METHOD OF PREPARING HOVENIA DULCIS THUNB EXTRACT RICH IN DIHYDROMYRICETIN

Abstract

A method for preparing a Hovenia dulcis Thunb extract rich in dihydromyricetin includes the following steps: (1) crushing Hovenia dulcis Thunb seeds to obtain a Hovenia dulcis Thunb powder; (2) adding a 10-95% ethanol solution in an amount of 3-15 times of an amount of the Hovenia dulcis Thunb powder, stirring and extracting at 20° C-80° C. twice; (3) filtering to obtain an extract solution; (4) concentrating the extract solution by evaporating ethanol under reduced pressure to obtain a crude extract, the crude extract having a solid content of 10%-40%; (5) placing the crude extract at −20° C. to 8° C. for 0.5 to 12 hours; (6) centrifuging the crude extract to obtain a supernatant; and (7) spray-drying the supernatant to obtain the Hovenia dulcis Thunb extract.

Claims

1. A method for preparing a Hovenia dulcis Thunb extract rich in dihydromyricetin, consisting of the following steps: (1) crushing Hovenia dulcis Thunb seeds to obtain a Hovenia dulcis Thunb powder; (2) adding a 10-95% ethanol solution in an amount of 3-15 times of an amount of the Hovenia dulcis Thunb powder, stirring and extracting at 20° C-80° C. twice; (3) filtering to obtain an extract solution; (4) concentrating the extract solution by evaporating ethanol under reduced pressure to obtain a crude extract, the crude extract having a solid content of 10%-40%; (5) placing the crude extract at −20° C. to 8° C. for 0.5 to 12 hours; (6) centrifuging the crude extract to obtain a supernatant; and (7) spray-drying the supernatant to obtain the Hovenia dulcis Thunb extract.

2. The method according to claim 1, wherein, in step (1), the Hovenia dulcis Thunb seeds are dried Hovenia dulcis Thunb seeds, and are crushed and passed through a 20 mesh screen.

3. The method according to claim 1, wherein in step (2), a 30-85% ethanol solution is added in an amount of 3-12 times of the amount of the Hovenia dulcis Thunb powder; and the 30-85% ethanol solution and the Hovenia dulcis Thunb powder are stirred and extracted at 20-70° C. for 1-4 hours twice.

4. The method according to claim 3, wherein in step (2), a 70% ethanol solution is added in an amount of 6 times of the amount of the Hovenia dulcis Thunb powder; and the 70% ethanol solution and the Hovenia dulcis Thunb powder are stirred and extracted at 60° C. for 1 hour twice.

5. The method according to claim 1, wherein in step (3), the extract is subjected to a plate and frame filtration.

6. The method according to claim 1, wherein in the step (4), rotary evaporation is used to remove ethanol at 60-80° C. under a vacuum of 0.06-0.095 Mpa; the crude extract has a solid content of 25%.

7. The method according to claim 1, wherein in the step (5), the crude extract is placed at 0° C. for 3 hours.

8. The method according to claim 1, wherein in the step (6), the crude extract is centrifuged at a centrifugation rate of 2000-5000 r/min.

9. The method according to claim 8, wherein in the step (6), the crude extract is centrifuged at a centrifugation rate of 3000 r/ min for 10 minutes.

10. The method according to claim 1, wherein the Hovenia dulcis Thunb extract has a dihydromyricetin extraction rate of 82.6% and a dihydromyricetin content of 12.2%.

11. A method for preparing a Hovenia dulcis Thunb extract rich in dihydromyricetin, consisting of the following steps: (1) crushing 1 kg of Hovenia dulcis Thunb seeds and passing through a 20 mesh screen to obtain a Hovenia dulcis Thunb powder; (2) adding 6 kg of 70% ethanol solution to the Hovenia dulcis Thunb powder, stirring and extracting at 60° C. for 1 hour twice; (3) filtering to obtain an extract solution via a plate and frame filtration; (4) concentrating the extract solution by evaporating ethanol under reduced pressure to obtain a crude extract, the crude extract having a solid content of 25%; (5) placing the crude extract at 0° C. for 3 hours; (6) centrifuging the crude extract at a centrifugation rate of 3000 r/ min for 10 minutes to obtain a supernatant; and (7) spray-drying the supernatant to obtain the Hovenia dulcis Thunb extract.

