CN102796152A - Method for preparing high-Reb-D-content stevioside - Google Patents

Abstract

The invention discloses a method for adsorbing and purifying stevioside in a serial way by using multi-column secondary resin. A stevioside product which contains over 80 percent of Reb-D glycosides is prepared by pretreating smashed stevioside leaves, desalting, adsorbing, treating with resin, eluting, decolorizing, performing ion exchange, performing nano-filtration and concentration, crystalizing and drying. According to the principle that adsorption resin has different affinity on different stevioside components, Reb-D glycosides are eluated with low-concentration ethanol, so that the relative content of Reb-D glycosides in an eluent is increased; and purification and refining are further performed with methods such as decolorizing impurity removal, ion exchange impurity removal, crystallization separation and the like, so that the total glycoside content of the obtained stevioside product is over 90 percent, and the content of Reb-D glycosides is over 80 percent. Compared with ordinary stevioside, the high-Reb-D-content stevioside prepared with the method has the advantages of higher saccharinity, purer mouthfeel and freeness from unpleasant aftertaste.

Description

Produce the method for high Reb-D Steviosides

Technical field

The present invention relates to a kind of preparation and purification techniques of Steviosides, especially a kind of method of producing high Reb-D Steviosides.

Background technology

Steviosides is that a kind of high sugariness that from the blade of catananche's sweet Stevia, extracts, low heat energy, flavor matter are good, the new type natural sweeting agent of safety non-toxic, can be widely used in industries such as food, beverage, medicine, day chemical industry.Steviosides is a polycomponent glucoside mixture, and sugariness and mouthfeel depend on its glucoside component and content.In the known nine kinds of components of Steviosides; Stevioside (being called for short the Stv glucoside), Rui Baodi A glucoside (being called for short the Reb-A glucoside), Rui Baodi C glucoside (being called for short the Reb-C glucoside) account for the overwhelming majority about 92%; And Rui Baodi D glucoside (be called for short Reb-D glucoside) relative content is less about 0.8%, but the highest 450 times of being about white sugar of the sugariness of Reb-D glucoside, and also flavor matter is best; Do not contain any bad pleasant impression; Be described as " gold in the Steviosides " by the insider, price also is 3-5 a times of other glucosides, is a kind of ideal natural sweeteners.Therefore, the Steviosides product of producing the high Reb-D glucoside of content has vast market prospect.

Summary of the invention

The object of the present invention is to provide a kind of method of producing high Reb-D Steviosides.

The technical solution adopted for the present invention to solve the technical problems is:

(a) pre-treatment: the stevioside leaf of pulverizing is mixed with 50 ℃ of-55 ℃ of softening waters; Continuous countercurrent extraction reaches more than 99.99% the glucoside percentage extraction of stevioside leaf, processes the Steviosides extraction liquid; After extraction liquid process flocculation sediment and the filter press two procedures, get into next process;

(b) desalination: with the desalination of above-mentioned filtrating spent ion exchange resin, get the desalination filtrating of transmittance>=65%, specific conductivity≤6700us/cm, desalination filtrating gets into next process;

(c) absorption: adopt Steviosides effective constituent in the above-mentioned desalination filtrating of resin absorption, only go out when sweet to resin;

(d) plastic resin treatment and wash-out: 1) plastic resin treatment: wash resin with dilute solution of sodium hydroxide, hydrochloric acid dilute solution, pure water, reach at 7 o'clock to effluent pH value and end; 2) resin is resolved: using concentration is that 30% ethanolic soln carries out wash-out to resin, must contain the elutriant of Reb-D glucoside 4-5%, and elutriant gets into next process;

(e) decolouring: gac is inserted mixing stirring in the elutriant, and the process Plate Filtration must contain the destainer of Reb-D glucoside 5-6%, and destainer gets into next process;

(f) IX: destainer through after Zeo-karb and the anionite-exchange resin removal of impurities, must contain the exchange liquid of Reb-D glucoside 6-7% successively, and exchange liquid gets into next process;

(g) nanofiltration concentrates: it is 25%-30% liquid concentrator that exchange liquid gets glucoside concentration through the nf membrane thickening filtration, and liquid concentrator gets into next process;

(h) crystallization: the liquid concentrator after the nanofiltration is positioned over static crystallization 48h below 10 ℃, filtration, drip washing crystal, xln gets into next process;

(i) drying:, obtain containing the Steviosides product of Reb-D glucoside more than 80% with xln vacuum-drying.

Effect of the present invention is: utilize polymeric adsorbent that the Steviosides different components is had different avidity principles, with low-concentration ethanol the Reb-D glucoside is carried out wash-out, improved the relative content of Reb-D glucoside in the elutriant; Through further purifications of method such as decolouring removal of impurities, IX removal of impurities, Crystallization Separation, last gained Steviosides product always contains the glucoside amount greater than 90% again, and wherein the Reb-D salidroside content reaches more than 80%.Compare with common Steviosides, sugariness is higher, and mouthfeel is purer, does not have bad pleasant impression.

