CN1641038A - Method for extracting effective component of sweet potato leaf stalk vine - Google Patents
Method for extracting effective component of sweet potato leaf stalk vine Download PDFInfo
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- CN1641038A CN1641038A CN 200410015807 CN200410015807A CN1641038A CN 1641038 A CN1641038 A CN 1641038A CN 200410015807 CN200410015807 CN 200410015807 CN 200410015807 A CN200410015807 A CN 200410015807A CN 1641038 A CN1641038 A CN 1641038A
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Abstract
The present invention relates to the extraction of effective components in plant material, and is especially the extraction process of effective components in sweet potato leaf stem and vine. Sweet potato leaf stem and vine after pre-treatment is extracted with water in 3-50 times and filtered to obtain filtrate and filter cake, and the filtrate and the filter cake are further extracted separately to obtain the effective components. The present invention features that during water extraction, pectase and cellulase as enzymolysing agent are added to reduce water consumption and power consumption greatly. The present invention has also the advantages of high extraction efficiency, high product yield, high product purity and no environmental pollution.
Description
Technical field
The present invention relates to a kind of extracting method of effective ingredients in plant, extraction of effective components in especially a kind of Sweet Potato Leaf rattan.
Background technology
Sweet potato belongs to convolvulaceae sweet potato genus (Ipomoea Batas.Lam) sweet potato kind herbaceous plant on the plant classification, have another name called sweet potato, Ipomoea batatas, originates in Southern Africa.Imported China into before 500 years, stable high yield, anti-disaster ability are strong because it has, wide adaptability, characteristics such as cultivation easily, so welcome by broad masses of the people, spread to various places, China north and south very soon.Now, China north from Liaoning, reach Hainan in the south and all plant sweet potato, cultivated area is more than 100,000,000 mu throughout the year, becomes the food crop that are only second to after paddy rice, wheat, the corn.At our province, the sweet potato cultivated area reaches 2,200,000 mu, produces 1,010 ten thousand tons of Folium Ipomoea, handle, rattan, produces 4,700,000 tons in Ipomoea batatas.In the past, sweet potato is mainly as grain and feed usefulness, but along with the development of industrial and agricultural production and the raising of living standards of the people, sweet potato is used as industrial raw material more and more and carries out multiple deep processing.Now, be that the converted products of raw material has hundreds of kinds such as starch, alcohol, monosodium glutamate, citric acid, fructose, butanols, butyric acid, acetone with the sweet potato root tuber.And seldom to the processing and utilization of Rhizoma Dioscoreae esculentae leaf, handle, rattan, general only as feed, though be used as on the nutrition dish dining table now, and major part all is discarded in by limit, field, the road, basically be abandoned as waste, cause the wasting of resources and environmental pollution.Pertinent data shows, contains abundant carotene, V in the Rhizoma Dioscoreae esculentae leaf
B1, V
B2, V
CAnd mineral element such as iron, calcium, magnesium.Show that according to modern medicine Rhizoma Dioscoreae esculentae leaf has the promotion gastrointestinal peristalsis, stimulate digestion that the treatment constipation promotes cholesterol to drain, and prevents the sedimentation of fat on the painstaking effort tube wall, keeps arteries elasticity, the lubricating effect of protection digestive tube, respiratory tract and joint cavity.On China's Chinese medicine data also the record, with (sweet potato) " cauline leaf is used as medicine, (its medicine) slightly cool in nature, sweet-puckery flavor, nontoxic; Have promoting lactation, the carbuncle sore of bursting, apocenosis, detoxifcation " effect, cure mainly married woman's galactostasis, the pain sore symptoms such as purulence, stool band blood, diarrhoea of not bursting for a long time.So Rhizoma Dioscoreae esculentae leaf is subject to people's attention day by day as the natural green vegetables, in some areas, China south, people just have the custom of edible Rhizoma Dioscoreae esculentae leaf, people usually use " leaf of sweet potato; the sheep liver is with boiling food " to control yctalopia, and it is long-pending to control the children's blood clam with " bright Rhizoma Dioscoreae esculentae leaf boils back its soup of salt-free diet ", uses " bright sweet potato tender leaf; bright wax gourd is an amount of, poach is obeyed " to control diabetes.Also a lot of as above example, though this is a folk remedy, the explanation Rhizoma Dioscoreae esculentae leaf can be as the healthy food material utilization.Be referred to as " vegetables queen " in Hong Kong, also be listed in " life prolonging food " in the U.S., Japan.Exploitation Rhizoma Dioscoreae esculentae leaf protective foods approach is a lot, Rhizoma Dioscoreae esculentae leaf or other vegetables can be pulled an oar together, filter, sterilized, add batching, make health-care vegetable juice drink, or potato piece and rattan leaf cooperation boiling, make tonic wine after the fermentation, also can be with stem, the lixiviate of piece root, concentrate protective foodss such as spray-dried one-tenth nutritive powder, sheet, electuary.But more important is the technology such as extraction, separation and purifying of research Rhizoma Dioscoreae esculentae leaf functional factor, keeps their activity to greatest extent, improves their stability in protective foods, adopts outer addition to produce third generation protective foods.
