# US 11,110,144 B2 · Wolfberry glycopeptide composition and methods for preparing and using the same

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- Number: US 11,110,144 B2
- Document ID: US11110144B2
- Status: Granted
- Kind: B2
- Application number: 16/049,238
- Filed: 2018-07-30
- Published: 2020-01-30
- Granted: 2021-09-07
- Earliest claimed: 2018-07-30
- Assignees: Shanghai Institute of Organic Chemistry, Chinese Academy of Sciences
- Applicants: Shanghai Institute of Organic Chemistry, Chinese Academy of Sciences
- Inventors: Long Lu; Yan Jiang; Juan Shen; Zhigang Ding; Yuhua Xiang; Guiqing Chen; Gengyuan Tian
- Web page: https://patentgrep.com/patent/US11110144B2

## CPC

- A61K 36/815: Lycium (desert-thorn)
- A23L 33/105: Plant extracts, their artificial duplicates or their derivatives
- A23L 33/18: Peptides; Protein hydrolysates
- A61K 8/64: Proteins; Peptides; Derivatives or degradation products thereof
- A61K 8/645: {Proteins of vegetable origin; Derivatives or degradation products thereof}
- A61K 8/9789: Magnoliopsida [dicotyledons]
- A61K 38/168: {from plants}
- A61P 3/06: Antihyperlipidemics
- A61P 9/00: Drugs for disorders of the cardiovascular system
- A61P 35/00: Antineoplastic agents
- A61P 37/00: Drugs for immunological or allergic disorders
- A61Q 19/00: Preparations for care of the skin
- A61Q 19/08: Anti-ageing preparations
- B01D 21/262: {by using a centrifuge}
- B01D 61/145: {Ultrafiltration}
- A23V 2002/00: Food compositions, function of food ingredients or processes for food or foodstuffs
- A61K 2236/331: using water, e.g. cold water, infusion, tea, steam distillation or decoction
- A61K 2236/39: Complex extraction schemes, e.g. fractionation or repeated extraction steps
- A61K 2236/51: Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
- B01D 61/16: Feed pretreatment
- B01D 61/22: Controlling or regulating
- B01D 2311/04: Specific process operations in the feed stream; Feed pretreatment
- B01D 2311/2642: Aggregation, sedimentation, flocculation, precipitation or coagulation
- B01D 2311/2676: Centrifugal separation
- A61K: PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES (devices or methods specially adapted for bringing pharmaceutical products into particular physical or administering forms A61J3/00; chemical aspects of, or use of materials for deodorisation of air, for disinfection or sterilisation, or for bandages, dressings, absorbent pads or surgical articles A61L; soap compositions C11D)
- A23L: FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES, NOT OTHERWISE PROVIDED FOR; PREPARATION OR TREATMENT THEREOF (preservation thereof A23B)
- A61P: SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61Q: SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- B01D: SEPARATION (separating solids from solids by wet methods B03B, B03D; by pneumatic jigs or tables B03B; by other dry methods B07; magnetic or electrostatic separation of solid materials from solid materials or fluids, separation by high-voltage electric fields B03C; centrifuges, vortex apparatus B04; presses per se for squeezing-out liquid from liquid-containing material B30B9/02; treatment of water C02F, e.g. softening by ion-exchange C02F1/42; {arrangements of air intake cleaners in gas turbine plants F02C7/05} ; arrangements or mounting of filters in air-conditioning, air-humidification or ventilation F24F13/28)
- A23V: INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION

## Abstract

Wolfberry glycopeptide composition and methods for preparing and using the same, the part with a molecular weight distribution of 1000 Da to 10000 Da of the wolfberry glycopeptide accounts for 50-85% on the HPLC differential refractive index map; and the protein content is 20-35% weight percentage, neutral polysaccharide content is 20-35% weight percentage. Optionally, the uronic acid content is 5-20% weight percentage. The preparation method of the present invention removes part of insoluble impurities by a heating flocculation method, instead of the conventional organic solvent extraction process, and without using any organic solvents in the whole process.

## Claims

### Claim 1

A method for preparing a glycopeptide composition, comprising:
(a) soaking fruit of wolfberry in water and centrifuging to remove precipitated solids to obtain a first extract solution;
(b) heating the first extract solution to provide a flocculation in the first extract solution, and centrifuging the first extract solution to remove the flocculation to obtain a second extract solution, wherein the second extract solution has a light transmittance at 50% or higher at 400 nm; and
(c) treating the second extract solution with an ultrafiltration membrane, obtaining a cut-off solution with a molecular weight cutoff of the ultrafiltration membrane, concentrating, and drying the cut-off solution to obtain a glycopeptide composition,
wherein the flocculation is formed by agglomerating insoluble substances in the first extract solution into precipitates, the molecular weight cutoff of the ultrafiltration membrane is in a range of 1000 Da to 2000 Da, and each of the steps (1) to (3) is conducted in water only.

### Claim 2 (depends on 1)

The method of claim 1, wherein the fruit wolfberry is soaked in water at a temperature in a range of 10° C. to 35° C. for 2 hours to 10 hours.

### Claim 3 (depends on 1)

The method of claim 1, wherein the first extract solution is heated at a temperature in a range of 45° C. to 70° C. for 0.5 hour to 5 hours to form the flocculation.

### Claim 4 (depends on 1)

The method of claim 1, wherein the mass ratio of the fruit of wolfberry to water for soaking in step (a) is 1:1 to 1:15.

### Claim 5 (depends on 4)

The method of claim 4, wherein the fruit of wolfberry is dried fruit, and the mass ratio of the dried fruit to the amount of the water for soaking is 1:5 to 1:15.

### Claim 6 (depends on 4)

The method of claim 4, wherein the fruit of wolfberry is fresh fruit, and the mass ratio of the fresh fruit to the amount of the water for soaking is 1:1 to 1:3.

### Claim 7 (depends on 1)

The method of claim 1, wherein centrifuging to obtain the first extract solution is at a centrifugal speed of 1000 rpm to 4000 rpm for 10 seconds to 1 minute.

### Claim 8 (depends on 1)

The method claim 1, wherein the light transmittance of the second extract solution is at 60% or more at 400 nm.

### Claim 9 (depends on 1)

The method of claim 1, wherein the first extract solution is heated to a temperature in a range of 45° C. to 70° C. for a time period of 0.5 hour to 5 hours, and centrifuged at a centrifugal speed of 6000 rpm to 16000 rpm for 5 seconds to 5 minutes.

### Claim 10 (depends on 1)

The method of claim 1, wherein the cut-off solution is dried by freeze drying, spray drying, or a combination thereof, to obtain the glycopeptide composition.

### Claim 11 (depends on 1)

The method of claim 1, further comprising:
continuously providing water to the cut-off solution during ultrafiltration in step (c); and
monitoring electrical conductivity and sugar degree of the cut-off solution; wherein the cut-off solution is collected when the electrical conductivity of the cut-off solution is below 1000us/cm and the sugar degree is below 1.2.