CN102786565A - Process for purifying stevia glycosides by multi-column resin series connection and alcoholic absorption - Google Patents

Abstract

The invention discloses a process for purifying stevia glycosides by multi-column resin series connection and alcoholic absorption. A high-purity stevia glycoside product can be prepared through procedures such as pretreatment, desalination, primary adsorption and desorption, decoloration, primary ion exchange, secondary adsorption and desorption, secondary ion exchange and spray drying of crushed stevia leaves. According to the process, different components of stevia glycosides are different in solubility in the same solvent, adsorbent resins have different adsorptive selectivity principles for different components of stevia glycosides, and the multi-column adsorbent resin series connection is used for absorbing alcoholic liquids, so that the purity of stevia glycosides can be improved, the glycoside content of the obtained stevia glycoside product can exceed 95% and the specific absorptivity is no more than 0.02. Compared with common stevia glycoside products with the purity of 90%, the high-purity stevia glycoside product has the advantages of being high in purity, high in sweetness, pure in taste, free of bad remaining taste and the like.

Description

The method of series connection of multicolumn resin and band alcohol absorption purification Steviosides

Technical field

The present invention relates to a kind of preparation and purification techniques of Steviosides, the method for especially a kind of multicolumn resin series connection and band alcohol absorption purification Steviosides.

Background technology

The Steviosides product is from catananche--a kind of high sugariness that extracts the blade of sweet Stevia, low heat energy, flavor matter are good, safety non-toxic, the extraordinary a kind of novel pure natural sweeting agent of market outlook; Can be widely used in industries such as food, beverage, medicine, day chemical industry.Steviosides is a polycomponent glucoside mixture, and present known sweet ingredient has 9 kinds, and its sugariness and mouthfeel depend on glucoside component and total salidroside content.At present; The market requirement of high purity stevioside product that contains glucoside amount>=95% is increasing; By being pursued the world market, yet its purity of product that the production purifying technique of existing Steviosides product is produced promptly contains glucoside amount≤90%, is difficult to reach the world market requirement.

Summary of the invention

The object of the present invention is to provide the method for a kind of multicolumn resin series connection and band alcohol absorption purification 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) primary sorption and parsing: adopt Steviosides effective constituent in the above-mentioned desalination filtrating of resin absorption, only go out when sweet to resin; Wash resin, reach at 7 o'clock to effluent pH value and end with dilute solution of sodium hydroxide, hydrochloric acid dilute solution, pure water; Using concentration is that 52% ethanolic soln carries out the branch post to resin and resolves, must contain the glucoside amount and be 80-82%, than absorbancy≤0.50, to contain the alcohol amount be 40% desorbed solution, desorbed solution gets into next process;

(d) decolouring: gac inserted in the desorbed solution to mix stirs, Plate Filtration cross filter contain glucoside amount 81-83%, than absorbancy≤0.20, to contain the alcohol amount be 35% destainer, destainer gets into next process;

(e) primary ions exchange: destainer is successively through after Zeo-karb and the anionite-exchange resin removal of impurities; To obtain containing the glucoside amount be 81-83%, than absorbancy≤0.10, contain the primary ions exchange liquid of alcohol amount for 30%-33%, primary ions exchange liquid gets into next process

(f) second adsorption is resolved: with the bigger serface polymeric adsorbent of HL-3 type; With placed in-line form 4 pillars that resin is housed are together in series; Adsorb above-mentioned primary ions exchange liquid, end when saturated, with the pure water drip washing resin column of connecting from first post to a last post;, do not end last column outlet effluent when having the alcohol flavor; Using concentration then is that 70% ethanolic soln carries out wash-out to polymeric adsorbent and resolves, and obtains being 55%, containing the glucoside amount greater than 95% desorbed solution that than absorbancy≤0.05, pure content desorbed solution gets into next process;

(g) secondary ions exchange: desorbed solution is got into dormant state once more carry out deep impurity-removing through Zeo-karb and anionite-exchange resin; Obtain containing the glucoside amount and be 55% secondary ions exchange liquid greater than 95%, than absorbancy≤0.03, pure content; This ion exchange liquid is carried out evaporation concentration; Using the aperture again is that 0.22 micron degerming filter core carries out Sterile Filtration, obtains containing the glucoside amount greater than 95%, get into next process than the liquid concentrator of absorbancy≤0.02;

(h) spraying drying: the liquid concentrator after the Sterile Filtration is carried out spraying drying, obtain containing glucoside amount>=95%, than absorbancy≤0.02 Steviosides product.

Effect of the present invention is: utilize that different components has different solubilities in the Steviosides in same solvent; And polymeric adsorbent has different adsorption selectivity principle to the Steviosides different components, adopts the series connection of multicolumn polymeric adsorbent to being with pure feed liquid to adsorb, and can reach the effect that improves Steviosides purity; Gained Steviosides product contains the glucoside amount and reaches more than 95%, than absorbancy≤0.02.This compares at 90% Steviosides product with ordinary purity, has the high purity stevioside product that purity is higher, the sugariness multiple is higher, mouthfeel is purer, do not have advantages such as bad pleasant impression.