Extraction of effective components in the existing Sweet Potato Leaf rattan, seldom adopt zymolysis technique, for guaranteeing higher extraction yield, need add a large amount of water could propose effective constituents such as polysaccharide, flavones, amino acid, and needing to consume a large amount of energy could remove a large amount of water.
Summary of the invention
The object of the present invention is to provide extraction of effective components in a kind of Sweet Potato Leaf rattan, this extracting method can obtain effective constituents such as Sweet Potato Leaf rattan polysaccharide, flavonoid compound.This method extraction efficiency height, water consumption is little, can save energy.
Technical scheme of the present invention is:
Extraction of effective components in a kind of Sweet Potato Leaf rattan, the Sweet Potato Leaf rattan is through the pre-treatment of routine, and Jia Shuishui carries, and filters, and obtains filtrate a and filter residue b; Filtrate a and filter residue b further extract each effective constituent, and the solid-to-liquid ratio between pretreated Sweet Potato Leaf rattan and the amount of water is: 1: 3-50; Water is carried in the process and to be adopted addition is that the polygalacturonase of 0.002-0.05% carries out enzymolysis, pectin enzymatic hydrolysis condition: PH is 3.0-6.0, temperature 40-60 degree centigrade, time 0.2-2 hour, polygalacturonase also increases the fiber enzymolysis step after separating end, the fiber enzymatic hydrolysis condition: the cellulase amount is 0.1-2%, and PH is 3.0-6.0, temperature 30-60 degree centigrade, time 0.5-2 hour.
The topmost contribution of the present invention is exactly to add pectinase enzymatic hydrolysis and cellulase is separated the associating use, solid-to-liquid ratio can be controlled in 1: 50, and the flavonoid yield can reach more than 4%, compares not add any enzyme enzymolysis, and solid-to-liquid ratio then need be controlled at 1: 100 flavonoid yield just can reach 4%.Under equal conditions, the little meaning of solid-to-liquid ratio can reduce energy consumption with more a spot of water extraction in follow-up enrichment step.
The technical scheme of more excellent invention has following:
Extraction of effective components in the Sweet Potato Leaf rattan, water are put forward process also increases the proteolysis step, the proteolysis condition: the proteolytic enzyme amount is 0.1-2%, and PH is 2-5.5, temperature 25-50 degree centigrade, and time 0.3-2 hour.
Extraction of effective components in the Sweet Potato Leaf rattan, filtrate a is step after filtration, be specially first ultrafiltration, it is the ultra-filtration membrane of 8000-12000 that molecular weight cut-off is adopted in ultrafiltration, dam liquid a1 vacuum or spraying drying, obtain polysaccharide, ultrafiltration obtains sees through liquid, through nanofiltration, it is the nanofiltration membrane of 400-8000 that molecular weight cut-off is adopted in nanofiltration, and the liquid a2 that dams can further reclaim useful matter, see through liquid through reverse osmosis concentration through what nanofiltration obtained, reverse osmosis pressure is 0.2-6mpa, and the liquid a3 that dams that obtains contains amino acid, and the liquid water that sees through of reverse osmosis can recycling use.
Extraction of effective components in the Sweet Potato Leaf rattan, pre-treatment also comprise pulverization process, and pulverization process is pulverized the Sweet Potato Leaf rattan and is 4-200 purpose fine powder.
Extraction of effective components in the Sweet Potato Leaf rattan, filter residue b by solid-to-liquid ratio is: 1: the consumption of 2-20 adds the ethanol that concentration is 50%-95%, under temperature 25-85 degrees celsius alcohol extracting 0.3-2 hour, refilter, the filtrate d that obtains, elder generation's ultrafiltration, it is the ultra-filtration membrane of 4000-7000 that molecular weight cut-off is adopted in ultrafiltration, the liquid b1 that dams can further reclaim useful matter, ultrafiltration obtains sees through liquid, through nanofiltration, it is the nanofiltration membrane of 400-1100 that molecular weight cut-off is adopted in nanofiltration, the further refining chromocor compound that obtains of the liquid b2 that dams, see through liquid through reverse osmosis concentration through what nanofiltration obtained, reverse osmosis pressure is 0.2-6mpa, and the liquid b3 that dams that obtains can further reclaim useful matter, reverse osmosis see through liquid contain a large amount of ethanol can recycling use.
The refining of chromocor compound can adopt conventional method: the liquid b2 that dams adsorbs through polycaprolactam through diatomite, resin absorption, 50% ethanol elution desorb, and ethanol reclaims, and obtains chromocor compound.Disclosed method in " research of Folium Bambosae flavone purified " document of 2001 (6) .-34-35 publication that flavones is refining can be adopted " grain and oil processing and food machinery ".
Effective constituents such as gained polysaccharide of the present invention, flavones adopt following method validation effect:
Polysaccharide precipitation thing and sulfuric acid phenol reagent react are orange-yellow, are blue-greenish colour with the reaction of sulfuric acid anthrone reagent, illustrate that two qualitative reactions all are positive.
UV spectrum
The ultraviolet spectrogram of polysaccharide precipitation thing.
