h washing To no sweet taste, water lotion is discarded, then with 1.5BV/h flow velocity, is first 15% with total volume 2000L(, that is, 2.5BV), volume fraction Edible ethanol solution respectively elutes 3 chromatographic columns, discards eluent, then with total volume 2000L(, that is, 2.5BV), volume The edible ethanol solution that score is 75% respectively elutes 3 chromatographic columns, collects eluent, at 80 DEG C, under -0.09MPa, Being concentrated under reduced pressure into solid content is 13%, obtains 1.75t concentrate;
(5) aluminium oxide refines: by 1.75t concentrate obtained by step (4) with flow velocity 2BV/h, (diameter is high for upper acidic alumina chromatographic column Than for 1:5, aluminium oxide volume is 80L) it is adsorbed, efflux is collected, no sweet taste is washed to speed 1BV/h, collects washing Liquid, efflux and water lotion are at 80 DEG C, and under -0.09MPa, being concentrated under reduced pressure into solid content is 52%, obtain 431.08kg concentrate;
(6) it takes away the puckery taste, de- hardship: in the 431.08kg concentrate obtained by step (5), the active carbon of addition 1.5kg, 100 mesh, 80 DEG C Under, 1.5h is stirred, then first carries out plate compression, then the ceramic membrane for being 0.5 μm with aperture with the board-like filter membrane that aperture is 1.0 μm It is filtered, at 80 DEG C, under -0.09MPa, being concentrated under reduced pressure into solid content is 50%, and concentrate is 200 DEG C in inlet air temperature, outlet air Temperature is to be spray-dried at 80 DEG C, obtain 224.6kg Rubusoside crude product;
(7) it crystallizes: by the methanol solution of 224.6kg Rubusoside crude product 1.5t volume fraction 95% obtained by step (6) at 70 DEG C Dissolution, filtering, then at 5 DEG C, crystallization for 24 hours, filters crystal, finally at 70 DEG C, under -0.08MPa, is dried in vacuo 8h, crushes, obtain 206.3kg Sweet tea glycoside product.
Through detecting, gained Sweet tea glycoside product is pure white, purity 99.5%, yield 91.2%.
Embodiment 3
(1) it crushes, extract: 5t sweet tea is crushed, cross 40 meshes, 75t water is added, at 90 DEG C, carry out Continuous Countercurrent Extraction 2h obtains 70t extracting solution with 200 mesh filter-cloth filterings;
(2) it digests, flocculate: 35kg cellulase preparation, 35kg protease preparation being added in the 70t extracting solution obtained by step (1) Under pH value is 6, enzymatic hydrolysis 1.5h is carried out at 60 DEG C with 35kg pectase preparation, enzymolysis liquid is at 90 DEG C, under normal pressure, inactivates 50s, plate Formula is cooled to room temperature, then FeCl3 is added in enzymolysis liquid and is flocculated, and is stirred continuously during addition, until pH value is 4, then 0.5h is stirred, 0.5h is stood, pH value is adjusted to 9 with saturated limewater, is stirred for 0.5h, stands 2h, be 0.5 μm with filter sizes Board-like filter membrane carry out plate compression, then use 7t water, washing filter residue obtains 77t and flocculates liquid to no sweet taste;
(3) ultrafiltration, nanofiltration: the ceramic membrane in 1.0 μm of aperture of the flocculation liquid of 77t obtained by step (2) is subjected to ultrafiltration, then ultrafiltrate The NF8040-1000D type nanofiltration membrane that molecular cut off is 1000 dalton is first passed through, water catches up with film, without sweet taste, to penetrate to permeate Liquid pass through again molecular cut off be 500 dalton NF8040-500D type nanofiltration membrane, water catch up with film to trapped fluid hundred benefit degree >= Until 30%, 13t nanofiltration retentate fluid is obtained;
