CN1939458B - Preparation of gardenia jasminoides by macroporous adsorbing resin - Google Patents
Preparation of gardenia jasminoides by macroporous adsorbing resin Download PDFInfo
- Publication number
- CN1939458B CN1939458B CN200610200965A CN200610200965A CN1939458B CN 1939458 B CN1939458 B CN 1939458B CN 200610200965 A CN200610200965 A CN 200610200965A CN 200610200965 A CN200610200965 A CN 200610200965A CN 1939458 B CN1939458 B CN 1939458B
- Authority
- CN
- China
- Prior art keywords
- fructus gardeniae
- extract
- membrane separation
- resin
- macroporous adsorbent
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Landscapes
- Separation Using Semi-Permeable Membranes (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
A process for preparing the extract from capejasmine fruit by use of macroreticular adsorption resin includes such steps as extracting in hydrophilic solvent to obtain coarse extract, membrane separation for removing impurities, adding water to become suspension, adsorbing by macroreticular resin, water washing for removing polar impurities, eluting with the aqueous solution of hydrophilic solvent, vacuum recovery of solvent, and vacuum concentrating.
Description
Technical field
The present invention relates to a kind of from plant the Green Chemistry preparation method of separation and purification medicinal active ingredient, more specifically relate to a kind of method that adopts macroporous adsorbent resin to prepare Fructus Gardeniae extract.
Background technology
Fructus Gardeniae is the fruit of Gardenia Ellis (Gardenia) Rubiaceae (Rubiaceae) evergreen shrubs Fructus Gardeniae; be the large Chinese medicine material of China; the selected first batch of medicinal and edible Chinese medicine material of ministry of Health of China register; main pharmacodynamics composition for national Chinese medicine protection kind QINKAILING ZHUSHEYE, Radix Gentianae eliminating pathogen in the liver sheet and YINDAN PINGGAN JIAONANG; be the choice drug of tcm clinical practice treatment icterohepatitis and the raw material that extracts the Fructus Gardeniae natural pigment, abound with in Fujian, province mountain areas such as Zhejiang, Jiangxi, emblem, Hunan.
Fructus Gardeniae from Compendium of Material Medica to " successive dynasties such as Chinese pharmacopoeia medicine masterpiece is all on the books.Fructus Gardeniae is for oral administration to have functions such as pathogenic fire purging relieving restlessness, clearing away heat and promoting diuresis, removing pathogenic heat from blood and toxic substance from the body, and external can be treated and be sprained, dampens, and the clinical application history reaches 1600 years in China.
Fructus Gardeniae contains medicinal active ingredients such as iridoid glycoside compounds, carotenoid compounds and organic acid.Wherein, be the iridoid glycoside compounds and the chlorogenic acid of main constituent with jasminoidin, have function of gallbladder promoting hepatoprotective, effects for removing toxic heat, be the wide Chinese medicine extract of market prospect, be widely used in tcm clinical practice treatment icterohepatitis.
Gardenia Yellow is the water-soluble carotenoid class natural pigment of the unique existence of nature of extracting from cape jasmine fruit, and main component is carotenoid compounds such as crocin and crocetin, also may have ursolic acid, jasminoidin and chlorogenic acid in the finished product.。
Gardenia Yellow has that strong coloring force, lovely luster, tone are soft naturally, good stability, dissolubility are strong, free from extraneous odour, have no side effect, the security performance advantages of higher, be widely used in food, fruit wine, beverage, medicine, daily-use chemical industry, cosmetics etc., being popular in the world at present natural additive for foodstuff, is herbal industry, beverage/food industry, cosmetics industry, the indispensable natural pigment raw material of pharmaceutical industries.
With the jasminoidin is raw material, adopts microbiological transformation technology can also produce the Fructus Gardeniae genipin.On this basis, utilize the reaction of Fructus Gardeniae genipin and aminoacid, also can produce gardenia blue pigment.The gardenia blue pigment dissolubility is good, and strong coloring force belongs to the water-soluble natural pigment.In the process of producing the natural gardenia cyanine, control different conversion conditions and also can produce the natural gardenia red pigment.By Gardenia Yellow, indigo plant, red three-primary colours, can modulate pigments such as, Fructus Gardeniae purple green such as Fructus Gardeniae.Therefore, carry out the intensive processing exploitation of natural pigment raw material Fructus Gardeniae, preparation contains the Fructus Gardeniae extract of compositions such as iridoid glycoside compounds, carotenoid compounds or organic acid, has vast market prospect.
Fructus Gardeniae gives birth to the type plant for high yield speed, and adaptability is extremely strong, get final product artificial growth, also can be wild in intermountain.Usually, plant and can bear fruit in the 2nd～3 year, the fresh fruit per mu yield can reach 200～250Kg, plants promptly to enter high yield period on the 4th～5 year, and the fresh fruit per mu yield can reach 1500～2000Kg.
In China, the Fructus Gardeniae aboundresources, cheap and easy to get, drug effect is clear and definite, and among the people being widely used in food and the medicine is rare large natural medicinal plant resource.But the annual whole nation has the Fructus Gardeniae of counting with ten thousand tons rationally to utilize, and has wasted valuable resource.For realizing the efficient utilization of Fructus Gardeniae resource and the sustainable development of production conscientiously, research is the preparation method and the purposes of the Fructus Gardeniae extract of main component with Fructus Gardeniae iridoid glycoside compounds, carotenoid compounds or organic acid, has certain directive significance for comprehensive utilization and the series product development of Fructus Gardeniae.