Spectrogram shows, the polysaccharide precipitation thing 260nm, 280nm and near do not have absorption peak, and these two absorption peaks are respectively nucleic acid and proteinic typical peaks, this illustrates in this polysaccharide precipitation thing and does not contain nucleic acid and protein, it is successful that the Sevage method is removed free protein, because the Sevage method does not have influence to conjugated protein, therefore also prove not contain conjugated protein in the Rhizoma Dioscoreae esculentae leaf in the polysaccharide precipitation thing.
Infrared spectra
The infrared spectrogram of polysaccharide precipitation thing.
Spectrogram demonstrates the charateristic avsorption band of polysaccharide, shows: by the caused 1200-1000cm of two kinds of C-O (C-O-H and C-O-C) stretching vibration
-1Between bigger absorption peak; By the 1400-1200cm that causes of angle vibration
-1Between absorption peak; The 1750cm that the C=O stretching vibration causes
-1The 1620cm that bigger absorption peak and its asymmetric stretching vibration cause
-1About absorption peak; The 3400cm that the O-H stretching vibration causes
-1Broad peak or the like.
Can identify from above color reaction and infrared spectra and ultraviolet spectral analysis result: throw out is the polysaccharide product, and does not contain protein.
The research of Rhizoma Dioscoreae esculentae leaf polysaccharide purification
Purification process
Polysaccharide by hot water lixiviate, method deproteinated, decolouring, ethanol sedimentation is a polysaccharide mixture, be commonly referred to Crude polysaccharides (crude polysaccharide), promptly contain the polysaccharide of different components (level part), its molecular weight of different components is different, and perhaps structure is also different, and its biological activity also is not quite similar, what have complements each other, have even opposite restriction or checking relation in five elements, therefore, further investigate polysaccharide structures and function, most critical be the purifying of Crude polysaccharides.
Adopt DEAE-cellulose chromatography method (DEAE-cellulos ColumnChromatography) purifying Rhizoma Dioscoreae esculentae leaf polysaccharide, comparison staged gradient method takes off method and the continous way gradient method is taken off method, select a kind of elution process preferably, the polysaccharide product purification is become the polysaccharide of one-component, be commonly referred to holosaccharide (pure polysaccharide).
The preparation of post
Take by weighing the 20gDEAE-Mierocrystalline cellulose, be immersed in the distilled water, it is fully expanded, filter the back and handle with 0.01mol/L (ethylenediamine tetraacetic acid (EDTA)); Soak 30min with 300ml0.5mol/L again, change in the B again in suction filtration, be washed till neutrality with distilled water, transfer in the beaker after draining; Use 300ml0.5mol/LNaOH solution soaking 30min then, transfer to suction filtration in the B then, be washed till neutrality with distilled water, transfer to after draining in the beaker, soak a moment, degassing back dress post with 300m10.02mol/L pH6.5 phosphate buffered saline buffer, use 2 times of distilled water balances again, standby.
Continous way gradient method wash-out
The polysaccharide soln (0.25%) that dissolving is good is gone up sample 2ml, opens the chromatography column outlet, allows polysaccharide soln penetrate in the DEAE-Mierocrystalline cellulose, use earlier the distilled water wash-out, the about 0.2ml/min of flow velocity collected a pipe in per 5 minutes, and pipe detects with the sulfuric acid phynol method, after going out the peak, return till the baseline, at this moment neutral sugar such as starch has been rinsed out, uses 0-1.0mol/L solution 500ml continous way gradient elution again, and flow velocity is constant, detect with quadrat method, till 500ml solution washes.
The staged gradient elution
Adopt above-mentioned same method upper prop, the distilled water wash-out is used 0.1mol/L, 0.2mol/L, 0.3mol/L, 0.4mol/LNaCl...... eluant solution afterwards successively, and flow velocity is the same, and detection method is the same, till no polysaccharide washes out.
Experiment material
The HPGFC condition:
Chromatographic column: M-Bondapak E-linear[300*3.9mmID]
Moving phase: methyl alcohol: water=1: 9
Flow velocity: 0 4ml/min
Temperature: 8-10 ℃
Adopt high performance gel filtration chromatography, make moving phase with methanol-water, separate through M-Bondapak E-Linear post, differential refraction detector detects, and makes standard with the serial Dextra of the T of known flat average molecular weight, and the molecular weight that records SPPS=II is 61.16 * 10
4Da.The linear relationship of molecular weight determination is good, and its relation conefficient is 0.9830, and has simplified operation steps greatly, has obviously improved detection efficiency.From the HPGFC spectrogram of SPPS=II, its bands of a spectrum wider distribution shows that the isolating SPPS=II of DEAE one cellulose chromatography awaits to be further purified, to obtain the narrower pure product of polysaccharide of molecular weight distribution.
Do the quantitative levels data that contrast can obtain polysaccharide by the collection of illustrative plates peak area and the standard substance that calculate high-efficient gel filtration chromatography.
The Study on Chromatographic Quantitative Analysis method of flavonoid compound of the present invention can adopt " Food science " .2001, and " Study on Chromatographic Quantitative Analysis of flavonoid compound " document disclosed method that 22 (2) .-57-61 publish is measured.