(4) macroporous absorbent resin adsorbs: macroporous adsorption resin chromatography column is by 3 X-5 type macroporous adsorption resin chromatography column (every root layers The diameter height of analysis column compares for 1:4, and total resin volume is 1000L) composition, first by 13t nanofiltration retentate fluid obtained by step (3) with flow velocity 1BV/h, upper 1st chromatographic column, after mass percent >=0.05% of Rubusoside in its efflux, concatenated on efflux the 2nd Root chromatographic column, while nanofiltration retentate fluid starts with flow velocity 1BV/h, upper 2nd chromatographic column, the quality to Rubusoside in its efflux After percentage >=0.05%, the 3rd chromatographic column concatenated on efflux, while nanofiltration retentate fluid starts with flow velocity 1BV/h, the upper 3rd Root chromatographic column after the completion of upper prop, the 1st and the 3rd chromatographic column is connected in series, are washed to no sweet taste, water with flow velocity 1.5BV/h Washing lotion discards, then with 1.0BV/h flow velocity, first with total volume 2000L(, that is, 2BV), the edible ethanol solution point that volume fraction is 20% It is other that 3 chromatographic columns are eluted, discard eluent, then with total volume 2000L(, that is, 2BV), the edible second that volume fraction is 70% Alcoholic solution respectively elutes 3 chromatographic columns, collects eluent, at 70 DEG C, under -0.08MPa, being concentrated under reduced pressure into solid content is 16%, obtain 1.55t concentrate;
(5) aluminium oxide refines: by 1.55t concentrate obtained by step (4) with flow velocity 1.0BV/h, upper acidic alumina chromatographic column (diameter For height than being 1:4, aluminium oxide volume is 90L) it is adsorbed, efflux is collected, no sweet taste is washed to speed 0.5BV/h, is collected Water lotion, efflux and water lotion are at 70 DEG C, and under -0.08MPa, being concentrated under reduced pressure into solid content is 50%, obtain 468.63kg concentration Liquid;
(6) it takes away the puckery taste, de- hardship: in the 468.63kg concentrate obtained by step (5), being added the active carbon of 2.3kg, 60 mesh, at 90 DEG C, 1h is stirred, then first carries out plate compression with the board-like filter membrane that aperture is 0.5 μm, then carried out with the ceramic membrane that aperture is 0.3 μm Filtering, at 70 DEG C, under -0.08MPa, being concentrated under reduced pressure into solid content is 45%, and concentrate is 180 DEG C in inlet air temperature, leaving air temp To be spray-dried at 70 DEG C, 234.31kg Rubusoside crude product is obtained;
(7) it crystallizes: by the ethanol solution of 234.31kg Rubusoside crude product 2.0t volume fraction 90% obtained by step (6) at 90 DEG C Lower dissolution, filtering, then at 0 DEG C, 12h is crystallized, crystal is filtered, finally at 80 DEG C, under -0.09MPa, is dried in vacuo 12h, powder It is broken, obtain 208.54kg Sweet tea glycoside product.
Through detecting, gained Sweet tea glycoside product is pure white, purity 99.8%, yield 92.5%.

Claims (9)

1. a kind of method for extracting Rubusoside from sweet tea, which comprises the following steps:
(1) it crushes, extract: sweet tea is crushed, be sieved, add water, carry out Continuous Countercurrent Extraction, filtering obtains extracting solution;
(2) it digests, flocculate: enzyme preparation is added in the extracting solution obtained by step (1), is digested, enzymolysis liquid inactivation, cooling, wadding Solidifying, filtering washes filter residue to no sweet taste, obtains flocculation liquid;
(3) ultrafiltration, nanofiltration: flocculation liquid obtained by step (2) is subjected to ultrafiltration, nanofiltration obtains nanofiltration retentate fluid;
(4) macroporous absorbent resin adsorbs: macroporous adsorption resin chromatography column in nanofiltration retentate fluid obtained by step (3) being adsorbed, washing To no sweet taste, water lotion is discarded, then with organic solvent gradient elution, is concentrated under reduced pressure, is obtained concentrate;
(5) aluminium oxide refines: alumina chromatographic column on concentrate obtained by step (4) being adsorbed, efflux is collected, is washed to no sweet tea Taste collects water lotion, and efflux and water lotion are concentrated under reduced pressure, and obtains concentrate;
(6) it takes away the puckery taste, de- hardship: in the concentrate obtained by step (5), active carbon is added, stirs, filters, is concentrated under reduced pressure, it is spraying dry It is dry, obtain Rubusoside crude product;
(7) it crystallizes: Rubusoside crude product obtained by step (6) being dissolved with organic solvent, filters, crystallizes, filter, vacuum drying, powder It is broken, obtain Sweet tea glycoside product.