The present invention will provide that a kind of equipment is simple, resin long service life, separation and purification is effective, product yield is high, production cost is low Fructus Gardeniae extract preparation method.
Summary of the invention
The object of the present invention is to provide a kind of method that adopts macroporous adsorbent resin to prepare Fructus Gardeniae extract, this method not only helps the yield and the quality that are further purified, greatly improve product of Fructus Gardeniae iridoid glycoside compounds, carotenoid compounds or organic acid isoreactivity composition, and can obviously prolong service life, the reduction preparation cost of macroporous adsorbent resin.
The method that employing macroporous adsorbent resin of the present invention prepares Fructus Gardeniae extract is achieved in that and comprises the membrane separation for removing impurities step that adopts hydrophilic solvent to extract Fructus Gardeniae crude extract and Fructus Gardeniae crude extract, it is characterized in that: with the Fructus Gardeniae crude extract or through the Fructus Gardeniae extract of membrane separation purification is raw material, add water and become suspension, adopt absorption with macroporous adsorbent resin to saturated, wash depolarization impurity with water, reuse hydrophilic solvent eluting target substance, filtrate becomes the Fructus Gardeniae extract through resin separation purification through decompression and solvent recovery, vacuum concentration.
The major advantage of preparation method of the present invention is:
The one, can effectively remove protein and polysaccharide and other macromole impurity by membrane separation technique, thereby make the Fructus Gardeniae crude extract that contains main medicinal active ingredient such as Fructus Gardeniae iridoid glycoside compounds, carotenoid compounds or organic acid obtain further purification, and help the preservation of these goods.
The 2nd, can effectively remove protein and polysaccharide and other macromole impurity by membrane separation technique, thereby help subsequent technique and adopt macroporous adsorbent resin or the further separation and purification Fructus Gardeniae iridoid glycoside of polyamide compounds, main medicinal active ingredient such as carotenoid compounds or organic acid, macroporous adsorbent resin or the polyamide separation and purification efficient to main medicinal active ingredient will obviously be improved, the saturated extent of adsorption of unit resin or polyamide will obviously be improved, with the service life of significant prolongation macroporous adsorbent resin or polyamide, can greatly improve the yield and the quality of product, significantly reduce the preparation cost of product.
The 3rd, combination adopts hydrophilic solvent to extract, the technology of membrane separation for removing impurities, can not only suitability for industrialized production Fructus Gardeniae crude extract or membrane separation purification after Fructus Gardeniae extract, and the concentrated solution behind the membrane separation for removing impurities of macromole impurity such as rich in proteins and polysaccharide can be further used for preparing Fructus Gardeniae fertilizer or Fructus Gardeniae feedstuff additive product after simple fermentation process, thereby safety veritably, easy, rationally, realize the full constituent comprehensive utilization of Fructus Gardeniae and the suitability for industrialized production of series of products economically, demonstrate fully the theory of Green Chemistry production and the strategy of recycling economy, it is theoretical novel to have, technology is reasonable, handling safety, technology is easy, economically feasible, advantages of environment protection.
The present invention preferentially selects for use the advantage of methanol or acetone to be: the extraction effect of hydrophilic solvents such as methanol, ethanol, propanol, isopropyl alcohol, acetone or different pH value buffer solution is suitable, but for other hydrophilic solvent, the boiling point of methanol or acetone is lower, energy consumption is littler, can significantly reduce the preparation cost of product.
The main medicinal active ingredient that the present invention adopts modernization of Chinese medicine production technology to extract Fructus Gardeniae is made the Chinese medicine extract of the current international practice, " three-hypers ", " three is little " and advantages such as " three just " with modern Chinese medicine product, energy adapts to and satisfies modern Chinese medicine clinical application demand, meets the modernization of Chinese medicine and international industrial policy that country advocates.
The specific embodiment
The present invention adopts macroporous adsorbent resin to prepare the method for Fructus Gardeniae extract, the hydrophilic solvent that comprises the Fructus Gardeniae crude extract extracts and the membrane separation for removing impurities step, it is characterized in that: with the Fructus Gardeniae crude extract or through the Fructus Gardeniae extract of membrane separation purification is raw material, add water and stir into suspension, make suspension proportion reach 1.05～1.18, extremely saturated with absorption with macroporous adsorbent resin then, earlier with water (V/V) the flush away polar impurity that is no less than 2 times of amount of resin, the hydrophilic solvent aqueous solution of 30～60% final concentrations of 4～8 times of amount of resin of reuse with 1～3 times of amount of resin/hour flow velocity (V/V) eluting target substance, filtrate-0.05～-0.09MPa, under 50～65 ℃ of conditions, through decompression and solvent recovery, vacuum concentration becomes the Fructus Gardeniae extract through resin separation purification.
The chemical composition of the skeleton of above-mentioned macroporous adsorbent resin can be one or more in polystyrene, polyacrylic acid or the phenolic aldehyde, preferentially selects polystyrene or polyacrylic acid for use.