Embodiment

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

(a) pre-treatment: the ratio in 1:15 is mixed the stevioside leaf end with 50 ℃ of-55 ℃ of softening waters; Process the Steviosides extracting solution with the continuous countercurrent extraction method; Through flocculation sediment and filter press two procedures; Cleaner liquid transmittance behind the Plate Filtration is 60.3%, and cleaner liquid gets into next process;

(b) desalination: with above-mentioned cleaner liquid with 732 positively charged ions and the desalination of YW-07t anionite-exchange resin, the desalination that transmittance is 78.0%, specific conductivity is 2290 μ s/cm filtrating, desalination filtrating gets into next process; Promptly adsorb waste liquid through the liquid after the absorption and after biochemical treatment reaches two types of emission standards of country, drain into rivers;

(c) absorption is resolved: with Steviosides effective constituent in the above-mentioned desalination filtrating of YW-03F resin absorption; The absorption waste liquid discharges after biochemical treatment is up to standard; After having adsorbed the resin of Steviosides effective constituent with 2BV resin volume 0.5% sodium hydroxide and the 0.5% salt s.t. of 2BV resin volume; Pure water with 2BV resin volume is washed acid, ends by 7 o'clock to the pH value, resolves with 52% ethanolic soln of 2BV resin volume again; Must be 0.468 than absorbancy, to contain the glucoside amount be 81.2% desorbed solution, desorbed solution gets into next process;

(d) decolouring: by the material liquid volume ratio is that 0.04% vegetable active charcoal is inserted in the desorbed solution to mix and stirred 1 hour, cross filter than absorbancy be 0.195, to contain the glucoside amount be 82.0% destainer, destainer gets into next process;

(e) IX: destainer is successively through 732 Zeo-karbs and the removal of impurities of YW-07t anionite-exchange resin, must be 0.082 than absorbancy, contain that the glucoside amount is 82.6%, ethanol content is 31.2% once exchange liquid, exchange liquid entering next process;

(f) second adsorption is resolved: with the above-mentioned band alcohol of multicolumn HL-3 type polymeric adsorbent series adsorption exchange liquid; Do not end when having the alcohol flavor with pure water drip washing to effluent then; Resolve with 70% ethanolic soln of 2BV resin volume again; Must be 0.048 than absorbancy, to contain the glucoside amount be 95.5% desorbed solution, desorbed solution gets into next process;

(g) secondary ions exchange: the 732 type Zeo-karbs and the YW-07t anionite-exchange resin columns in series that desorbed solution are got into once more dormant state carry out deep impurity-removing; Obtain secondary exchange liquid; Carry out evaporation concentration to secondary exchange liquid, obtain than absorbancy be 0.017, to contain the glucoside amount be 95.96% liquid concentrator, using the aperture again is that 0.22 micron degerming filter core carries out Sterile Filtration; Obtain Sterile Filtration liquid, Sterile Filtration liquid gets into next process;

(h) spraying drying:, get the Steviosides product with the liquid concentrator spraying drying after the Sterile Filtration.Through analyzing, it is 95.96% that product contains the glucoside amount, is 0.017 than absorbancy.

The present invention and traditional technology and industry M.L. are following:

Technical indicator (do not indicate especially be MV)	Traditional technology	Improve back technology	The industry M.L.
				Than absorbancy ( ）	0.08	0.04	0.08
Contain glucoside amount (%)	90	≥95	90
				Impurity ratio (%)	7.8	1.5	7.8

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. a multicolumn resin is connected and the pure method of adsorbing the purification Steviosides of band, and 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) primary sorption and parsing: adopt Steviosides effective constituent in the above-mentioned desalination filtrating of resin absorption, only go out when sweet to resin; Wash resin, reach at 7 o'clock to effluent pH value and end with dilute solution of sodium hydroxide, hydrochloric acid dilute solution, pure water; Using concentration is that 52% ethanolic soln carries out the branch post to resin and resolves, must contain the glucoside amount and be 80-82%, than absorbancy≤0.50, to contain the alcohol amount be 40% desorbed solution, desorbed solution gets into next process;

(d) decolouring: gac inserted in the desorbed solution to mix stirs, Plate Filtration cross filter contain glucoside amount 81-83%, than absorbancy≤0.20, to contain the alcohol amount be 35% destainer, destainer gets into next process;

(e) primary ions exchange: destainer is successively through after Zeo-karb and the anionite-exchange resin removal of impurities; To obtain containing the glucoside amount be 81-83%, than absorbancy≤0.10, contain the primary ions exchange liquid of alcohol amount for 30%-33%, primary ions exchange liquid gets into next process

(f) second adsorption is resolved: with the bigger serface polymeric adsorbent of HL-3 type; With placed in-line form 4 pillars that resin is housed are together in series; Adsorb above-mentioned primary ions exchange liquid, end when saturated, with the pure water drip washing resin column of connecting from first post to a last post;, do not end last column outlet effluent when having the alcohol flavor; Using concentration then is that 70% ethanolic soln carries out wash-out to polymeric adsorbent and resolves, and obtains being 55%, containing the glucoside amount greater than 95% desorbed solution that than absorbancy≤0.05, pure content desorbed solution gets into next process;

(g) secondary ions exchange: desorbed solution is got into dormant state once more carry out deep impurity-removing through Zeo-karb and anionite-exchange resin; Obtain containing the glucoside amount and be 55% secondary ions exchange liquid greater than 95%, than absorbancy≤0.03, pure content; This ion exchange liquid is carried out evaporation concentration; Using the aperture again is that 0.22 micron degerming filter core carries out Sterile Filtration, obtains containing the glucoside amount greater than 95%, get into next process than the liquid concentrator of absorbancy≤0.02;

(h) spraying drying: the liquid concentrator after the Sterile Filtration is carried out spraying drying, obtain containing glucoside amount>=95%, than absorbancy≤0.02 Steviosides product.