US 2026/0265801 A1Published application

Method for preparing glucosyl stevioside using mother liquor sugar, separating and purifying glucosyl stevioside and recovering glucose

AssigneeDongtai Haorui Biotechnology Co., Ltd.

InventorsLiping ZHU, Dongsheng HE, Xiaojie GUO, Hao LIU, Xinxin CAO, Min JU, Pengfei ZANG

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Abstract

A method for preparing glucosyl stevioside using a mother liquor sugar, separating and purifying the glucosyl stevioside and recovering glucose. By taking a mother liquor sugar as a raw material to prepare glucosyl stevioside, the route of utilization of mother liquor sugars is enriched, the technical gap of preparing glucosyl stevioside using a mother liquor sugar as a raw material is filled, and the prepared product has the advantages of good mouthfeel and high total glycoside content. A method for purifying glucosyl stevioside, wherein dextrin is recycled, which reduces the discharge of waste liquid, reduces the energy consumption and cost of production, and improves the yield of glucosyl stevioside with high purity. Further, a method for separating and purifying glucosyl stevioside and recovering glucose, which is simple and easy to operate, and can obtain glucosyl stevioside with high purity, and also recycle unreacted substrates to reduce the cost.

Claims28

Dependent claims

A method for preparing a glucosylated steviol glycoside (GSG) with mother liquor sugar (MLS), comprising the following steps:

(1) mixing the MLS, maltodextrin, and water, and stirring until the MLS and the maltodextrin are fully dissolved;
and adding an enzyme, and allowing enzymatic hydrolysis to produce an enzymatic hydrolysate, wherein the MLS, the maltodextrin, and the water are in a mass ratio of 1:(1-3):(5-10), and the enzymatic hydrolysis is conducted for 36 h to 48 h at a temperature of 60° C. to 80° C. and a pH of 5.5 to 6.0;
(2) adding activated carbon to the enzymatic hydrolysate obtained in the step (1) for impurity removal to produce an impurity-free solution;
subjecting the impurity-free solution to enzyme inactivation and then filtration to produce a filtrate;
and subjecting the filtrate to an adsorption treatment with a macroporous adsorption resin, wherein an amount of the activated carbon added is 1% to 3% of a mass of the enzymatic hydrolysate, and the impurity removal lasts for 1 h to 6 h;
(3) conducting desorption with an acid-alcohol solution that is produced from an ethanol solution and a hydrochloric acid solution and has a pH of 1 to 3 to produce a desorption solution, wherein a concentration of the ethanol solution is 40 v/v % to 60 v/v % and a concentration of the hydrochloric acid solution is 0.3 wt % to 0.5 wt %;
and during the desorption, a volume of the acid-alcohol solution is 2 BV to 4 BV of a volume of a macroporous adsorption resin undergoing adsorption, and a flow rate of the acid-alcohol solution is 1 BV/h to 3 BV/h;
(4) adjusting a pH of the desorption solution to 5 to 6, and concentrating with a nanofiltration membrane to produce a concentrate, wherein molecular weight cut-off of the nanofiltration membrane is 400 Da to 500 Da;
and
(5) adding a taste modifier to the concentrate, and spray-drying to produce the GSG, wherein the taste modifier is a composition of erythritol, sodium alginate, and valine in a mass ratio of 2:(2-4):(5-8);
and an amount of the taste modifier added is 0.1% to 0.5% of a mass of a product in the concentrate.

8 more elements

A method for purifying GSG, comprising the following steps:

(1) dissolving a crude GSG product in an ethanol solution to produce a GSG-containing ethanol solution;
subjecting the GSG-containing ethanol solution to an adsorption treatment with a macroporous adsorption resin, and collecting an effluent;
and conducting desorption with an acid aqueous solution and a high-purity ethanol solution successively, and collecting an acid-water desorption solution and a high-purity ethanol desorption solution, wherein a concentration of the ethanol solution is 5 wt % to 15 wt %;
a concentration of GSGs in the GSG-containing ethanol solution is 30 g/L to 50 g/L;
the acid aqueous solution is a hydrochloric acid solution with a concentration of 0.04 wt % to 0.06 wt %;
and a concentration of the high-purity ethanol solution is 70 wt % to 80 wt %;
(2) concentrating a mixed solution of the effluent and the acid-water desorption solution obtained in the step (1) to produce a first concentrate;
adding α-1,4-glucosidase to the first concentrate, and heating to allow hydrolysis to produce a hydrolysis system;
and adjusting a pH of the hydrolysis system to 3 for inactivating the α-1,4-glucosidase to produce a hydrolysate, wherein a concentration factor for the concentrating is 3 to 5;
and the hydrolysis is conducted at 40° C. to 50° C. for 1 h to 3 h;
(3) adding a steviol glycoside to the hydrolysate, and adjusting a pH of a resulting solution to 6.0;
adding a glucosyltransferase, and heating to allow a reaction;
after the reaction is completed, further heating for inactivating the glucosyltransferase to produce a reaction solution;
concentrating the reaction solution until a solid content is 40 wt % to 50 wt % to produce a second concentrate;
and spray-drying the second concentrate to produce high-purity GSG A, wherein the reaction is conducted at 70° C. to 80° C. for 6 h to 10 h;
and the glucosyltransferase is inactivated at 95° C.;
and
(4) concentrating the high-purity ethanol desorption solution until a solid content is 40 wt % to 50 wt % to produce a third concentrate, and spray-drying the third concentrate to produce high-purity GSG B.

15 more elements

A method for separating and purifying GSG and recovering glucose, comprising the following steps:

(1) re-dissolving a crude GSG product with purified water to prepare a raw material solution;
(2) concentrating the raw material solution through nanofiltration, and collecting a retentate and a permeate;
(3) removing solvents in the retentate and the permeate separately to produce an intermediate A and an intermediate B, respectively;
(4) mixing the intermediate A with methanol, and allowing a settlement;
conducting vacuum filtration to produce a first filter cake and a first filtrate;
and drying the first filtrate to produce high-purity GSG;
(5) mixing the intermediate B with the first filter cake, adding purified water, and stirring until the intermediate B and the first filter cake are fully dissolved;
adding α-1,4-glucosidase, and allowing enzymatic hydrolysis;
and after the enzymatic hydrolysis is completed, heating for inactivating the α-1,4-glucosidase to produce a glucose-containing solution;
and
(6) subjecting the glucose-containing solution to high-temperature concentration to produce a paste-like intermediate C;
and slowly cooling the paste-like intermediate C for crystallization, and conducting vacuum filtration to produce a second filtrate and a second filter cake, wherein the second filtrate is recovered for subsequent production and the second filter cake is high-purity glucose.

9 more elements

Dependencies are inferred from the claim text.