Above-mentioned macroporous adsorbent resin can be HZ801, HZ802, HZ803, the HZ806 of polystyrene skeleton, among HZ816, the HZ818 one or more.Also can be D101, the DK110 of polyacrylic acid skeleton, among the D113 one or more.
The method that employing membrane separation technique of the present invention prepares Fructus Gardeniae extract is achieved in that the Fructus Gardeniae crude extract that extracts with hydrophilic solvent is a raw material, add water and become suspension, make suspension proportion reach 1.03～1.22, under 0.25～0.75MPa,, remove the Fructus Gardeniae extract that promptly gets behind protein and polysaccharide and other macromole impurity behind the membrane separation purification through membrane separation for removing impurities.
Above-mentioned membrane separation for removing impurities process can be selected the diffusion barrier of 6000 molecular cut offs～0.22 μ m membrane aperture for use.
The separation membrane material of above-mentioned membrane separation for removing impurities process can be one or more hybrid films materials in mineral-type, polysulfones, fluoro-containing macromolecule material class, TPO, polyamide-based, chitin kind or the cellulose family membrane material, preferentially selects inorganic ceramic film, polysulfone membrane or polyvinylidene fluoride film for use.
The method that employing hydrophilic solvent of the present invention extracts the Fructus Gardeniae crude extract is: with bright Fructus Gardeniae or Cape Jasmine Fruit is raw material, adopt 25～75% hydrophilic solvent aqueous solutions of 5～15 times of Fructus Gardeniae dry weights (W/W), under 50～80 ℃ of conditions, extract 1～3 time, each 1～3 hour, merge extractive liquid,, filter, filtrate becomes Fructus Gardeniae extract through decompression and solvent recovery, vacuum concentration under-0.06～0.095MPa, 50～80 ℃ of conditions.
Above-mentioned hydrophilic solvent can be one or more mixed solvents of methanol, ethanol, propanol, isopropyl alcohol or acetone, wherein preferentially selects methanol or acetone for use, and hydrophilic solvent also can be different pH value buffer solution.
The physical and chemical parameter assay method of each prepared product of the present invention is as follows:
(1) Fructus Gardeniae iridoid glycoside compounds, carotenoid compounds and chlorogenic acid contents adopt the high performance liquid chromatograph mensuration that the ultraviolet-visible three-wavelength detects simultaneously.Condition determination: Agilent 1100 type high performance liquid chromatographs (DAD diode array detector), Waters Nova-Pak C18 chromatographic column (Ф 3.9 * 150mm, 5 μ m), methanol-0.2% phosphate aqueous solution is that mobile phase is carried out gradient elution, the methanol ratio rises to 100% from 15% linear gradient in 60min, keeps 2min then.Flow velocity 1.0mL/min, 34 ℃ of column temperatures, sample size 20 μ L.The detection wavelength of carotenoid compounds, chlorogenic acid and Fructus Gardeniae iridoid glycoside compounds is respectively 440nm, 320nm and 238nm.
Standard substance: jasminoidin, different jasminoidin, gardenia acid, genipin gentiobiose glycosides are purchased in Yoneyama company (Japan), and crocetin is purchased the company in Sigma, and chlorogenic acid, crocin are purchased in Nat'l Pharmaceutical ﹠ Biological Products Control Institute.
After measured, the used Fujian of the experiment content that produces main medicinal active ingredients such as Fructus Gardeniae iridoid glycoside compounds, carotenoid compounds and chlorogenic acid in the Fructus Gardeniae (water content 5.3%) is respectively 69.8～77.3g/kg, 2.1～3.9g/kg and 12.3～15.6g/kg.
(2) measurement of the polysaccharide content: adopting the phenolsulfuric acid method, is contrast with glucose or D-galactose.
(3) mensuration of protein content: adopting FoLin-phenol method to measure, is contrast with the bSA.
The embodiment of preparation method of the present invention is presented below:
Embodiment 1
Producing Fructus Gardeniae with Fujian is raw material, with the washing of bright Fructus Gardeniae, dry (air-dry, all can dry or dry), pulverize, cross 20～30 mesh sieves and get Cape Jasmine Fruit, the 2.9kg Cape Jasmine Fruit is put into extraction pot, methanol-acetone (1: 1) aqueous solution of 40% with 10 times of dry weights of Cape Jasmine Fruit (W/W), reflux, extract, is 3 times under 68 ℃ of conditions, each 2 hours, merge extractive liquid,, filter, filtrate-0.06～-0.095MPa, 50～80 ℃ of conditions under, become Fructus Gardeniae extract through decompression and solvent recovery, vacuum concentration.After measured, Fructus Gardeniae iridoid glycoside compounds, carotenoid compounds and chlorogenic acid extraction ratio are respectively 93.2%, 96.3% and 93.1%.
Then, earlier the Fructus Gardeniae crude extract is added suitable quantity of water and stir into suspension, make suspension proportion reach 1.03, adopting molecular cut off then is 6000 polysulfone membrane, under 0.75MPa, carry out membrane separation for removing impurities, remove the Fructus Gardeniae extract that promptly gets behind protein and polysaccharide and other macromole impurity behind the membrane separation purification.After measured, the response rate of Fructus Gardeniae iridoid glycoside compounds, carotenoid compounds and chlorogenic acid is respectively 94.2%, 93.9% and 97.5%, and the protein removal rate is 96.8%, and the polysaccharide clearance is 97.2%.