Embodiment
Embodiment 1
Extraction of effective components in a kind of Sweet Potato Leaf rattan is selected 3000 kilograms in Sweet Potato Leaf rattan for use.The Sweet Potato Leaf rattan is cleaned in impurity elimination, debranching, stalk, the air-dry stamp mill and fully smashs leaf, handle to pieces through the pre-treatment of routine, and rattan crosses 50 mesh sieves, adds water water after pre-treatment finishes and carries, and filters, and obtains filtrate a and filter residue b; Filtrate a and filter residue b further extract each effective constituent, and the solid-to-liquid ratio between pretreated Sweet Potato Leaf rattan and the amount of water is: 1: 30; Water is carried in the process and to be adopted addition is that 0.03% polygalacturonase carries out enzymolysis, pectin enzymatic hydrolysis condition: PH is 4.1,45 degrees centigrade of temperature, 1 hour time, polygalacturonase also increases the fiber enzymolysis step after separating end, the fiber enzymatic hydrolysis condition: the cellulase amount is 1%, and PH is 5.2,55 degrees centigrade of temperature, 1 hour time.
Filtrate a is step after filtration, is specially first ultrafiltration, and ultrafiltration employing molecular weight cut-off is 10000 ultra-filtration membrane, dam liquid a1 vacuum or spraying drying, obtain polysaccharide, ultrafiltration obtains sees through liquid, through nanofiltration, nanofiltration employing molecular weight cut-off is 1100 nanofiltration membrane, the liquid a2 that dams can further reclaim useful matter, sees through liquid through reverse osmosis concentration through what nanofiltration obtained, and reverse osmosis pressure is 0.5mpa, the liquid a3 that dams that obtains contains amino acid, and the liquid water that sees through of reverse osmosis can recycling use.
Filter residue b by solid-to-liquid ratio is: it is 75% ethanol that 1: 10 consumption adds concentration, alcohol extracting is 1 hour under temperature 55 degrees celsius, refilter, the filtrate d that obtains, elder generation's ultrafiltration, ultrafiltration employing molecular weight cut-off is 5000 ultra-filtration membrane, the liquid b1 that dams can further reclaim useful matter, and ultrafiltration obtains sees through liquid, through nanofiltration, nanofiltration employing molecular weight cut-off is 1100 nanofiltration membrane, the further refining chromocor compound that obtains of the liquid b2 that dams sees through liquid through reverse osmosis concentration through what nanofiltration obtained, and reverse osmosis pressure is 0.5mpa, the liquid b3 that dams that obtains can further reclaim useful matter, reverse osmosis see through liquid contain a large amount of ethanol can recycling use.
After testing, the extraction rate reached 5.5% of polysaccharide (30%).The extraction rate reached 5.6% of flavones (45%).Isolating polysaccharide, flavones sample detect through Jiangxi Province's Food Hygiene Surveillance check, and the quality of product and sanitary index meet national related food quality hygienic standard.
Embodiment 2
Water is put forward process also increases the proteolysis step, the proteolysis condition: the proteolytic enzyme amount is 2%, and PH is 4.5,45 degrees centigrade of temperature, 1 hour time.All the other are with embodiment 1.
After testing, the extraction rate reached 6.8% of polysaccharide (30%).The extraction rate reached 6.3% of flavones (45%).Increase proteolysis step flavonoid yield, the extraction yield of polysaccharide has raising.
Embodiment 3
Pre-treatment is not added any enzyme after finishing, and directly the Sweet Potato Leaf rattan is added water water and carries.60 ℃ of the extraction temperatures that water is carried, pretreated Sweet Potato Leaf rattan and add lixiviate solid-to-liquid ratio 1: 100 between the water water yield, lixiviate is after 5.5 hours, and pH value is controlled at 6.5.
Filtrate a after filtration, heating concentrates 10 hours most water is removed, and enters other steps again, all the other are with embodiment 1.Flavones (45%) yield 4.062%.
For obtaining the flavonoid yield more than 4%, just must could dissolve and leach enough flavones with a large amount of water, the lixiviate solid-to-liquid ratio was up to 1: 100.And, needing long heating evaporation in order to remove a large amount of water, energy expenditure is big.
Embodiment 4
Filtrate a is step after filtration, is specially first ultrafiltration, sees through liquid through reverse osmosis, enters enrichment step again, and wherein ultrafiltration employing molecular weight cut-off is 10000 ultra-filtration membrane.All the other are with embodiment 1.
Adopt ultra-filtration membrane the polysaccharide of macromolecule can be separated preferably with the little flavonoid of relative molecular weight, ultra-filtration membrane and reverse osmosis logotype can be simplified concentrated program, and can reduce the lixiviate solid-to-liquid ratio, for example only need flavonoid (45%) yield that just can guarantee 4% or more at 1: 30, and can concentrate at normal temperatures, do not need heating, this is with a large amount of save energy.
Embodiment 5
The embodiment of one group of solid-to-liquid ratio aspect:
(1) solid-to-liquid ratio is: all the other were with embodiment 1 in 1: 3.
(2) solid-to-liquid ratio is: all the other were with embodiment 1 in 1: 50.
(3) solid-to-liquid ratio is: all the other were with embodiment 1 in 1: 8.