2. the method for Rubusoside is extracted from sweet tea according to claim 1, it is characterised in that: in step (1), the mistake The mesh number of sieve is 10~50 mesh;Total dosage of the water is 5~30 times of Sweet tea leaf quality;The temperature of the Continuous Countercurrent Extraction It is 80~100 DEG C, the time extracted every time is 1~4h, number >=1 time of extraction;With 100~300 mesh filter-cloth filterings.
3. the method according to claim 1 or claim 2 for extracting Rubusoside from sweet tea, it is characterised in that: in step (2), institute The additive amount for stating enzyme preparation is the 0.01~0.5% of extracting solution quality;The enzyme preparation is cellulase preparation, hemicellulase One or more of preparation, pectase preparation or protease preparation;The temperature of the enzymatic hydrolysis is 40~60 DEG C, pH value 2.0 ~9.0, the time is 1~2h;The temperature of the inactivation is 90~120 DEG C, and the time is 30~60s, and pressure is normal pressure.
4. the method for Rubusoside is extracted described according to claim 1~one of 3 from sweet tea, it is characterised in that: step (2) In, the flocculation is: flocculant is added in enzymolysis liquid and is flocculated, is stirred continuously during addition, until pH value is 2~6, It is stirred for 0.5~1.5h, stands 0.5~1.5h, then adjusts pH value >=8, is stirred for 0.5~1.5h, stands 1~4h;It is described Flocculant is one or more of FeCl3, FeSO4 or AlCl3;PH value >=8 are adjusted with saturated limewater;The filter type For plate compression, filter sizes are 0.4~30 μm;The water consumption for washing filter residue is 1~2 times of sweet tea material quality.
5. the method for Rubusoside is extracted described according to claim 1~one of 4 from sweet tea, it is characterised in that: step (3) In, the ultrafiltration membrane for ultrafiltration is ceramic membrane, and aperture is 0.3~1.0 μm;The nanofiltration is that ultrafiltrate is first passed through to retention molecule Amount is the nanofiltration membrane of 800~5000 dalton, and water catches up with film to permeate without sweet taste, and it is 100 that permeate passes through molecular cut off again The nanofiltration membrane of~500 dalton obtains nanofiltration retentate fluid until water catches up with film to hundred benefit degree >=20% of trapped fluid.
6. the method for Rubusoside is extracted described according to claim 1~one of 5 from sweet tea, it is characterised in that: step (4) In, the macroporous adsorption resin chromatography column is made of >=2 chromatographic columns, first upper 1st chromatographic column of nanofiltration retentate fluid, to its outflow After liquid is pleasantly sweet, the 2nd chromatographic column concatenated on efflux, while nanofiltration retentate fluid starts upper 2nd chromatographic column, with such It pushes away, after the completion of upper prop, the 1st is connected in series to 1 chromatographic column of most end and is washed, water lotion discards, then uses organic solvent Gradient elution is carried out to every chromatographic column respectively;The diameter height of the macroporous adsorption resin chromatography column compares for 1:2~8;The macropore The volume mass ratio for adsorbing resin and Sweet tea leaf raw material is 1:5~10;The flow velocity of the upper prop is 1~4BV/h;The macropore is inhaled One or more of model D-101, AB-8, LX-T28, DM-130 or X-5 of attached resin;The flow velocity of the washing is 1.0 ~3.0BV/h;The flow velocity of the organic solvent gradient elution is 0.5~2.0BV/h;The gradient elution refers to: first with 1~ The organic solvent of 3BV volume fraction 10~30% elutes, and discards eluent, then organic molten with 1~3BV volume fraction 60~95% Agent elution, collects eluent;The organic solvent is edible ethanol solution;The temperature of the reduced pressure is 60~90 DEG C, pressure Power is -0.09~-0.07MPa, and being concentrated under reduced pressure into solid content is 10~30%.