To Fructus Gardeniae extract through membrane separation purification, adopt the HZ806 macroporous adsorbent resin, enrichment is adsorbed to saturated, earlier with water (V/V) the flush away polar impurity that is no less than 2 times of amount of resin, 60% ethanol water of 8 times of amount of resin of reuse, with 3 times of amount of resin/hour flow velocity (V/V) eluting target substance, reclaim the Fructus Gardeniae extract that promptly gets behind the solvent through resin separation purification.After measured, the response rate 96.2% of Fructus Gardeniae iridoid glycoside compounds, the response rate 93.2% of Fructus Gardeniae carotenoid compounds, the response rate 95.8% of Fructus Gardeniae chlorogenic acid.
Embodiment 2
20～30 order Cape Jasmine Fruit 2.6kg are put into extraction pot, 25% methanol aqueous solution with 15 times of dry weights of Cape Jasmine Fruit (W/W), under 50 ℃ of conditions, extract 2 times, each 3 hours, merge extractive liquid,, filter, filtrate-0.06～-0.095MPa, 50～80 ℃ of conditions under, become Fructus Gardeniae extract through decompression and solvent recovery, vacuum concentration.After measured, Fructus Gardeniae iridoid glycoside compounds, carotenoid compounds and chlorogenic acid extraction ratio are respectively 92.3%, 92.8% and 91.8%.
The Fructus Gardeniae crude extract is added suitable quantity of water stir into suspension, make suspension proportion reach 1.12, adopting molecular cut off then is 30000 polyvinylidene fluoride film, under 0.60MPa, carry out membrane separation for removing impurities, remove the Fructus Gardeniae extract that promptly gets behind protein and polysaccharide and other macromole impurity behind the membrane separation purification.After measured, the response rate of Fructus Gardeniae iridoid glycoside compounds, carotenoid compounds and chlorogenic acid is respectively 95.3%, 94.8% and 96.8%, and the protein removal rate is 95.6%, and the polysaccharide clearance is 96.8%.
To Fructus Gardeniae extract through membrane separation purification, adopt the HZ801 macroporous adsorbent resin, enrichment is adsorbed to saturated, earlier with water (V/V) the flush away polar impurity that is no less than 2 times of amount of resin, 45% ethanol water of 6 times of amount of resin of reuse with 1 times of amount of resin/hour flow velocity (V/V) eluting target substance, reclaim the Fructus Gardeniae extract that promptly gets behind the solvent through resin separation purification.After measured, the response rate 97.2% of Fructus Gardeniae iridoid glycoside compounds, the response rate 94.5% of Fructus Gardeniae carotenoid compounds, the response rate 98.3% of Fructus Gardeniae chlorogenic acid.
Embodiment 3
20～30 order Cape Jasmine Fruit 2.7kg are put into extraction pot, 75% methanol aqueous solution with 5 times of dry weights of Cape Jasmine Fruit (W/W), reflux, extract, is 1 hour under 80 ℃ of conditions, filter, filtrate-0.06～-0.095MPa, 50～80 ℃ of conditions under, become Fructus Gardeniae extract through decompression and solvent recovery, vacuum concentration.After measured, Fructus Gardeniae iridoid glycoside compounds, carotenoid compounds and chlorogenic acid extraction ratio are respectively 95.6%, 95.0% and 93.5%.
The Fructus Gardeniae crude extract is added suitable quantity of water stir into suspension, make suspension proportion reach 1.03, adopting membrane aperture then is the inorganic ceramic film of 0.22 μ m, carries out membrane separation for removing impurities under 0.25MPa, removes the Fructus Gardeniae extract that promptly gets behind the macromole impurity such as protein and polysaccharide behind the membrane separation purification.After measured, the response rate of Fructus Gardeniae iridoid glycoside compounds, carotenoid compounds and chlorogenic acid is respectively 97.0%, 96.9% and 97.8%, and the protein removal rate is 94.7%, and the polysaccharide clearance is 96.1%.
To Fructus Gardeniae extract through membrane separation purification, adopt the HZ816 macroporous adsorbent resin, enrichment is adsorbed to saturated, earlier with water (V/V) the flush away polar impurity that is no less than 2 times of amount of resin, 30% ethanol water of 8 times of amount of resin of reuse with 2 times of amount of resin/hour flow velocity (V/V) eluting target substance, reclaim the Fructus Gardeniae extract that promptly gets behind the solvent through resin separation purification.After measured, the response rate 95.4% of Fructus Gardeniae iridoid glycoside compounds, the response rate %91.6 of Fructus Gardeniae carotenoid compounds, the response rate 95.9% of Fructus Gardeniae chlorogenic acid.
Embodiment 4
Producing Fructus Gardeniae with Fujian is raw material, with the washing of bright Fructus Gardeniae, dry (air-dry, all can dry or dry), pulverize, cross 20～30 mesh sieves and get Cape Jasmine Fruit, the 2.9kg Cape Jasmine Fruit is put into extraction pot, 75% ethanol water with 5 times of dry weights of Cape Jasmine Fruit (W/W), under 80 ℃ of conditions, extracted 1 hour, filter, filtrate-0.06～-0.095MPa, 50～80 ℃ of conditions under, become Fructus Gardeniae extract through decompression and solvent recovery, vacuum concentration.After measured, Fructus Gardeniae iridoid glycoside compounds, carotenoid compounds and chlorogenic acid extraction ratio are respectively 94.8%, 94.3% and 93.6%.
