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A kind of extraction method of high-purity rubusoside

An extraction method and rubaside technology are applied in the extraction field of high-purity rubaside, which can solve the problems of prolonging the filtration cycle, incomplete alcohol precipitation, prolonging the production cycle, etc. Effect

Active Publication Date: 2018-06-08
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 500 kg of dried sweet tea raw materials (the content of rubusoside is 6.42%), crush them, and pass through a 40-mesh sieve to obtain sweet tea raw material powder;

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

[0039](3) Centrifugation: The 3125 kg 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 tube Type centrifuge carries out tubular centrifugation with centrifugal speed 14000r / min, obtains 3120kg centrifugate;

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

Embodiment 2

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

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

[0048] (3) Centrifugation: The 3133 kg 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 tube Type centrifuge carries out tubular centrifugation with centrifugal rate 12000r / min, obtains 3125kg centrifugate;

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

Embodiment 3

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

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

[0057] (3) Centrifugation: The 3127 kg 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 spiral centrifuge at a centrifugal rate of 3000r / min, and then used a tube Type centrifuge carries out tubular centrifugation with centrifugal rate 12000r / min, obtains 3122kg centrifugate;

[0058] (4) Macroporous resin adso...

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Abstract

A high-purity rubusoside extraction method, comprising the following steps: (1) Pretreatment: removing impurities from dried sweet tea raw materials, crushing, and sieving to obtain sweet tea raw material powder; (2) Microwave countercurrent extraction: microwave sweet tea raw material powder Countercurrent extraction, extruding the extraction slag, mixing the extruded liquid with the sweet tea material liquid, filtering to obtain the extract; (3) centrifuging to obtain the centrifuge; (4) macroporous resin adsorption separation: adjust the pH of the centrifuge to 10.0~ 11.0, adsorbed by macroporous resin, washed with water after standing still, eluted, and collected the target eluent; (5) ultrafiltrated to obtain ultrafiltrate; (6) concentrated to obtain concentrated solution; (7) crystallization and recrystallization: to An organic solvent is added to the concentrated solution for crystallization, recrystallization and drying to obtain rubusoside. The rubusoside product obtained according to the method of the invention has a purity of ≥99% and a yield of ≥5.35%. The process of the invention is simple, the cycle is short, the energy consumption and production cost are low, continuous extraction is possible, and it is suitable for continuous production in factories.

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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Patent Type & Authority Patents(China)
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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