7. the method for Rubusoside is extracted described according to claim 1~one of 6 from sweet tea, it is characterised in that: step (5) In, the flow velocity of the upper prop is 0.5~2.0BV/h;The diameter height of the alumina chromatographic column compares for 1:2~8;The aluminium oxide with The volume mass ratio of Sweet tea leaf raw material is 1:40~100;The aluminium oxide is acidic alumina or neutral alumina;The oxidation Aluminium is first activated using preceding: first by aluminium oxide under 500~600 DEG C of hot conditions, after activating 10~20h, then using body Fraction be 85~98% ethanol solution clean it is colorless and transparent to efflux, and in addition to ethanol flavor without other smells until, finally It is washed to no ethanol flavor;The mesh number of the aluminium oxide is 80~300 mesh;The flow velocity of the washing is 0.5~1.0BV/h;It is described The temperature of reduced pressure is 60~90 DEG C, and pressure is -0.09~-0.07MPa, and being concentrated under reduced pressure into solid content is 40~60%.
8. the method for Rubusoside is extracted described according to claim 1~one of 7 from sweet tea, it is characterised in that: step (6) In, the dosage of the active carbon is the 0.1~0.5% of concentrate quality;The mesh number of the active carbon is 60~200 mesh;It is described to stir The temperature mixed is 80~100 DEG C, and the time is 0.5~1.5h;Described be filtered into first uses plate compression, then uses ceramic membrane filter;Institute The aperture for stating board-like filter membrane used in plate compression is 0.4~30 μm, and the aperture of the ceramic membrane is 0.3~1.0 μm;The decompression The temperature of concentration is 60~90 DEG C, and pressure is -0.09~-0.07MPa, and being concentrated under reduced pressure into solid content is 40~60%;It is described spraying Dry inlet air temperature is 180~220 DEG C, and leaving air temp is 70~90 DEG C.
9. the method for Rubusoside is extracted described according to claim 1~one of 8 from sweet tea, it is characterised in that: step (7) In, the mass ratio of the Rubusoside crude product and organic solvent is 1:5~15;The volume fraction of the organic solvent is 60~95%; The temperature of the dissolution is 60~90 DEG C;The temperature of the crystallization be -5~10 DEG C, the time be 2~for 24 hours;The organic solvent is One or more of methanol, ethyl alcohol, propyl alcohol or isopropanol;The vacuum drying temperature be 60~90 DEG C, vacuum degree be- 0.01~-0.09MPa, the time be 2~for 24 hours.
CN201811102849.4A 2018-09-20 2018-09-20 A method of extracting Rubusoside from sweet tea Withdrawn CN109180755A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110615819A (en) * 2019-10-10 2019-12-27 合肥极世茗香生物科技有限公司 Method for rapidly extracting rubusoside
CN110786443A (en) * 2019-10-22 2020-02-14 湖南华诚生物资源股份有限公司 Method for debitterizing and deastringent taste of sweet tea extract
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
CN113603742A (en) * 2021-08-06 2021-11-05 湖南华诚生物资源股份有限公司 Preparation method of mogroside V
CN113637038A (en) * 2021-08-24 2021-11-12 湖南华诚生物资源股份有限公司 Method for extracting sweet tea glycoside and sweet tea polyphenol without bitter taste from sweet tea leaves

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110615819A (en) * 2019-10-10 2019-12-27 合肥极世茗香生物科技有限公司 Method for rapidly extracting rubusoside
CN110786443A (en) * 2019-10-22 2020-02-14 湖南华诚生物资源股份有限公司 Method for debitterizing and deastringent taste of sweet tea extract
CN110786443B (en) * 2019-10-22 2022-08-02 湖南华诚生物资源股份有限公司 Method for debitterizing and deastringent taste of sweet tea extract
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
CN113603742A (en) * 2021-08-06 2021-11-05 湖南华诚生物资源股份有限公司 Preparation method of mogroside V
CN113637038A (en) * 2021-08-24 2021-11-12 湖南华诚生物资源股份有限公司 Method for extracting sweet tea glycoside and sweet tea polyphenol without bitter taste from sweet tea leaves
CN113637038B (en) * 2021-08-24 2022-06-21 湖南华诚生物资源股份有限公司 Method for extracting sweet tea glycoside and sweet tea polyphenol without bitter taste from sweet tea leaves

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