CN102861130A - Preparation method of hops total flavone with hops stem and leaf and imperfect flower as raw materials - Google Patents
Preparation method of hops total flavone with hops stem and leaf and imperfect flower as raw materials Download PDFInfo
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- CN102861130A CN102861130A CN2012104121839A CN201210412183A CN102861130A CN 102861130 A CN102861130 A CN 102861130A CN 2012104121839 A CN2012104121839 A CN 2012104121839A CN 201210412183 A CN201210412183 A CN 201210412183A CN 102861130 A CN102861130 A CN 102861130A
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Abstract
The invention relates to a preparation method of hops total flavone with hops stem and leaf and imperfect flower as raw materials. The method comprises the steps as follows: getting a byproduct (waste)-stem and leaf and the imperfect flower produced in the production of the hops as the raw materials to extract the hops total flavone rich in active components; crushing the stem and leaf and the imperfect flower of the hops through a crushing machine, and drying; extracting with the ethanol as the solvent; filtering; carrying out membrane concentration; then carrying out vacuum concentration, thus obtaining 30-40% of hops total flavone. According to the preparation method provided by the invention, most of the ethanol in the extracting liquid is separated through the nanofiltration membrane at a low temperature; the ethanol has no phase change during the concentrating process; the damage to the effective components and the energy consumption are reduced; the separated ethanol can be directly recycled again, so that the cost is reduced, the production efficiency and the comprehensive utilization rate of the hops are improved, and the added value of products can be increased.
Description
Technical field
The invention belongs to processing of farm products and comprehensive utilization technique field, relate to a kind of Flos lupuli (Flos Humuli Lupuli) total flavones preparation method take Flos lupuli (Flos Humuli Lupuli) stem and leaf and inferior flower as raw material.
Background technology
Flos lupuli (Flos Humuli Lupuli) (
Humunus Lupulus L) its formal name used at school is Fols lupuli, claims again Flos lupuli, hop and hops, is the perennial herbaceous stem of the Moraceae Humulus liana of overgrowing.Flower unisexuality, dioecism is brewageed the used female flower that is.The female flower quirk is yellow or yellow green, is the strobile shape, long 2-4cm.Per 2 life one bracts are arranged in a rotund spike in armpit by 30-50 bract imbricate on floral axis, and the base portion of bract has the body of gland of many secretion resins, hop oil, isoamylene radical chromocor, is the Fols lupuli gland.The geographical position that Flos lupuli (Flos Humuli Lupuli) distributes is north latitude 40-60 degree, originates in Europe, Asia and America.China plantation area mainly is distributed in Xinjiang, Gansu, Inner Mongol, and the provinces and regions such as Shaanxi, Liaoning, Jilin, Heilungkiang, Hebei, Shandong all have promotes and cultivation.
The chemical constituent of Flos lupuli (Flos Humuli Lupuli) can be summarized as several aspects such as resin, volatile oil, polyphenol compound, flavone compound.The resin main component is alpha-acid (.alpha.-bitter acid etc.) and β-acid (.beta.-bitter acid etc.), studies show that alpha-acid and β-acid are the antibacterial main effective ingredient of Flos lupuli (Flos Humuli Lupuli), and β-acid is being better than alpha-acid aspect tubercule bacillus, bacillus subtilis, the staphylococcus aureus antibacterial action
[2]The volatile oil kind is kind more than ten in the Flos lupuli (Flos Humuli Lupuli), be mainly myrcene (myrcene 30%-50%) Humuleno (humu1ene 8%-33%), and a small amount of linalool (linalool), humulus alcohol (geraniol), Fols lupuli alcohol (luparenol) etc.Flavonoid mainly is the compositions such as flavonol, flavone former times, prenyl are looked into youngster's ketone, different canopy skin element, nimbecetin is general, Folium Symplocoris Caudatae is general.By the amplification in vitro that studies show that the Flos lupuli (Flos Humuli Lupuli) Flavonoid substances can anticancer, flavone also has antibiotic, estrogen-like function, presses down the effect such as hyperosteogeny in the Flos lupuli (Flos Humuli Lupuli).Polyphenol compound Wheat Protein in the Flos lupuli (Flos Humuli Lupuli) mainly is flavan-3-alcohol, as: catechin, epicatechin and leucoanthocyanidin.In addition, Flos lupuli (Flos Humuli Lupuli) also contains the compositions such as choline, fructose (about 0.15%), sucrose (0.22%), glucose (0.41%) and lipoid, crude fibre (16.7%), crude protein (22.4%).The leaf of Flos lupuli (Flos Humuli Lupuli) and spend in contain Leucodelphinidin (leucodelphinidin) and white arrow Aster dubius (Thunb.) Onno aglycon (leucocyanidin), also contain kaempferol (kaempferol) in the leaf.The research report of relevant Flos lupuli (Flos Humuli Lupuli) stem and leaf is rarely seen, and Shandong is among the people has obtained preferably effect with Flos lupuli (Flos Humuli Lupuli) stem and leaf treatment cancer.Also be rich in flavone compound in the Flos lupuli (Flos Humuli Lupuli) stem and leaf, general flavone content is 1.4% in the bine according to surveying and determination, and the general flavone content in the medicated beer floral leaf is 1%.The ethanol extraction that shows after deliberation the Flos lupuli (Flos Humuli Lupuli) stem and leaf has obvious dose-dependent inhibition effect to A549 and H epG2 Growth of Cells, wherein, there is stronger antitumor action at the ethyl acetate extraction position, and therefrom identifies B-sitosterol, B-daucosterol, Quercetin, Quercitroside and 5 chemical compounds of hyperin.