Earlier the Fructus Gardeniae crude extract is added suitable quantity of water and stir into suspension, make suspension proportion reach 1.13, adopting molecular cut off then is 60000 polyvinylidene fluoride films, under 0.50MPa, carry out membrane separation for removing impurities, remove the Fructus Gardeniae extract that promptly gets behind protein and polysaccharide and other macromole impurity behind the membrane separation purification.After measured, the response rate of Fructus Gardeniae iridoid glycoside compounds, carotenoid compounds and chlorogenic acid is respectively 96.7%, 96.1% and 96.6%, and the protein removal rate is 95.3%, and the polysaccharide clearance is 96.9%.
To Fructus Gardeniae extract through membrane separation purification, adopt the D101 macroporous adsorbent resin, enrichment is adsorbed to saturated, earlier with water (V/V) the flush away polar impurity that is no less than 2 times of amount of resin, 40% methanol aqueous solution of 4 times of amount of resin of reuse with 2 times of amount of resin/hour flow velocity (V/V) eluting target substance, reclaim the Fructus Gardeniae extract that promptly gets behind the solvent through resin separation purification.After measured, the response rate 96.3% of Fructus Gardeniae iridoid glycoside compounds, the response rate 93.4% of Fructus Gardeniae carotenoid compounds, the response rate 96.4% of Fructus Gardeniae chlorogenic acid.
Embodiment 5
20～30 order Cape Jasmine Fruit 2.6kg are put into extraction pot, 45% methanol-isopropyl alcohol (1: 1) aqueous solution with 8 times of dry weights of Cape Jasmine Fruit (W/W), under 73 ℃ of conditions, extract 2 times, each 2 hours, merge extractive liquid,, filter, filtrate-0.06～-0.095MPa, 50～80 ℃ of conditions under, become Fructus Gardeniae extract through decompression and solvent recovery, vacuum concentration.After measured, Fructus Gardeniae iridoid glycoside compounds, carotenoid compounds and chlorogenic acid extraction ratio are respectively 94.3%, 95.4% and 93.7%.
The Fructus Gardeniae crude extract is added suitable quantity of water stir into suspension, make suspension proportion reach 1.16, adopting molecular cut off then is 100000 inorganic ceramic film, under 0.45MPa, carry out membrane separation for removing impurities, remove the Fructus Gardeniae extract that promptly gets behind protein and polysaccharide and other macromole impurity behind the membrane separation purification.After measured, the response rate of Fructus Gardeniae iridoid glycoside compounds, carotenoid compounds and chlorogenic acid is respectively 97.6%, 96.8% and 97.0%, and the protein removal rate is 94.1%, and the polysaccharide clearance is 96.4%.
To Fructus Gardeniae extract through membrane separation purification, adopt the DK110 macroporous adsorbent resin, enrichment is adsorbed to saturated, earlier with water (V/V) the flush away polar impurity that is no less than 2 times of amount of resin, 30% methanol aqueous solution of 6 times of amount of resin of reuse with 3 times of amount of resin/hour flow velocity (V/V) eluting target substance, reclaim the Fructus Gardeniae extract that promptly gets behind the solvent through resin separation purification.After measured, the response rate 93.9% of Fructus Gardeniae iridoid glycoside compounds, the response rate 90.1% of Fructus Gardeniae carotenoid compounds, the response rate 94.7% of Fructus Gardeniae chlorogenic acid.
Embodiment 6
20～30 order Cape Jasmine Fruit 2.4kg are put into extraction pot, 38% ethanol water with 15 times of dry weights of Cape Jasmine Fruit (W/W), under 50 ℃ of conditions, extract 3 times, each 3 hours, merge extractive liquid,, filter, filtrate-0.06～-0.095MPa, 50～80 ℃ of conditions under, become Fructus Gardeniae extract through decompression and solvent recovery, vacuum concentration.After measured, Fructus Gardeniae iridoid glycoside compounds, carotenoid compounds and chlorogenic acid extraction ratio are respectively 92.5%, 92.7% and 91.2%.
The Fructus Gardeniae crude extract is added suitable quantity of water stir into suspension, make suspension proportion reach 1.06, adopting molecular cut off then is 20000 polysulfone membrane, under 0.75MPa, carry out membrane separation for removing impurities, remove the Fructus Gardeniae extract that promptly gets behind protein and polysaccharide and other macromole impurity behind the membrane separation purification.After measured, the response rate of Fructus Gardeniae iridoid glycoside compounds, carotenoid compounds and chlorogenic acid is respectively 94.5%, 93.8% and 96.4%, and the protein removal rate is 95.8%, and the polysaccharide clearance is 97.0%.
To Fructus Gardeniae extract through membrane separation purification, adopt the AB-8 macroporous adsorbent resin, enrichment is adsorbed to saturated, earlier with water (V/V) the flush away polar impurity that is no less than 2 times of amount of resin, 60% methanol aqueous solution of 6 times of amount of resin of reuse with 1 times of amount of resin/hour flow velocity (V/V) eluting target substance, reclaim the Fructus Gardeniae extract that promptly gets behind the solvent through resin separation purification.After measured, the response rate 95.7% of Fructus Gardeniae iridoid glycoside compounds, the response rate 91.8% of Fructus Gardeniae carotenoid compounds, the response rate 96.4% of Fructus Gardeniae chlorogenic acid.
