CN103467557A

CN103467557A - Method for extracting fructus momordicae extract through supercritical fluid

Info

Publication number: CN103467557A
Application number: CN201310410867XA
Authority: CN
Inventors: 苏刘花
Original assignee: Nanjing Zelang Agricultural Development Co Ltd
Current assignee: Nanjing Zelang Agricultural Development Co Ltd
Priority date: 2013-09-11
Filing date: 2013-09-11
Publication date: 2013-12-25

Abstract

The invention relates to a method for extracting mogroside, in particular to a method for extracting mogroside through supercritical CO2. The method is characterized by comprising the following steps: a, crushing fructus momordicae, adding a certain amount of ethanol aqueous solution, adding saccharifying enzyme accounting for 2-5 per mill of the weight of the fructus momordicae, uniformly stirring and stewing the solution for 2-3 h; b, extracting the crushed fructus momordicae through the supercritical CO2 to obtain extract liquor; and c, discharging, centrifugally removing impurities, decoloring and purifying supernatant through macroporous anion resin with strong basicity, eluting the supernatant through ethanol, recycling the ethanol, and carrying out concentrating, spray drying and crushing treatments to obtain a fructus momordicae extract. As tested by an HPLC (High Performance Liquid Chromatography) method, the weight content of mogroside V in the extract obtained by the extraction process is higher than 65%.

Description

A kind of method of supercritical fluid extraction Fructus Monordicae extract

Technical field

The present invention relates to a kind of separation purification method of effective components in plants, particularly a kind of supercritical CO ₂the method of the Fructus Monordicae extract of extraction.

Background technology

Grosvenor Momordica, be described as " angle fruit " by people, be the distinctive precious cucurbitaceous plant of China, have the title of the good fruit of good medicine.Function with clearing heat and moistening lung, cough-relieving, relieve sore throat, laxation defaecation, be usually used in the diseases such as lung-fire cough caused by dryness, pharyngalgia aphonia, the dry constipation of intestines.The main component of Fructus Monordicae extract is mogroside.Effective constituent in mogroside is mainly terpenoid, comprise glycosides III, glycosides IV, glycosides V etc., wherein the mogroside V is the main component of its sweet taste, sugariness is 256 ~ 344 times of sucrose, soluble in water, the ethanol isopolarity solvent because it is combined with glycosyl, being insoluble in the organic solvents such as acetone, ethyl acetate, is the unformed powder of white.Relevant research shows, mogroside has good health-care effect, more remarkable to the effect that promotes stomach function and clearing and antitussive, laxation toxin expelling, tender skin benefit face, clearing heat and moistening lung, can be widely used in the industries such as dietary supplements, food, medicine.

At present, the extracting method about Fructus Monordicae extract mainly contains: (1) water extraction resin isolation method; (2) alcohol extracting membrane separation process (comprising that ultrasonic wave or microwave-assisted extract); (3) method that also someone adopts heating to extract, but in leaching process, excess Temperature can increase the impurity of leaching, the color burn of extracting solution, and be unfavorable for follow-up decolorization and purification treatment.All there is complicated operation in above several method, resulting extract color and luster is dark and have strong taste of traditional Chinese medicine and the strong shortcoming that rear bitter taste, active constituent content are low, energy consumption is large, production cost is high.

Summary of the invention

The object of the invention is to the existing defect of method for preparing the high-content mogroside for existing, but provide, a kind of technique is simple, efficiency is high, the separation purification method of the low realization of industrialization of energy consumption.

Technical scheme of the present invention is carried out according to the following step:

1. the Grosvenor Momordica dry fruit is pulverized, added 30% ~ 50% aqueous ethanolic solution of 2 ~ 3 times of Grosvenor Momordica weight, then add the saccharifying enzyme of Grosvenor Momordica weight 2 ~ 5 ‰, stir, standing 2 ~ 3h;

2. by the mixture supercritical CO after standing ₂extraction, obtain the extracting solution that contains mogroside, and actual conditions is: CO ₂flow is 5 ~ 10L/h, extracts pressure 15 ~ 20MPa, 35 ~ 45 ℃ of temperature, and the pressure in separating still is 5 ~ 10MPa, and temperature is 40 ~ 60 ℃, and extraction time is 3 ~ 5h;

3. discharging, centrifugal removal of impurities, supernatant liquor advances macroporous adsorbent resin, the washing polymeric adsorbent is colourless to effluent liquid, then uses 50% ~ 60% ethanolic soln wash-out of 8 ~ 10 times of weight resins, removes pigment and impurity, collect ethanol eluate, reclaim ethanol, spraying drying obtains white crystalline powder.

Macroreticular resin described in step 3 is ADS-4, ADS-5, ADS-7, ADS-17 etc.