Xinjiang is owing to have climate resources, geographical position and the wide land resource of the superior uniqueness of suitable Flos lupuli (Flos Humuli Lupuli) growth promoter, become the important base that the Domestic Beer Semen arachidis hypogaeae produces, at present, 2740 hectares of full boundary plantation Flos lupuli (Flos Humuli Lupuli)s, cultivated area accounts for 65% of the whole nation, average every per mu yield is spent 280 kilograms, and 11628 tons of gross outputs are the major production areas of domestic and international Flos lupuli (Flos Humuli Lupuli).The Flos lupuli (Flos Humuli Lupuli) of China's export almost all originates in Xinjiang, and also being supplied by Xinjiang more than 70% of sold inside the country Flos lupuli (Flos Humuli Lupuli) supplied the medicated beer producer in the whole nation 70%, and found a good sale in tens countries such as English, moral.
Flos lupuli (Flos Humuli Lupuli) is how ripe in mid-August, and three autumn jobs as harvesting, tilling and planting rush season at a time when this, labour force's wretched insufficiency, and heat bring very big difficulty for artificial the harvesting, and the efficient of gathering is very low.At present, the Xinjiang growing area adopts mechanical picking to clean Flos lupuli (Flos Humuli Lupuli) mostly, greatly improves the picking efficiency of Flos lupuli (Flos Humuli Lupuli).At present, mechanical picking is cleaned the mode that Flos lupuli (Flos Humuli Lupuli) generally adopts and is: Flos lupuli (Flos Humuli Lupuli) is together gathered together with stem and leaf is transported to factory, and recycling mechanical picking cleaner separates the stem and leaf of Flos lupuli (Flos Humuli Lupuli), and the amount of this part stem and leaf accounts for Flos lupuli (Flos Humuli Lupuli) output 3-5 doubly.
Mechanical picking sorting Flos lupuli (Flos Humuli Lupuli), be subjected to the impact of pick up rate, loss rate and the breakage rate of mechanical picking screening installation, the loss rate of Flos lupuli (Flos Humuli Lupuli) is generally at 10-30% in the actual production, the Flos lupuli (Flos Humuli Lupuli) of this part loss is mingled in can't be recycled in the stem and leaf and go out of use, and causes very large resource allocation waste.Because Flos lupuli (Flos Humuli Lupuli) stem and leaf height combines in medicated beer flower shop, for comprehensive utilization provides advantage.
The Study on Extraction Method of flavone compound report is a lot of at present, large multiplex solvent extraction, and the extraction solvent that usage comparison is many is mainly the ethanol of variable concentrations.Use the solvent extraction natural product, general solid-liquid ratio is at 1:5-1:20, solvent load is large, heating extraction liquid evaporation desolventizing is all adopted in the recovery concentrated and solvent of extracting solution, the solvent vapo(u)r condensation is reclaimed, solvent generation secondary phase changes again, and energy consumption is high, improve the cost of by-product utilized, increased the difficulty that byproduct comprehensive utilizes.
Summary of the invention
Goal of the invention is, a kind of Flos lupuli (Flos Humuli Lupuli) total flavones preparation method take Flos lupuli (Flos Humuli Lupuli) stem and leaf and inferior flower as raw material is provided.The method be from the Flos lupuli (Flos Humuli Lupuli) production process by-product (garbage)-stem and leaf, inferiorly spend middle Extraction and enrichment flavone compound, employing with bine, leaf, inferior flower through chipper chopping, drying, ethonal extraction, filter, utilize NF membrane to leach ethanol in the extracting solution, again through vacuum concentration, obtaining content is the Flos lupuli (Flos Humuli Lupuli) total flavones of 30-40% after concentrated.The present invention adopts the most of ethanol in the nanofiltration membrane separation extracting solution under the low temperature, ethanol does not undergo phase transition in concentration process, destruction and energy resource consumption to effective ingredient have been reduced, isolated ethanol can directly recycle again, reduce cost, improved comprehensive utilization ratio and the added value of product of production efficiency and Flos lupuli (Flos Humuli Lupuli).