Embodiment 7
Producing Fructus Gardeniae with Fujian is raw material, with the washing of bright Fructus Gardeniae, dry (air-dry, all can dry or dry), pulverize, cross 20～30 mesh sieves and get Cape Jasmine Fruit, the 2.6kg Cape Jasmine Fruit is put into extraction pot, with 25% aqueous acetone solution of 15 times of dry weights of Cape Jasmine Fruit (W/W), under 50 ℃ of conditions, extract 3 times each 3 hours, merge extractive liquid,, filter, filtrate-0.06～-0.095MPa, 50～80 ℃ of conditions under, become Fructus Gardeniae extract through decompression and solvent recovery, vacuum concentration.After measured, Fructus Gardeniae iridoid glycoside compounds, carotenoid compounds and chlorogenic acid extraction ratio are respectively 93.8%, 91.5% and 91.8%.
The Fructus Gardeniae crude extract is added suitable quantity of water stir into suspension, make suspension proportion reach 1.22, adopting membrane aperture then is the polyvinylidene fluoride film of 0.22 μ m, under 0.38MPa, carry out membrane separation for removing impurities, remove the Fructus Gardeniae extract that promptly gets behind protein and polysaccharide and other macromole impurity behind the membrane separation purification.After measured, the response rate of Fructus Gardeniae iridoid glycoside compounds, carotenoid compounds and chlorogenic acid is respectively 97.6%, 96.6% and 97.2%, and the protein removal rate is 94.2%, and the polysaccharide clearance is 96.1%.
To Fructus Gardeniae extract through membrane separation purification, adopt the D113 macroporous adsorbent resin, enrichment is adsorbed to saturated, earlier with water (V/V) the flush away polar impurity that is no less than 2 times of amount of resin, 30% aqueous acetone solution of 4 times of amount of resin of reuse with 1 times of amount of resin/hour flow velocity (V/V) eluting target substance, reclaim the Fructus Gardeniae extract that promptly gets behind the solvent through resin separation purification.After measured, the response rate 95.8% of Fructus Gardeniae iridoid glycoside compounds, the response rate 92.4% of Fructus Gardeniae carotenoid compounds, the response rate 96.1% of Fructus Gardeniae chlorogenic acid.
Embodiment 8
20～30 order Cape Jasmine Fruit 2.5kg are put into extraction pot, 75% aqueous acetone solution with 5 times of dry weights of Fructus Gardeniae powder (W/W), reflux, extract, is 2 times under 80 ℃ of conditions, each 1 hour, merge extractive liquid,, filter, filtrate-0.06～-0.095MPa, 50～80 ℃ of conditions under, become Fructus Gardeniae extract through decompression and solvent recovery, vacuum concentration.After measured, Fructus Gardeniae iridoid glycoside compounds, carotenoid compounds and chlorogenic acid extraction ratio are respectively 93.9%, 93.2% and 93.5%.
The Fructus Gardeniae crude extract is added suitable quantity of water stir into suspension, make suspension proportion reach 1.08, adopting molecular cut off then is 50000 polysulfone membrane, under 0.50MPa, carry out membrane separation for removing impurities, remove the Fructus Gardeniae extract that promptly gets behind protein and polysaccharide and other macromole impurity behind the membrane separation purification.After measured, the response rate of Fructus Gardeniae iridoid glycoside compounds, carotenoid compounds and chlorogenic acid is respectively 95.8%, 97.7% and 96.1%, and the protein removal rate is 95.9%, and the polysaccharide clearance is 96.7%.
To Fructus Gardeniae extract through membrane separation purification, adopt the HZ802 macroporous adsorbent resin, enrichment is adsorbed to saturated, earlier with water (V/V) the flush away polar impurity that is no less than 2 times of amount of resin, 60% aqueous acetone solution of 4 times of amount of resin of reuse with 2 times of amount of resin/hour flow velocity (V/V) eluting target substance, reclaim the Fructus Gardeniae extract that promptly gets behind the solvent through resin separation purification.After measured, the response rate 93.6% of Fructus Gardeniae iridoid glycoside compounds, the response rate 89.6% of Fructus Gardeniae carotenoid compounds, the response rate 94.3% of Fructus Gardeniae chlorogenic acid.
Embodiment 9
20～30 order Cape Jasmine Fruit 2.3kg are put into extraction pot, sodium hydrogen phosphate-potassium dihydrogen phosphate buffer solution with the pH 8.0 of 15 times of dry weights of Cape Jasmine Fruit (W/W), under 80 ℃ of conditions, extract 3 times, each 2 hours, filter, filtrate-0.06～-0.095MPa, 65～80 ℃ of conditions under, become Fructus Gardeniae extract through decompression and solvent recovery, vacuum concentration.After measured, Fructus Gardeniae iridoid glycoside compounds, carotenoid compounds and chlorogenic acid extraction ratio are respectively 90.1%, 82.6% and 88.9%.