(4) solid-to-liquid ratio is: all the other were with embodiment 1 in 1: 27.
(5) solid-to-liquid ratio is: all the other were with embodiment 1 in 1: 36.
(6) solid-to-liquid ratio is: all the other were with embodiment 1 in 1: 17.
(7) solid-to-liquid ratio is: all the other were with embodiment 1 in 1: 45.
Embodiment 6
The embodiment of one group of cellulase hydrolysis aspect:
(1) to carry addition in the process be 0.01% cellulase to water, and PH is 3.0,30 degrees centigrade of temperature, and 0.5 hour time, all the other are with embodiment 1.
(2) to carry addition in the process be 0.1% cellulase to water, and PH is 3.0,33 degrees centigrade of temperature, and 2 hours time, all the other are with embodiment 1.
(3) to carry addition in the process be 0.5% cellulase to water, and PH is 3.2,40 degrees centigrade of temperature, and 1 hour time, all the other are with embodiment 1.
(4) to carry addition in the process be 0.8% cellulase to water, and PH is 3.5,45 degrees centigrade of temperature, and all the other are with embodiment 1.
(5) to carry addition in the process be 1.0% cellulase to water, and PH is 3.9,55 degrees centigrade of temperature, and all the other are with embodiment 1.
(6) to carry addition in the process be 1.2% cellulase to water, and PH is 4.4,58 degrees centigrade of temperature, and all the other are with embodiment 1.
(7) to carry addition in the process be 0.3% cellulase to water, and PH is 5.2,60 degrees centigrade of temperature, and all the other are with embodiment 1.
(8) to carry addition in the process be 0.2% cellulase to water, and PH is 6.0,31 degrees centigrade of temperature, and all the other are with embodiment 1.
(9) to carry addition in the process be 2.0% cellulase to water, and PH is 6.6,30 degrees centigrade of temperature, and all the other are with embodiment 1.
Embodiment 7
The embodiment of one histone enzymolysis aspect:
(1) the proteolytic enzyme amount is 2%, and PH is 3.5,28 degrees centigrade of temperature, and 2 hours time, all the other are with embodiment 2.
(2) the proteolytic enzyme amount is 0.1%, and PH is 2.5,25 degrees centigrade of temperature, and 0.5 hour time, all the other are with embodiment 2.
(3) the proteolytic enzyme amount is 0.2%, and PH is 3.5,30 degrees centigrade of temperature, and 0.8 hour time, all the other are with embodiment 2.
(4) the proteolytic enzyme amount is 0.3%, and PH is 4.5,35 degrees centigrade of temperature, and 1.0 hours time, all the other are with embodiment 2.
(5) the proteolytic enzyme amount is 0.5%, and PH is 5.5,40 degrees centigrade of temperature, and 1.5 hours time, all the other are with embodiment 2.
(6) the proteolytic enzyme amount is 0.8%, and PH is 2.5,45 degrees centigrade of temperature, and 2.0 hours time, all the other are with embodiment 2.
(7) the proteolytic enzyme amount is 1.2%, and PH is 2.5,50 degrees centigrade of temperature, and 2.0 hours time, all the other are with embodiment 2.
Embodiment 8
The embodiment of one group of pectin enzymolysis aspect:
(8) the polygalacturonase amount is 2%, and PH is 3.5,28 degrees centigrade of temperature, and 2 hours time, all the other are with embodiment 1.
(9) the polygalacturonase amount is 0.002%, and PH is 2.5,25 degrees centigrade of temperature, and 0.5 hour time, all the other are with embodiment 1.
(10) the polygalacturonase amount is 0.008%, and PH is 3.5,30 degrees centigrade of temperature, and 0.8 hour time, all the other are together
Embodiment 1.
(11) the polygalacturonase amount is 0.01%, and PH is 4.5,35 degrees centigrade of temperature, and 1.0 hours time, all the other are together
Embodiment 1.
(12) the polygalacturonase amount is 0.02%, and PH is 5.5,40 degrees centigrade of temperature, and 1.5 hours time, all the other are together
Embodiment 1.
(13) the polygalacturonase amount is 0.03%, and PH is 2.5,45 degrees centigrade of temperature, and 2.0 hours time, all the other are together
Embodiment 1.
(14) the polygalacturonase amount is 0.05%, and PH is 2.5,50 degrees centigrade of temperature, and 2.0 hours time, all the other are with embodiment 1.
Embodiment 9
The embodiment of one group of ultrafiltration aspect:
(1) filter residue b by solid-to-liquid ratio is: it is 85% ethanol that 1: 5 consumption adds concentration, alcohol extracting is 1 hour under temperature 60 degrees celsius, refilter, the filtrate d that obtains, elder generation's ultrafiltration, ultrafiltration employing molecular weight cut-off is 6000 ultra-filtration membrane, the liquid b1 that dams can further reclaim useful matter, and ultrafiltration obtains sees through liquid, through nanofiltration, nanofiltration employing molecular weight cut-off is 1050 nanofiltration membrane, the further refining chromocor compound that obtains of the liquid b2 that dams sees through liquid through reverse osmosis concentration through what nanofiltration obtained, and reverse osmosis pressure is 0.2-6mpa, the liquid b3 that dams that obtains can further reclaim useful matter, reverse osmosis see through liquid contain a large amount of ethanol can recycling use.All the other are with embodiment 1.