Embodiment

Below in conjunction with embodiment the present invention is done and to describe in further detail.

(a) pre-treatment: with sweet Stevia and 50 ℃ of-55 ℃ of soft water by weight/volume ratio 1:15 mixes, soak to make the Steviosides extracting solution, through flocculation sediment and filter press two procedures, the cleaner liquid entering next process behind the Plate Filtration;

(b) desalination: with 732 types sun, the desalination of LK-330 anionite-exchange resin, gained demineralised liquid transmittance is 78.2%, specific conductivity is 4950 μ s/cm with above-mentioned filtrating, and demineralised liquid gets into next process;

(c) absorb-elute: adsorb the Steviosides effective constituent in the above-mentioned desalination filtrating with the YW-03F polymeric adsorbent; Adsorb the resin after saturated; Clean resin column with 2BV resin volume 0.5% sodium hydroxide solution and 2BV resin volume 0.5% hydrochloric acid dilute solution earlier, using pure water drip washing adsorption column to the effluent pH value of capacity then is 7, and the ethanolic soln with 2BV resin volume 30% carries out wash-out to resin column again; Obtain containing the elutriant of Reb-D glucoside 4.8%, elutriant gets into next process;

(d) decolour: the vegetable active charcoal is inserted to mix in the elutriant by 0.4% of effluent volume stirred 1 hour, Plate Filtration obtains containing the destainer of Reb-D glucoside 5.6%, and destainer gets into next process;

(e) IX: destainer carries out removal of impurities through 732 type Zeo-karbs and YW-07t anionite-exchange resin successively to be handled, and obtains containing the exchange liquid of Reb-D glucoside 7.8%, and exchange liquid gets into next process;

(f) nanofiltration concentrates: it is 28% liquid concentrator that exchange liquid gets glucoside concentration through the nf membrane thickening filtration, and liquid concentrator gets into next process;

(g) crystallization: the liquid concentrator after the nanofiltration is positioned over static crystallization 48h below 10 ℃, and filtration, drip washing get crystal, and crystal gets into next process;

(h) drying:, get the Steviosides product with crystal vacuum-drying.Through efficient liquid phase chromatographic analysis, it is 92.75% that product contains the glucoside amount, and wherein the Reb-D salidroside content is 84.63%.

The measuring method of each parameter is in the literary composition:

(1) contains the detection method that the glucoside amount is a purity: press JECFA 2010 Steviol Glycosides;

(2) determination of light transmittance method: 25 ℃ of 722 type visible spectrophotometer of room temperature wavelength, 480 nanometers;

(3) conductance measurement method: 25 ℃ of conductivitimeters of room temperature;

(4) than absorbance measurement method: press GB 8270-1999.

Claims (1)

1. method of producing high Reb-D Steviosides, its characteristic is following in the preparation method:

(a) pre-treatment: the stevioside leaf of pulverizing is mixed with 50 ℃ of-55 ℃ of softening waters; Continuous countercurrent extraction reaches more than 99.99% the glucoside percentage extraction of stevioside leaf, processes the Steviosides extraction liquid; After extraction liquid process flocculation sediment and the filter press two procedures, get into next process;

(b) desalination: with the desalination of above-mentioned filtrating spent ion exchange resin, get the desalination filtrating of transmittance>=65%, specific conductivity≤6700us/cm, desalination filtrating gets into next process;

(c) absorption: adopt Steviosides effective constituent in the above-mentioned desalination filtrating of resin absorption, only go out when sweet to resin;

(d) plastic resin treatment and wash-out: 1) plastic resin treatment: wash resin with dilute solution of sodium hydroxide, hydrochloric acid dilute solution, pure water, reach at 7 o'clock to effluent pH value and end; 2) resin is resolved: using concentration is that 30% ethanolic soln carries out wash-out to resin, must contain the elutriant of Reb-D glucoside 4-5%, and elutriant gets into next process;

(e) decolouring: gac is inserted mixing stirring in the elutriant, and the process Plate Filtration must contain the destainer of Reb-D glucoside 5-6%, and destainer gets into next process;

(f) IX: destainer through after Zeo-karb and the anionite-exchange resin removal of impurities, must contain the exchange liquid of Reb-D glucoside 6-7% successively, and exchange liquid gets into next process;

(g) nanofiltration concentrates: it is 25%-30% liquid concentrator that exchange liquid gets glucoside concentration through the nf membrane thickening filtration, and liquid concentrator gets into next process;

(h) crystallization: the liquid concentrator after the nanofiltration is positioned over static crystallization 48h below 10 ℃, filtration, drip washing crystal, xln gets into next process;

(i) drying:, obtain containing the Steviosides product of Reb-D glucoside more than 80% with xln vacuum-drying.