The Fructus Gardeniae crude extract is added suitable quantity of water stir into suspension, make suspension proportion reach 1.16, adopting membrane aperture then is the inorganic ceramic film of 0.22 μ m, under 0.35MPa, carry out membrane separation for removing impurities, remove the Fructus Gardeniae extract that promptly gets behind protein and polysaccharide and other macromole impurity behind the membrane separation purification.After measured, the response rate of Fructus Gardeniae iridoid glycoside compounds, carotenoid compounds and chlorogenic acid is respectively 98.3%, 96.5% and 97.2%, and the protein removal rate is 94.3%, and the polysaccharide clearance is 95.9%.
To Fructus Gardeniae extract through membrane separation purification, adopt the HZ803 macroporous adsorbent resin, enrichment is adsorbed to saturated, earlier with water (V/V) the flush away polar impurity that is no less than 2 times of amount of resin, 45% aqueous acetone solution of 8 times of amount of resin of reuse with 3 times of amount of resin/hour flow velocity (V/V) eluting target substance, reclaim the Fructus Gardeniae extract that promptly gets behind the solvent through resin separation purification.After measured, the response rate 93.8% of Fructus Gardeniae iridoid glycoside compounds, the response rate 88.5% of Fructus Gardeniae carotenoid compounds, the response rate 94.2% of Fructus Gardeniae chlorogenic acid.
Above embodiment is intended to further describe for example the present invention, rather than limits the present invention by any way.
The present invention is novel, and technology is simple, the extraction efficiency height, and production cost is low, meets the modernization of Chinese medicine and international industrial policy that country advocates, has bigger dissemination.
Claims (5)
1. method that adopts macroporous adsorbent resin to prepare Fructus Gardeniae extract, comprise the membrane separation for removing impurities step that adopts hydrophilic solvent to extract Fructus Gardeniae crude extract and Fructus Gardeniae crude extract, it is characterized in that: the method that described employing hydrophilic solvent extracts the Fructus Gardeniae crude extract is: be raw material with the Fructus Gardeniae, adopt 25～75% hydrophilic solvent aqueous solutions of 5～15 times of Fructus Gardeniae dry weights (W/W), under 50～80 ℃ of conditions, extract 1～3 time, each 1～3 hour, merge extractive liquid,, filter, filtrate-0.06～-0.095MPa, under 50～80 ℃ of conditions, through decompression and solvent recovery, the get married Fructus Gardeniae crude extract of aqueous solvent extraction of vacuum concentration, hydrophilic solvent is a methanol, acetone, ethanol, one or more mixed solvents in propanol or the isopropyl alcohol or described hydrophilic solvent are different pH value buffer solution; Described membrane separation for removing impurities method is: the Fructus Gardeniae crude extract that extracts with hydrophilic solvent is a raw material, add water and become suspension, make suspension proportion reach 1.03～1.22, under 0.25～0.75MPa through membrane separation for removing impurities, promptly get Fructus Gardeniae membrane separation purification extract after removing protein and polysaccharide and other macromole impurity, the membrane separation for removing impurities process is selected the diffusion barrier of 6000 molecular cut offs～0.22 μ m membrane aperture for use; The separation membrane material of membrane separation for removing impurities process is one or more hybrid films materials in mineral-type, polysulfones, fluoro-containing macromolecule material class, TPO, polyamide-based, chitin kind or the cellulose family membrane material; With Fructus Gardeniae membrane separation purification extract is that raw material carries out the macroporous adsorbent resin separation and purification: with Fructus Gardeniae membrane separation purification extract is raw material, add water and stir into suspension, make suspension proportion reach 1.05～1.18, adopt absorption with macroporous adsorbent resin to saturated, earlier with water (V/V) the flush away polar impurity that is no less than 2 times of amount of resin, 30～60% hydrophilic solvent aqueous solution of 4～8 times of amount of resin of reuse with 1～3 times of amount of resin/hour flow velocity (V/V) eluting target substance, filtrate-0.05～-0.09MPa, under 50～65 ℃ of conditions, through decompression and solvent recovery, vacuum concentration becomes the Fructus Gardeniae extract through resin separation purification, and the chemical composition of macroporous adsorbent resin skeleton is a polystyrene, in polyacrylic acid or the phenolic aldehyde one or more.
2. employing macroporous adsorbent resin according to claim 1 prepares the method for Fructus Gardeniae extract, it is characterized in that: hydrophilic solvent is selected methanol or acetone for use.
3. employing macroporous adsorbent resin according to claim 1 prepares the method for Fructus Gardeniae extract, it is characterized in that: the main component of described Fructus Gardeniae extract is iridoid glycoside compounds, carotenoid compounds or chlorogenic acid; Described Fructus Gardeniae iridoid glycoside compounds is one or more chemical compounds in jasminoidin, different jasminoidin, genipin gentiobiose glycosides or the gardenia acid; Described carotenoid compounds is one or more chemical compounds in crocetin, crocin 1, crocin 2 or the crocin 3.
4. employing macroporous adsorbent resin according to claim 1 prepares the method for Fructus Gardeniae extract, it is characterized in that: the separation membrane material of membrane separation for removing impurities process is selected inorganic ceramic film, polysulfone membrane or polyvinylidene fluoride film for use.
