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Extraction method for high purity rubusoside

An extraction method and technology of rubusoside, which is applied in the field of high-purity rubusoside extraction, can solve the problems of incomplete alcohol precipitation, prolong the filtration cycle, and high production cost, and achieve the effects of shortening the production cycle, simplifying the process and low production cost

Active Publication Date: 2015-11-18
HUNAN HUACHENG BIOTECH
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AI Technical Summary

Problems solved by technology

[0004] CN102702284A discloses a production method of high-purity rubusoside. The method is to extract, concentrate, flocculate and clarify sweet tea raw materials, centrifuge, and then undergo adsorption and separation of macroporous resins, ion resin exchange decolorization, desalination, compound decolorization, and concentrate The product is dried and prepared with a purity of 98%, but the yield is only 3.7-4.5%, and the process is complicated and the loss is large, resulting in a very low yield of the final product
[0005] CN102838644B discloses a production method for extracting rubusoside from sweet tea leaves. The method is to carry out ultrasonic-assisted extraction of sweet tea raw materials, alcohol precipitation and filtration after concentration under reduced pressure, adsorption and separation by macroporous resin, polyamide resin chromatography, crystallization And recrystallization to obtain the product, the product purity reaches more than 98%, and the yield is about 3.7-3.9%. This method has a low yield of the final product due to incomplete alcohol precipitation and incomplete elution of polyamide
[0006] CN104262425A discloses a new method for extracting rubusoside. The method is to carry out water extraction of sweet tea raw materials, and after membrane filtration, the product is obtained through macroporous resin adsorption separation, anion and cation resin separation, concentration, crystallization and recrystallization, and the product purity reaches 99%, and the yield is about 5.31%. Due to the repeated use of acid-base treatment during the adsorption and separation of macroporous resins, the subsequent treatment process is increased, the production cycle is prolonged, and higher requirements are placed on the equipment. The production cost Relatively high
[0007] CN104558088A discloses a method of using microwave countercurrent extraction, through multi-stage filtration, macroporous resin adsorption separation, membrane filtration, concentration, and drying, to obtain the process of mogroside V60% product, but in multi-stage filtration, use centrifugal It is carried out with multi-stage ultrafiltration, which increases the process, prolongs the filtration cycle, has low efficiency, and consumes a lot of energy. In addition, after purification by macroporous resin, it also contains a large amount of impurities. Nanofiltration is used to remove inorganic salts and solvents. , in order to achieve the purpose of concentration, the pressure in the process is high, the energy consumption is large, the damage to the membrane is also large, and the extraction efficiency and process cost are not good.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] (1) Pre-treatment: remove impurities from 500kg of dried sweet tea raw materials (rubusaside content: 6.42%), pulverize them, and pass through a 40-mesh sieve to obtain sweet tea raw material powder;

[0038] (2) Microwave countercurrent extraction: 500kg of sweet tea raw material powder obtained in step (1) was subjected to microwave countercurrent extraction with 3295L deionized water at 90°C, microwave power 900w, and frequency 5000MHz for 60min, and the flow of material and water was reversed. Continuous dynamic flow, to get 3125kg extract;

[0039](3) Centrifugation: The 3125kg extract obtained in step (2) was rapidly cooled to 20°C through a plate-and-frame heat exchanger, and then spirally centrifuged with a horizontal spiral centrifuge at a centrifugal rate of 5000r / min, and then used a tubular type The centrifuge performs tubular centrifugation at a centrifugal rate of 14000r / min to obtain 3120kg of centrifugate;

[0040] (4) Macroporous resin adsorption separ...