(2) filter residue b by solid-to-liquid ratio is: it is 85% ethanol that 1: 4 consumption adds concentration, alcohol extracting is 1 hour under temperature 25 degrees celsius, refilter, the filtrate d that obtains, elder generation's ultrafiltration, ultrafiltration employing molecular weight cut-off is 4000 ultra-filtration membrane, the liquid b1 that dams can further reclaim useful matter, and ultrafiltration obtains sees through liquid, through nanofiltration, nanofiltration employing molecular weight cut-off is 1000 nanofiltration membrane, the further refining chromocor compound that obtains of the liquid b2 that dams sees through liquid through reverse osmosis concentration through what nanofiltration obtained, and reverse osmosis pressure is 0.2mpa, the liquid b3 that dams that obtains can further reclaim useful matter, reverse osmosis see through liquid contain a large amount of ethanol can recycling use.。All the other are with embodiment 1.
(3) filter residue b by solid-to-liquid ratio is: it is 85% ethanol that 1: 20 consumption adds concentration, alcohol extracting is 2 hours under temperature 85 degrees celsius, refilter, the filtrate d that obtains, elder generation's ultrafiltration, ultrafiltration employing molecular weight cut-off is 7000 ultra-filtration membrane, the liquid b1 that dams can further reclaim useful matter, and ultrafiltration obtains sees through liquid, through nanofiltration, nanofiltration employing molecular weight cut-off is 900 nanofiltration membrane, the further refining chromocor compound that obtains of the liquid b2 that dams sees through liquid through reverse osmosis concentration through what nanofiltration obtained, and reverse osmosis pressure is 6mpa, the liquid b3 that dams that obtains can further reclaim useful matter, reverse osmosis see through liquid contain a large amount of ethanol can recycling use.All the other are with embodiment 1.(4) filter residue b by solid-to-liquid ratio is: it is 85% ethanol that 1: 15 consumption adds concentration, alcohol extracting is 1 hour under temperature 50 degrees celsius, refilter, the filtrate d that obtains, elder generation's ultrafiltration, ultrafiltration employing molecular weight cut-off is 5000 ultra-filtration membrane, the liquid b1 that dams can further reclaim useful matter, and ultrafiltration obtains sees through liquid, through nanofiltration, nanofiltration employing molecular weight cut-off is 1050 nanofiltration membrane, the further refining chromocor compound that obtains of the liquid b2 that dams sees through liquid through reverse osmosis concentration through what nanofiltration obtained, and reverse osmosis pressure is 0.2-6mpa, the liquid b3 that dams that obtains can further reclaim useful matter, reverse osmosis see through liquid contain a large amount of ethanol can recycling use.All the other are with embodiment 1.
Embodiment 10
The embodiment of one group of ultrafiltration aspect:
(1) filtrate a step after filtration is specially first ultrafiltration, and it is 8000 ultra-filtration membrane that molecular weight cut-off is adopted in ultrafiltration, dam liquid a1 vacuum or spraying drying, obtain polysaccharide, ultrafiltration obtains sees through liquid, through nanofiltration, nanofiltration employing molecular weight cut-off is 1100 nanofiltration membrane, the liquid a2 that dams can further reclaim useful matter, sees through liquid through reverse osmosis concentration through what nanofiltration obtained, and reverse osmosis pressure is 0.2mpa, the liquid a3 that dams that obtains contains amino acid, and the liquid water that sees through of reverse osmosis can recycling use.All the other are with embodiment 1.
(2) filtrate a step after filtration is specially first ultrafiltration, and it is 9000 ultra-filtration membrane that molecular weight cut-off is adopted in ultrafiltration, dam liquid a1 vacuum or spraying drying, obtain polysaccharide, ultrafiltration obtains sees through liquid, through nanofiltration, nanofiltration employing molecular weight cut-off is 400 nanofiltration membrane, the liquid a2 that dams can further reclaim useful matter, sees through liquid through reverse osmosis concentration through what nanofiltration obtained, and reverse osmosis pressure is 6mpa, the liquid a3 that dams that obtains contains amino acid, and the liquid water that sees through of reverse osmosis can recycling use.All the other are with embodiment 1.
(3) filtrate a step after filtration is specially first ultrafiltration, and it is 12000 ultra-filtration membrane that molecular weight cut-off is adopted in ultrafiltration, dam liquid a1 vacuum or spraying drying, obtain polysaccharide, ultrafiltration obtains sees through liquid, through nanofiltration, nanofiltration employing molecular weight cut-off is 8000 nanofiltration membrane, the liquid a2 that dams can further reclaim useful matter, sees through liquid through reverse osmosis concentration through what nanofiltration obtained, and reverse osmosis pressure is 3mpa, the liquid a3 that dams that obtains contains amino acid, and the liquid water that sees through of reverse osmosis can recycling use.All the other are with embodiment 1.