5. employing macroporous adsorbent resin according to claim 1 prepares the method for Fructus Gardeniae extract, it is characterized in that: the chemical composition of macroporous adsorbent resin skeleton is selected polystyrene or polyacrylic acid for use.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200610200965A CN1939458B (en) | 2006-09-30 | 2006-09-30 | Preparation of gardenia jasminoides by macroporous adsorbing resin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200610200965A CN1939458B (en) | 2006-09-30 | 2006-09-30 | Preparation of gardenia jasminoides by macroporous adsorbing resin |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1939458A CN1939458A (en) | 2007-04-04 |
| CN1939458B true CN1939458B (en) | 2010-05-19 |
Family
ID=37958160
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN200610200965A Expired - Fee Related CN1939458B (en) | 2006-09-30 | 2006-09-30 | Preparation of gardenia jasminoides by macroporous adsorbing resin |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1939458B (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101037467B (en) * | 2007-04-10 | 2010-05-19 | 福州大学 | Method for separating purifying ursolic acid from loquat leaf |
| CN102304554B (en) * | 2011-06-01 | 2013-03-27 | 武汉绿孚生物工程有限责任公司 | Method for producing gardenia red pigment with high color value |
| CN105017356B (en) * | 2015-08-31 | 2018-11-13 | 广西红瑶药业有限公司 | A method of extracting Geniposidic acid from cape jasmine |
| CN105963389B (en) * | 2016-05-10 | 2019-05-24 | 李茂星 | The separation method of anti-high altitude anoxia anti-fatigue activity ingredient and its application in cape jasmine |
| CN105902488A (en) * | 2016-05-20 | 2016-08-31 | 贵州瑞和制药有限公司龙里药厂 | Process for preparing Shuganning preparation |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1660198A (en) * | 2004-12-14 | 2005-08-31 | 武汉健民中药工程有限责任公司 | Medication for treating cholecystitis and cholelithiasis, and preparation method |
| CN1670037A (en) * | 2005-02-24 | 2005-09-21 | 河南大学 | Complex utilization of Gardenia |
-
2006
- 2006-09-30 CN CN200610200965A patent/CN1939458B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1660198A (en) * | 2004-12-14 | 2005-08-31 | 武汉健民中药工程有限责任公司 | Medication for treating cholecystitis and cholelithiasis, and preparation method |
| CN1670037A (en) * | 2005-02-24 | 2005-09-21 | 河南大学 | Complex utilization of Gardenia |
Non-Patent Citations (4)
| Title |
|---|
| 毛红骞.栀子黄色素的提取及性质研究.食品科技 1.2003,(1),29-31. |
| 毛红骞.栀子黄色素的提取及性质研究.食品科技 1.2003,(1),29-31. * |
| 谢学建, 张俊慧, 马爱华.中药栀子研究进展.时珍国医国药11 10.2000,11(10),943-945. |
| 谢学建, 张俊慧, 马爱华.中药栀子研究进展.时珍国医国药11 10.2000,11(10),943-945. * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1939458A (en) | 2007-04-04 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN100528970C (en) | Method for separating and purifying high-tone jasmine flavine from jasmine | |
| CN102732050B (en) | Method for preparing gardenia pigments from Gardenia jasminoides Ellis | |
| CN100473657C (en) | Isolation and purification method of geniposide | |
| An et al. | An efficiency strategy for extraction and recovery of ellagic acid from waste chestnut shell and its biological activity evaluation | |
| CN102021106B (en) | Traditional Chinese medicine health wine and production technology thereof | |
| CN1923829B (en) | Preparation method and use of separating and purifying lotus leaf flavone and lotus leaf alkaloid by employing polyamide | |
| CN1939458B (en) | Preparation of gardenia jasminoides by macroporous adsorbing resin | |
| CN102319282B (en) | Aqueous two-phase extraction method for total flavones in kudzu root | |
| CN103494862B (en) | Method for extracting olive polyphenol from olive processing waste liquor | |
| CN101007064A (en) | Isolation and purification method of lotus leaf extract by macroporous resin and its application thereof | |
| CN101037467B (en) | Method for separating purifying ursolic acid from loquat leaf | |
| CN104523836A (en) | Method for comprehensively extracting protein, polysaccharide and polyphenol from avocado kernels | |
| CN1939459B (en) | Preparation of gardenia jasminoides by membrane separation technology | |
| CN100475828C (en) | Isolation and purification method of amygdalin from loquat core | |
| CN104096381A (en) | Method for extracting effective components of natural products through mixing of ethyl alcohol and sub-critical fluid | |
| CN102796203A (en) | Method for preparing anti-oxidization active camellia olefera cake polysaccharide | |
| CN110981921B (en) | Continuous method for synchronously extracting multiple effective components from figs | |
| CN1939457B (en) | Preparation of gardenia jasminoides extracts | |
| WO2012061984A1 (en) | Method for preparing albiflorin and paeoniflorin | |
| CN114515008A (en) | Cistanche tubulosa extract and preparation method thereof | |
| CN101659793A (en) | Method for extracting gynura bicolor purpurin | |
| RU2381245C1 (en) | Method of production of concentrated colouring agent | |
| CN101186757B (en) | Method for producing purple sweet potato haematochrome | |
| CN110141605A (en) | A kind of preparation method of snowpoppy total alkaloid nanoparticle | |
| CN116139055A (en) | Preparation method and application of vitamin C-enriched roxburgh rose extract |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20100519 Termination date: 20130930 |