The invention provides a kind ofly take Flos lupuli (Flos Humuli Lupuli) stem and leaf and inferior flower as the Flos lupuli (Flos Humuli Lupuli) total flavones preparation method of raw material, follow these steps to carry out:
A, Flos lupuli (Flos Humuli Lupuli) stem and leaf and inferior flower are chopped into 0.5-2cm, are dried to water content 8-20%;
B, with the extraction pot of packing into of the dry thing among the step a, extract as 50-95% ethanol as solvent take 5-15 concentration doubly, temperature 20-70 ℃, time 1-6h obtains extracting solution;
C, the extracting solution among the step b is filtered with diatomite filter or butterfly chip filter centrifugal, remove the particle in the extracting solution;
D, with the extracting solution Al among the step c
2O
3, Al
2O
3+ TiO
2Or Al
2O
3+ ZnO
2For the inoranic membrane of membrane material carries out ultrafiltration, temperature 20-50 ℃, pressure is 0.1-0.3MPa, and flow velocity 2-3.5m/s removes small float and colloidal substance in the extracting solution;
E, the extracting solution of steps d is leached the ethanol of 50-80% in the extracting solution by polysulfones, polyether sulfone or Kynoar NF membrane, temperature is 20-50 ℃, and operating pressure is 0.4-0.8MPa, flow velocity 2-3.5m/s, concentrated, Recycled ethanol, wherein the molecular cut off of NF membrane is 200-1000MW;
F, the extracting solution after step e is concentrated are again through vacuum concentration, and temperature is 40-70 ℃, and vacuum is 0.05-0.08MPa, removes alcohol solvent, and can obtain content is the Flos lupuli (Flos Humuli Lupuli) total flavones of 30-40%.
Ultrafilter membrane pattern in the steps d is the tubular type of external-compression type or inner pressed, and membrane aperture is 0.1-0.2 μ m.
NF membrane is polysulfone membrane among the step e.
The molecular cut off of step e NF membrane is 300-500MW.
The membranous type formula of step e NF membrane is external-compression type or inner pressed tubular membrane or multichannel tube bank formula.
A kind of Flos lupuli (Flos Humuli Lupuli) total flavones preparation method take Flos lupuli (Flos Humuli Lupuli) stem and leaf and inferior flower as raw material of the present invention, the by-product (garbage) that the method is produced take Flos lupuli (Flos Humuli Lupuli)-stem and leaf, inferior flower extract the Flos lupuli (Flos Humuli Lupuli) total flavones that is rich in active component as raw material, reduced the wasting of resources, the comprehensive utilization ratio and the added value of product that have improved.The present invention adopts the most of solvent in the nanofiltration membrane separation extracting solution, realizes the preliminary of extracting solution concentrated, and the ethanol in the nanofiltration membrane separation extracting solution, ethanol does not undergo phase transition, and significantly reduces energy resource consumption; Isolated ethanol can be directly used in and extract next time, has improved production efficiency; Membrance separation ethanol is to carry out at normal temperatures, and the low destruction of having reduced effective ingredient of temperature has been improved effective component yield.
The specific embodiment
Embodiment 1
A, Flos lupuli (Flos Humuli Lupuli) stem and leaf and inferior flower are chopped into 0.5cm, are dried to water content 8%;
B, the dry thing 100Kg among the step a is packed in the extraction pot, the concentration that adds 5 times is that 50% alcohol solvent extracts, 20 ℃ of temperature, and time 1h obtains extracting solution;
C, the extracting solution among the step b is filtered with diatomite filter, remove the particle in the extracting solution;
D, with the extracting solution among the step c with inner pressed tubular type ultrafilter, Al
2O
3For membrane material carries out ultrafiltration, membrane aperture is 0.1 μ m, 20 ℃ of temperature, and pressure is 0.1MPa, flow velocity 2m/s removes small float and colloidal substance in the extracting solution;
E, with the extracting solution of steps d by inner pressed pipe collecting and filtering apparatus, molecular cut off is that the polysulfones NF membrane of 200MW leaches in the extracting solution 50% ethanol, temperature is 20 ℃, operating pressure is 0.4MPa, flow velocity 2m/s is concentrated, Recycled ethanol;
F, the extracting solution after step e is concentrated are again through vacuum concentration, and temperature is 40 ℃, and vacuum is 0.05MPa, removes alcohol solvent, and can obtain content is the Flos lupuli (Flos Humuli Lupuli) total flavones of 30-40%.
