IP Library › Granted Patent US 11,891,411
Granted Patent B2
US 11,891,411 · App. 17/216,928 · Granted Feb 6, 2024

Industrial utilization method for

Inventors: Meili Xu (Hebei, CN); Yunhe Lian (Hebei, CN); Hong Tian (Hebei, CN); Wei Gao (Hebei, CN); Yachao Xu (Hebei, CN)
Assignee: Chenguang Biotech Group Co., Ltd.
C07H15/24C07C67/56
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Quick Facts
Patent No.
US 11,891,411
App. No.
17/216,928
Granted
Feb 6, 2024
Kind
B2
Abstract

An industrialization method for comprehensive utilization of Stevia rebaudiana . The major improvement is in that the Stevia rebaudiana is extracted by using a high-concentration alcohol solution, then the extracted solution is purified by using an organic solvent, and the pH of the extracted solution is adjusted to be alkaline according to the acidic characteristic of chlorogenic acid to enable the chlorogenic acid to be formed into a salt and have an increased polarity so as to achieve effective separation of the chlorogenic acid and a glucoside component in an adsorption process. The method allows the high-quality stevioside and chlorogenic acid to be obtained, significantly improves the comprehensive utilization rate of Stevia rebaudiana , reduces the waste of natural Stevia rebaudiana resources, reduces the resource consumption in a production process, reduces waste discharge, and is a high-benefit green production process.

Claims (18)

1. An industrial utilization method for extracting Stevia rebaudiana , comprising:

1) Extracting Stevia rebaudiana powder with a high-concentration short-chain alcohol aqueous solution to obtain an extract solution, wherein the short-chain alcohol in the high-concentration short-chain alcohol aqueous solution is selected from methanol, ethanol, propanol or any combination thereof, and a volume fraction of the short-chain alcohol in the short-chain alcohol aqueous solution is 70% to 95%;

2) Removing the short-chain alcohol in the extract solution by vacuum concentration, and subjecting the extract solution to liquid-liquid extraction with an organic solvent, and taking water layer to obtain a low-polar impurity-removed extract solution, wherein the organic solvent is a low-polar organic solvent that is water insoluble; and

3) Adjusting pH of the low-polar impurity-removed extract solution to be alkaline, and passing the extract solution through a stevioside adsorption resin to obtain a stevioside extract.

2. The method according to claim 1 , wherein the method comprises adjusting pH of a post-column solution obtained by passing the low-polar impurity-removed extract solution through a stevioside resin to be acidic, and passing the post-column solution through a chlorogenic acid adsorption resin to obtain a chlorogenic acid extract.

3. The method according to claim 2 , wherein the organic solvent is selected from the group of pentane, n-hexane, octane, diethyl ether or cyclohexane.

4. The method according to claim 2 , wherein the pH of the post-column solution obtained by passing the low-polar impurity-removed extract solution through a stevioside resin is adjusted to 2 to 3.

5. The method according to claim 1 , wherein the Stevia rebaudiana extraction is performed at a material-liquid ratio of 1:3.5 to 1:6, and an extraction temperature of 20° C. to 80° C.; and/or the extraction is performed for 2 to 3 times with 0.5 h to 3 h for each extraction.

6. The method according to claim 2 , further comprising:

removing the short-chain alcohol in the extract solution by vacuum concentration;

subjecting the stevioside adsorption resin to elution with water, subjecting the stevioside adsorption resin to desorption with an alcohol solution, and collecting the desorbed solution to obtain a stevioside extract; and

mixing the post-column solution, adjusting pH of resultant mixed liquid to be acidic, passing the mixed liquid through a chlorogenic acid adsorption resin for adsorption, subjecting the chlorogenic acid adsorption resin to elution with water, and subjecting the chlorogenic acid adsorption resin to desorption with an alcohol solution, and collecting the desorbed solution to obtain a chlorogenic acid extract.

7. The method according to claim 2 , wherein the organic solvent is a low-polar organic solvent that is water insoluble, selected from the group of pentane, n-hexane, octane, diethyl ether or cyclohexane.

8. The method according to claim 2 , wherein in the step 3), the pH of the low-polar impurity-removed extract solution is adjusted to 9 to 11.

9. The method according to claim 1 , wherein in the step 3), the pH of the low-polar impurity-removed extract solution is adjusted to 9 to 11.

10. The method according to claim 3 , wherein in the step 3), the pH of the low-polar impurity-removed extract solution is adjusted to 9 to 11.

11. The method according to claim 3 , wherein the pH of the post-column solution obtained by passing the low-polar impurity-removed extract solution through a stevioside resin is adjusted to 2 to 3.

12. The method according to claim 2 , wherein the Stevia rebaudiana extraction is performed at a material-liquid ratio of 1:3.5 to 1:6, and an extraction temperature of 20° C. to 80° C.; and/or the extraction is performed for 2 to 3 times with 0.5 h to 3 h for each extraction.

Assignments (1)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Apr 15, 2021
From: XU, MEILI; LIAN, YUNHE; TIAN, HONG; GAO, WEI; XU, YACHAO
To: CHENGUANG BIOTECH GROUP CO.,LTD.
Reel/Frame 055934/0475 →
Priority Claims (1)
CN 201811159791.7 · Sep 30, 2018 · national
Continuity (2)
Continuation PCTCN2019108619 · Sep 27, 2019
Related Publication 20210230204A1 · Jul 29, 2021