(4) filtrate a step after filtration is specially first ultrafiltration, and it is 10500 ultra-filtration membrane that molecular weight cut-off is adopted in ultrafiltration, dam liquid a1 vacuum or spraying drying, obtain polysaccharide, ultrafiltration obtains sees through liquid, through nanofiltration, nanofiltration employing molecular weight cut-off is 7000 nanofiltration membrane, the liquid a2 that dams can further reclaim useful matter, sees through liquid through reverse osmosis concentration through what nanofiltration obtained, and reverse osmosis pressure is 1mpa, the liquid a3 that dams that obtains contains amino acid, and the liquid water that sees through of reverse osmosis can recycling use.All the other are with embodiment 1.
(5) filtrate a step after filtration is specially first ultrafiltration, and it is 10000 ultra-filtration membrane that molecular weight cut-off is adopted in ultrafiltration, dam liquid a1 vacuum or spraying drying, obtain polysaccharide, ultrafiltration obtains sees through liquid, through nanofiltration, nanofiltration employing molecular weight cut-off is 4000 nanofiltration membrane, the liquid a2 that dams can further reclaim useful matter, sees through liquid through reverse osmosis concentration through what nanofiltration obtained, and reverse osmosis pressure is 3mpa, the liquid a3 that dams that obtains contains amino acid, and the liquid water that sees through of reverse osmosis can recycling use.All the other are with embodiment 1.
(6) filtrate a step after filtration is specially first ultrafiltration, and it is 12000 ultra-filtration membrane that molecular weight cut-off is adopted in ultrafiltration, dam liquid a1 vacuum or spraying drying, obtain polysaccharide, ultrafiltration obtains sees through liquid, through nanofiltration, nanofiltration employing molecular weight cut-off is 3000 nanofiltration membrane, the liquid a2 that dams can further reclaim useful matter, sees through liquid through reverse osmosis concentration through what nanofiltration obtained, and reverse osmosis pressure is 3mpa, the liquid a3 that dams that obtains contains amino acid, and the liquid water that sees through of reverse osmosis can recycling use.All the other are with embodiment 1.
(7) filtrate a step after filtration is specially first ultrafiltration, and it is 10000 ultra-filtration membrane that molecular weight cut-off is adopted in ultrafiltration, dam liquid a1 vacuum or spraying drying, obtain polysaccharide, ultrafiltration obtains sees through liquid, through nanofiltration, nanofiltration employing molecular weight cut-off is 2000 nanofiltration membrane, the liquid a2 that dams can further reclaim useful matter, sees through liquid through reverse osmosis concentration through what nanofiltration obtained, and reverse osmosis pressure is 4mpa, the liquid a3 that dams that obtains contains amino acid, and the liquid water that sees through of reverse osmosis can recycling use.All the other are with embodiment 1.
(8) filtrate a step after filtration is specially first ultrafiltration, and it is 12000 ultra-filtration membrane that molecular weight cut-off is adopted in ultrafiltration, dam liquid a1 vacuum or spraying drying, obtain polysaccharide, ultrafiltration obtains sees through liquid, through nanofiltration, nanofiltration employing molecular weight cut-off is 500 nanofiltration membrane, the liquid a2 that dams can further reclaim useful matter, sees through liquid through reverse osmosis concentration through what nanofiltration obtained, and reverse osmosis pressure is 3mpa, the liquid a3 that dams that obtains contains amino acid, and the liquid water that sees through of reverse osmosis can recycling use.All the other are with embodiment 1.
(9) filtrate a step after filtration is specially first ultrafiltration, and it is 12000 ultra-filtration membrane that molecular weight cut-off is adopted in ultrafiltration, dam liquid a1 vacuum or spraying drying, obtain polysaccharide, ultrafiltration obtains sees through liquid, through nanofiltration, nanofiltration employing molecular weight cut-off is 700 nanofiltration membrane, the liquid a2 that dams can further reclaim useful matter, sees through liquid through reverse osmosis concentration through what nanofiltration obtained, and reverse osmosis pressure is 3mpa, the liquid a3 that dams that obtains contains amino acid, and the liquid water that sees through of reverse osmosis can recycling use.All the other are with embodiment 1.
(10) filtrate a step after filtration is specially first ultrafiltration, and it is 12000 ultra-filtration membrane that molecular weight cut-off is adopted in ultrafiltration, dam liquid a1 vacuum or spraying drying, obtain polysaccharide, ultrafiltration obtains sees through liquid, through nanofiltration, nanofiltration employing molecular weight cut-off is 800 nanofiltration membrane, the liquid a2 that dams can further reclaim useful matter, sees through liquid through reverse osmosis concentration through what nanofiltration obtained, and reverse osmosis pressure is 3mpa, the liquid a3 that dams that obtains contains amino acid, and the liquid water that sees through of reverse osmosis can recycling use.All the other are with embodiment 1.
Embodiment 11
It is 4 purpose fine powders that pulverization process is pulverized the Sweet Potato Leaf rattan, and all the other are with embodiment 1.
Embodiment 12
It is 200 purpose fine powders that pulverization process is pulverized the Sweet Potato Leaf rattan, and all the other are with embodiment 1.
Embodiment 13
It is 100 purpose fine powders that pulverization process is pulverized the Sweet Potato Leaf rattan, and all the other are with embodiment 1.