12. The method according to claim 111, wherein the Hovenia dulcis Thunb extract has a dihydromyricetin extraction rate of 82.6% and a dihydromyricetin content of 12.2%.

Description

DETAILED DESCRIPTION

EXAMPLE 1

[0034] Taking 1 kg of Hovenia dulcis Thunb seeds, crushing them into coarse powder, passing through a 20 mesh sieve, adding 6 kg of 70% ethanol, stirring and extracting at 60° C. 2 times, 1 h each time, combining the extracts, filtering by a plate and frame filtration, and recovering ethanol under reduced pressure. A crude extract solution with a solid content of 25% was obtained, and the crude extract was refrigerated to stand at 0° C. for 3 h, centrifuged at 3000 r/min for 10 minutes, and the supernatant was collected and directly spray-dried to obtain 94.8 g of Hovenia dulcis Thunb extract. The dihydromyricetin extraction rate was 82.6%, the dihydromyricetin content was 12.2%, the 2% aqueous solution of the extract was clear and translucent, and the turbidity was 0.8 NTU.

EXAMPLE 2

[0035] Taking 1 kg of Hovenia dulcis Thunb seeds, crushing them into coarse powder, passing through a 20 mesh sieve, adding 6 kg of 70% ethanol, stirring and extracting at 60° C. 2 times, 1 h each time, combining the extracts, filtering by a plate and frame filtration, and recovering ethanol under reduced pressure. A crude extract solution with a solid content of 45% was obtained, and the crude extract was refrigerated to stand at 0° C. for 3 h, centrifuged at 3000 r/min for 10 minutes, and the supernatant was collected and directly spray-dried to obtain 166 g of Hovenia dulcis Thunb extract. The dihydromyricetin extraction rate was 80.7%, the dihydromyricetin content was 6.8%, and the 2% aqueous solution of the extract had a large amount of precipitates.

EXAMPLE 3

[0036] Taking 1 kg of Hovenia dulcis Thunb seeds, crushing them into coarse powder, passing through a 20 mesh sieve, adding 6 kg of 30% ethanol, stirring and extracting at 60° C. 2 times, 1 h each time, combining the extracts, filtering by a plate and frame filtration, and recovering ethanol under reduced pressure. A crude extract solution with a solid content of 45% was obtained, and the crude extract was refrigerated to stand at 0° C. for 12 h, centrifuged at 3000 r/min for 10 minutes, and the supernatant was collected and directly spray-dried to obtain 163 g of Hovenia dulcis Thunb extract. The dihydromyricetin extraction rate was 67.6%, the dihydromyricetin content was 5.8%, the 2% aqueous solution of the extract was turbid, and the turbidity was 54 NTU.

COMPARATIVE EXAMPLE

[0037] Taking 1 kg of Hovenia dulcis Thunb seeds, crushing them into coarse powder, passing through a 20 mesh sieve, adding 6 kg of 95% ethanol, stirring and extracting at 60° C. 2 times, 1 h each time, combining the extracts, filtering by a plate and frame filtration, recovering ethanol under reduced pressure, and vacuum-drying to constant weight to obtain 123 g of of Hovenia dulcis Thunb extract. The dihydromyricetin extraction rate was 24.2%, the dihydromyricetin content was 2.7%, the 2% aqueous solution of the extract was turbid, and there were a lot of floating substrates and precipitations.

[0038] The comparison results between the present invention and CN10390979 products are shown in the following table:

TABLE-US-00001 Hovenia dulcis Thunb Dihydromyricetin 2% aqueous solution extract extraction rate % turbidity (NTU) Example 1 82.6   0.8 Example 2 80.7 Precipitates Example 3 67.6 54  CN 10390979 Product 24.2 Floating substrates, turbid solution, precipitates

[0039] It can be seen that the Hovenia dulcis Thunb extract obtained by the present invention has excellent water solubility, high dihydromyricetin content and high yield, and can be used in food, beverages and oral liquids. The process operation is simple and feasible, and is suitable for industrial production.

[0040] Finally, it should be noted that obviously, the above-mentioned embodiments are merely examples for clearly illustrating the present invention, rather than limiting the implementation manners. For those of ordinary skill in the art, other changes or changes in different forms can be made on the basis of the above description. There is no need and cannot give an exhaustive list of all implementation methods. The obvious changes or changes derived from this are still within the protection scope of the present invention.