Method for preparing geniposide in eucommia leaf

A technology of geniposide and Eucommia ulmoides leaves is applied in the field of preparing geniposide from Eucommia ulmoides leaves, which can solve the problems of large amount of waste water, low product purity, low extraction rate and the like, and achieves low water extraction temperature and simple membrane operation process. , the effect of shortening the extraction time

Inactive Publication Date: 2014-05-14
HUBEI LAOLONGDONG DUZHONG DEV
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Problems solved by technology

[0004] In order to overcome the problems and shortcomings in the above-mentioned prior art, the present invention provides a method for preparing geniposide from Eucommia leaves. Extract geniposide from Eucommia ulmoides leaves, then separate and purify the extracted geniposide through two-stage membrane separation technol...
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Abstract

The invention discloses a method for preparing geniposide in eucommia leaf. The method comprises the following steps of crushing eucommia leaf, carrying out cellulase-assistant middle temperature-water extraction, carrying out routine filtration, carrying out ultrafilter membrane impurity-removal, carrying out nanofiltration condensation, carrying out macroporous resin-based separation purification, carrying out condensation and carrying out drying to obtain geniposide powder. The method utilizes cellulase-assistant middle temperature-water extraction of geniposide in eucommia leaf, has an extraction rate of 95%, a low water extraction temperature and short extraction time, utilizes an ultrafilter membrane to remove impurities and separate other side products in the extract, has simple membrane processes and realizes long-term membrane flux stabilization, easy membrane cleaning, a long service life and industrialization. Through the nanofiltration membrane, the extract subjected to impurity removal is concentrate d so that follow-up technical load is reduced and a resin service life is prolonged. Through the method, a nanofiltrated liquid has a COD value <=100 and can be reused in production and basically, waste water is not produced. Through the macroporous adsorption resin, geniposide can be effectively purified. The powder produced by the method has geniposide purity greater than 80% and an extraction rate more than 1.2%.

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  • Method for preparing geniposide in eucommia leaf

Examples

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Example Embodiment

[0024] Example 1. See the instructions attached figure 1 , Take 10Kg of dried Eucommia leaves, pulverize and pass through 80 mesh sieve, add 120Kg of water, adjust the temperature to 55℃, keep the temperature constant and adjust the pH to 4.5, then add 10g of cellulase, extract 60min under these conditions, filter, filter the residue again Extract for the second time according to the aforementioned extraction conditions, combine the two filtrates, and routinely filter. The extraction rate of geniposide is 95.8%; the operating conditions are P=0.3Mpa, T=45℃, PH=4.5, Q=70L/min The filtrate was passed through a 0.03μm ultrafiltration membrane, the extract was concentrated 11.2 times under this condition, and the average flux of the ultrafiltration membrane was 226.3L/m 2 ·H; Under the operating conditions P=1.5Mpa, T=50℃, PH=4.5, Q=20L/min, the ultrafiltration filtrate is then passed through a 200 molecular weight nanofiltration membrane, the ultrafiltration filtrate is concentrated 16.6 times under this condition, inorganic The salt ion removal rate is 63%, and the average flux of the nanofiltration membrane is 18.7L/m 2 ·H, the COD of the nanofiltration filtrate is 94; the nanofiltration concentrate is purified by D301R resin, first eluting impurities with 2 times the volume of the resin column, and then eluting with 2.5 times the volume of the resin at a concentration of 70% ethanol After collecting the ethanol eluates under reduced pressure and vacuum drying (the temperature of vacuum concentration and vacuum drying are not higher than 60℃), geniposide powder can be obtained. The purity of geniposide is 82.5% by HPLC. The rate is 1.35%.
[0025] Example 2: See the attachment figure 1 , Take 10Kg of dried eucommia leaves, pulverize and pass through an 80-mesh sieve, add 120Kg of water, adjust the temperature to 50℃, keep the temperature constant and adjust the pH to 4.5, then add 10g of cellulase, extract 80min under these conditions, filter, and filter the residue again Extract for the second time according to the aforementioned extraction conditions, combine the two filtrates, and routinely filter. The extraction rate of geniposide is 95.3%; the operating conditions are P=0.3Mpa, T=45℃, PH=4.5, Q=70L/min The filtrate was passed through a 0.02μm ultrafiltration membrane, and the extract was concentrated 12.8 times under this condition. The average flux of the ultrafiltration membrane was 221.3L/m 2 ·H; Under the operating conditions P=1.5Mpa, T=50℃, PH=4.5, Q=20L/min, the ultrafiltration filtrate is then concentrated through a 400 molecular weight nanofiltration membrane, and the ultrafiltration membrane filtrate is concentrated 15.2 times under these conditions , The removal rate of inorganic salt ions is 60%, and the average flux of the nanofiltration membrane is 19.5L/m 2 ·H, the COD of the nanofiltration filtrate is 91; the nanofiltration concentrate is purified by H103 resin, first eluting impurities with 2 times the volume of the resin column, and then eluting with 2.5 times the volume of the resin at a concentration of 70% ethanol After collecting the ethanol eluate under reduced pressure and vacuum drying (the temperature of vacuum concentration and vacuum drying are not higher than 60℃), geniposide powder can be obtained. The purity of geniposide is 83.6% by HPLC. The rate is 1.21%.
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