Compared with prior art, the present invention adopts supercritical CO ₂cO used in the method for mogroside in the extraction Grosvenor Momordica ₂purity is more than or equal to 99%, CO ₂for rare gas element, can operate at normal temperatures, can effectively prevent oxidation and the decomposition of thermo-sensitivity composition and chemically unstable composition, utilize CO ₂the character that the high-density had under supercritical state, low viscosity and spread coefficient are large is extracted the effective constituent in Grosvenor Momordica, then in the method heated up with step-down, will be dissolved in CO ₂solute in fluid separates, and plays the dual function of extracting and distilling.The method operational cycle is short, extraction yield is high, can avoid the residual of organic solvent simultaneously, in addition, and due to CO ₂cheap and easy to get, general recyclable 80%, saved the energy, simultaneously due to CO ₂without incendivity, use safety and environmentally safe.With the mogroside of the method extraction, wherein the content of mogroside V reaches more than 65%, and effect of extracting is obvious.

Embodiment

Embodiment 1: the Grosvenor Momordica dry fruit is pulverized, added 30% aqueous ethanolic solution of 2 times of Grosvenor Momordica weight, then add the saccharifying enzyme of Grosvenor Momordica weight 2 ‰, stir, standing 2h; By the mixture supercritical CO after standing ₂extraction, obtain the extracting solution that contains mogroside, and actual conditions is: CO ₂flow is 8L/h, extracts pressure 15MPa, 35 ℃ of temperature, and the pressure in separating still is 8MPa, and temperature is 50 ℃, and extraction time is 4h; Discharging, centrifugal removal of impurities, supernatant liquor advances ADS-17 type macroporous adsorbent resin, the washing polymeric adsorbent is colourless to effluent liquid, then uses 50% ethanolic soln wash-out of 8 times of weight resins, removes pigment and impurity, collect ethanol eluate, reclaim ethanol, spraying drying obtains white crystalline powder.Through HPLC, detect, the content of mogroside V is 64.1%.

Embodiment 2: the Grosvenor Momordica dry fruit is pulverized, added 50% aqueous ethanolic solution of 2.5 times of Grosvenor Momordica weight, then add the saccharifying enzyme of Grosvenor Momordica weight 5 ‰, stir, standing 3h; By the mixture supercritical CO after standing ₂extraction, obtain the extracting solution that contains mogroside, and actual conditions is: CO ₂flow is 10L/h, extracts pressure 18MPa, temperature 45 C, and the pressure in separating still is 9MPa, and temperature is 40 ℃, and extraction time is 5h; Discharging, centrifugal removal of impurities, supernatant liquor advances ADS-7 type macroporous adsorbent resin, the washing polymeric adsorbent is colourless to effluent liquid, then uses 55% ethanolic soln wash-out of 10 times of weight resins, removes pigment and impurity, collect ethanol eluate, reclaim ethanol, spraying drying obtains white crystalline powder.Through HPLC, detect, the content of mogroside V is 67.6%.

Embodiment 3: the Grosvenor Momordica dry fruit is pulverized, added 40% aqueous ethanolic solution of 3 times of Grosvenor Momordica weight, then add the saccharifying enzyme of Grosvenor Momordica weight 4 ‰, stir, standing 2.5h; By the mixture supercritical CO after standing ₂extraction, obtain the extracting solution that contains mogroside, and actual conditions is: CO ₂flow is 9L/h, extracts pressure 20MPa, 40 ℃ of temperature, and the pressure in separating still is 10MPa, and temperature is 60 ℃, and extraction time is 3h; Discharging, centrifugal removal of impurities, supernatant liquor advances ADS-5 type macroporous adsorbent resin, the washing polymeric adsorbent is colourless to effluent liquid, then uses 60% ethanolic soln wash-out of 9 times of weight resins, removes pigment and impurity, collect ethanol eluate, reclaim ethanol, spraying drying obtains white crystalline powder.Through HPLC, detect, the content of mogroside V is 65.3%.

Claims

1. the method for a supercritical fluid extraction Fructus Monordicae extract, is characterized in that, comprises the steps:

A. the Grosvenor Momordica dry fruit is pulverized, added aqueous ethanolic solution, then add the saccharifying enzyme of Grosvenor Momordica weight 2 ~ 5 ‰, stir, standing 2 ~ 3h;

B. by the mixture supercritical CO after standing ₂extraction, obtain the extracting solution that contains mogroside, and actual conditions is: CO ₂flow is 5 ~ 10L/h, extracts pressure 15 ~ 20MPa, 35 ~ 45 ℃ of temperature, and the pressure in separating still is 5 ~ 10MPa, and temperature is 40 ~ 60 ℃, and extraction time is 3 ~ 5h;

C. discharging, centrifugal removal of impurities, supernatant liquor adopt macroporous adsorbent resin to extract decoloured, removal of impurities, then use 50 ~ 60% ethanolic soln wash-out, through concentrated, spraying drying, obtain white crystalline powder.

2. mogroside supercritical extraction method according to claim 1, is characterized in that, the aqueous ethanolic solution in step a is the ethanolic soln that volume ratio is 30 ~ 50%, and solid-liquid ratio is 1:2 ~ 1:3.

3. mogroside supercritical extraction method according to claim 1, is characterized in that, the macroreticular resin described in step c is ADS-4, ADS-5, ADS-7, ADS-17 etc.

4. mogroside supercritical extraction method according to claim 1, is characterized in that, the ethanolic soln described in step c is weight resin 8 ~ 10 times, volume ratio is 50 ~ 60%.