Embodiment 14
It is 150 purpose fine powders that pulverization process is pulverized the Sweet Potato Leaf rattan, and all the other are with embodiment 1.
Embodiment 15
It is 60 purpose fine powders that pulverization process is pulverized the Sweet Potato Leaf rattan, and all the other are with embodiment 1.
Embodiment 16
It is 15 purpose fine powders that pulverization process is pulverized the Sweet Potato Leaf rattan, and all the other are with embodiment 1.
Claims (6)
1, extraction of effective components in a kind of Sweet Potato Leaf rattan, the Sweet Potato Leaf rattan is through the pre-treatment of routine, and Jia Shuishui carries, and filters, and obtains filtrate a and filter residue b; Filtrate a and filter residue b further extract each effective constituent, it is characterized in that: the solid-to-liquid ratio between pretreated Sweet Potato Leaf rattan and the amount of water is: 1: 3-50; Water is carried in the process and to be adopted addition is that the polygalacturonase of 0.002-0.05% carries out enzymolysis, pectin enzymatic hydrolysis condition: PH is 3.0-6.0, temperature 40-60 degree centigrade, time 0.2-2 hour, polygalacturonase also increases the fiber enzymolysis step after separating end, the fiber enzymatic hydrolysis condition: the cellulase amount is 0.1-2%, and PH is 3.0-6.0, temperature 30-60 degree centigrade, time 0.5-2 hour.
2, extraction of effective components in the Sweet Potato Leaf rattan according to claim 1, it is characterized in that: water is put forward process also increases the proteolysis step, the proteolysis condition: the proteolytic enzyme amount is 0.1-2%, and PH is 2-5.5, temperature 25-50 degree centigrade, time 0.3-2 hour.
3, extraction of effective components in the Sweet Potato Leaf rattan according to claim 1 and 2, it is characterized in that: filtrate a is step after filtration, be specially first ultrafiltration, it is the ultra-filtration membrane of 8000-12000 that molecular weight cut-off is adopted in ultrafiltration, dam liquid a1 vacuum or spraying drying, obtain polysaccharide, ultrafiltration obtains sees through liquid, through nanofiltration, it is the nanofiltration membrane of 400-8000 that molecular weight cut-off is adopted in nanofiltration, and the liquid a2 that dams can further reclaim useful matter, see through liquid through reverse osmosis concentration through what nanofiltration obtained, reverse osmosis pressure is 0.2-6mpa, and the liquid a3 that dams that obtains contains amino acid, and the liquid water that sees through of reverse osmosis can recycling use.
4, extraction of effective components in the Sweet Potato Leaf rattan according to claim 1, it is characterized in that: pre-treatment also comprises pulverization process, pulverization process is pulverized the Sweet Potato Leaf rattan and is 4-200 purpose fine powder.
5, extraction of effective components in the Sweet Potato Leaf rattan according to claim 1, it is characterized in that: filter residue b by solid-to-liquid ratio is: 1: the consumption of 2-20 adds the ethanol that concentration is 50%-95%, under temperature 25-85 degrees celsius alcohol extracting 0.3-2 hour, refilter, the filtrate d that obtains, elder generation's ultrafiltration, it is the ultra-filtration membrane of 4000-7000 that molecular weight cut-off is adopted in ultrafiltration, the liquid b1 that dams can further reclaim useful matter, ultrafiltration obtains sees through liquid, through nanofiltration, it is the nanofiltration membrane of 400-1100 that molecular weight cut-off is adopted in nanofiltration, the further refining chromocor compound that obtains of the liquid b2 that dams, see through liquid through reverse osmosis concentration through what nanofiltration obtained, reverse osmosis pressure is 0.2-6mpa, and the liquid b3 that dams that obtains can further reclaim useful matter, reverse osmosis see through liquid contain a large amount of ethanol can recycling use.
6, extraction of effective components in the Sweet Potato Leaf rattan according to claim 3 is characterized in that: it is the nanofiltration membrane of 400-1100 that molecular weight cut-off is adopted in nanofiltration, and the liquid a2 that dams contains chromocor compound.
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| CNB2004100158079A CN100449001C (en) | 2004-01-08 | 2004-01-08 | Method for extracting effective component of sweet potato leaf stalk vine |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106902540A (en) * | 2017-04-21 | 2017-06-30 | 浩宇康宁健康科技（湖北）有限公司 | The holographic biochemistry high-valued extraction separation method of physics coupled system of Chinese medicine and Magnolia cortex P.E |
| CN108634313A (en) * | 2018-05-11 | 2018-10-12 | 江苏大学 | A kind of sweet potato stem leaf high nutrition activity extract and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1030892C (en) * | 1992-05-25 | 1996-02-07 | 王寒 | Method for producing sweet potato series health products |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106902540A (en) * | 2017-04-21 | 2017-06-30 | 浩宇康宁健康科技（湖北）有限公司 | The holographic biochemistry high-valued extraction separation method of physics coupled system of Chinese medicine and Magnolia cortex P.E |
| CN108634313A (en) * | 2018-05-11 | 2018-10-12 | 江苏大学 | A kind of sweet potato stem leaf high nutrition activity extract and preparation method thereof |
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