Embodiment 2

[0046] (1) Pre-treatment: remove impurities from 500kg of dry sweet tea raw materials (rubusaside content is 6.45%), pulverize them, and pass through a 20-mesh sieve to obtain sweet tea raw material powder;

[0047] (2) Microwave countercurrent extraction: 500kg of sweet tea raw material powder obtained in step (1) was subjected to microwave countercurrent extraction with 3298L deionized water for 40min at 70°C, with a microwave power of 900w and a frequency of 7000MHz, and the flow of material and water was reversed. Continuous dynamic flow, to get 3133kg extract;

[0048] (3) Centrifugation: The 3133kg extract obtained in step (2) was rapidly cooled to 25°C through a plate-and-frame heat exchanger, and then spirally centrifuged with a horizontal spiral centrifuge at a centrifugal rate of 3000r / min, and then used a tubular type The centrifuge performs tubular centrifugation at a centrifugal rate of 12000r / min to obtain 3125kg of centrifugate;

[0049] (4) Macroporous resin a...

Embodiment 3

[0055] (1) Pre-treatment: remove impurities from 500kg of dried sweet tea raw materials (rubusaside content is 6.51%), pulverize them, and pass through a 30-mesh sieve to obtain sweet tea raw material powder;

[0056] (2) Microwave countercurrent extraction: 500kg of sweet tea raw material powder obtained in step (1) was subjected to microwave countercurrent extraction with 3290L deionized water for 50min at 80°C, with a microwave power of 800w and a frequency of 6000MHz, and the flow of material and water was reversed. Continuous dynamic flow, to obtain 3127kg extract;

[0057] (3) Centrifugation: The 3127kg extract obtained in step (2) was rapidly cooled to 23°C through a plate-and-frame heat exchanger, and then spirally centrifuged with a horizontal screw centrifuge at a centrifugal rate of 3000r / min, and then used a tubular type The centrifuge carries out tubular centrifugation at a centrifugal rate of 12000r / min to obtain 3122kg of centrifugate;

[0058] (4) Macroporous ...

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Abstract

The present invention discloses an extraction method for high purity rubusoside. The extraction method comprises the following steps: (1) pre-treatment: removing impurities from a dried sweet tea raw material, and smashing, sieving and obtaining the dried sweet tea raw material to sweet tea raw material powder; (2) microwave counter-current extraction: performing microwave counter-current extraction on the sweet tea raw material, extruding extracted residues, and mixing and filtering an extruding liquid and a sweet tea feed liquid to obtain an extracting liquid; (3) performing centrifugation to obtain centrifugate; (4) macroporous resin adsorptive separation: adjusting the pH value of the centrifugate to 10.0-11.0, passing the centrifugate through macroporous resin for adsorption, and after leaving the centrifugate to stand, performing water-washing and eluting to collect a target eluent; (5) performing ultra-filtration to obtain ultrafiltrate; (6) performing concentration to obtain a concentrate; and (7) crystallization and recrystallization: adding an organic solvent into the concentrate for crystallization, then performing recrystallization and drying to obtain a rubusoside product. According to the rubusoside product obtained by the method provided by the invention, the purity is greater than or equal to 99%, and the yield is greater than or equal to 5.35%. The extraction method provided by the present invention is simple and convenient in process, short in period, low in energy consumption and production cost and can be used for continuous extraction, and is suitable for continuous production in a factory.

Description

technical field [0001] The invention relates to a method for extracting rubusoside, in particular to a method for extracting high-purity rubusoside suitable for industrial production. Background technique [0002] Sweet tea is the sweet tea of ​​the genus Rubus of Rosaceae ( Rubus Suatrssimus S. Lee ) dry leaves, mainly distributed in the Dayao Mountains of Guangxi, and a small amount of planting in Guangdong, Hunan, Jiangxi and other places. It is sweet and has the effects of anti-pollen allergy, promoting insulin secretion, and preventing and treating cardiovascular diseases. Its main component is rubusoside, whose sweetness is about 300 times that of sucrose, and its calorific value is 5% of that of sucrose. It is mainly used as a sweetener , widely used in food, beverage and other industries, because of its remarkable characteristics of high sweetness and low calorific value, it is quite popular in the market. [0003] At present, the domestic research on extracting hi...

Claims

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Application Information

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IPC IPC(8): C07H15/256C07H1/08
Inventor 唐方华欧阳逸斌黄华学
Owner HUNAN HUACHENG BIOTECH
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