Embodiment 2
A, Flos lupuli (Flos Humuli Lupuli) stem and leaf and inferior flower are chopped into 1.5cm, are dried to water content 10%;
B, with the extraction pot of packing into of the dry thing 50Kg among the step a, extract take 15 times concentration as 95% alcohol solvent, temperature 50 C, time 5h obtains extracting solution;
C, the extracting solution among the step b is filtered with butterfly chip filter centrifugal, remove the particle in the extracting solution;
D, with the extracting solution among the step c with external-compression type tubular type ultrafilter, Al
2O
3+ TiO
2For membrane material carries out ultrafiltration, membrane aperture is 0.2 μ m, 40 ℃ of temperature, and pressure is 0.2MPa, flow velocity 3m/s removes small float and colloidal substance in the extracting solution;
E, with the extracting solution of steps d by external-compression type tubular type collecting and filtering apparatus, molecular cut off is that the 500MW polyether sulfone filtering film leaches in the extracting solution 70% ethanol, temperature is 40 ℃, operating pressure is 0.6MPa, flow velocity 3m/s is concentrated, Recycled ethanol;
F, the extracting solution after step e is concentrated are again through vacuum concentration, and temperature is 50 ℃, and vacuum is 0.06MPa, removes alcohol solvent, and can obtain content is the Flos lupuli (Flos Humuli Lupuli) total flavones of 30-40%.
Embodiment 3
A, Flos lupuli (Flos Humuli Lupuli) stem and leaf and inferior flower are chopped into 2cm, are dried to water content 15%;
B, with the extraction pot of packing into of the dry thing 150Kg among the step a, extract as 75% ethanol as solvent take 10 times concentration, temperature 70 C, time 6h obtains extracting solution;
C, the extracting solution among the step b is filtered with diatomite filter, remove the particle in the extracting solution;
D, with the extracting solution among the step c with the tubular type ultrafilter of inner pressed, Al
2O
3+ ZnO
2For membrane material carries out ultrafiltration, membrane aperture is 0.2 μ m, and temperature 50 C, pressure are 0.3MPa, and flow velocity 3.5m/s removes small float and colloidal substance in the extracting solution;
E, the extracting solution of steps d is restrained formula by multichannel, molecular cut off is that the Kynoar NF membrane of 800MW leaches in the extracting solution 80% ethanol, and temperature is 50 ℃, and operating pressure is 0.8MPa, and flow velocity 3.5m/s is concentrated, Recycled ethanol;
F, the extracting solution after step e is concentrated are again through vacuum concentration, and temperature is 70 ℃, and vacuum is 0.08MPa, removes alcohol solvent, and can obtain content is the Flos lupuli (Flos Humuli Lupuli) total flavones of 30-40%.
Embodiment 4
A, Flos lupuli (Flos Humuli Lupuli) stem and leaf and inferior flower are chopped into 1.0cm, are dried to water content 20%;
B, with the extraction pot of packing into of the dry thing 80kg among the step a, extract as 90% ethanol as solvent take 12 times concentration, 40 ℃ of temperature, time 3h obtains extracting solution;
C, the extracting solution among the step b is filtered with butterfly chip filter centrifugal, remove the particle in the extracting solution;
D, with the extracting solution among the step c with the tubular type ultrafilter Al of external-compression type
2O
3For membrane material carries out ultrafiltration, membrane aperture is 0.1 μ m, 35 ℃ of temperature, and pressure is 0.2MPa, flow velocity 2.5m/s removes small float and colloidal substance in the extracting solution;
E, with the extracting solution of steps d by inner pressed tubular type collecting and filtering apparatus, molecular cut off is 1000MW, the polysulfones NF membrane leaches in the extracting solution 75% ethanol, temperature is 35 ℃, operating pressure is 0.6MPa, flow velocity 2.5m/s is concentrated, Recycled ethanol;
F, the extracting solution after step e is concentrated are again through vacuum concentration, and temperature is 60 ℃, and vacuum is 0.07MPa, removes alcohol solvent, and can obtain content is the Flos lupuli (Flos Humuli Lupuli) total flavones of 30-40%.
Claims (5)
1. one kind take Flos lupuli (Flos Humuli Lupuli) stem and leaf and inferior flower as the Flos lupuli (Flos Humuli Lupuli) total flavones preparation method of raw material, it is characterized in that following these steps to carrying out:
A, Flos lupuli (Flos Humuli Lupuli) stem and leaf and inferior flower are chopped into 0.5-2cm, are dried to water content 8-20%;
B, with the extraction pot of packing into of the dry thing among the step a, extract as 50-95% ethanol as solvent take 5-15 concentration doubly, temperature 20-70 ℃, time 1-6h obtains extracting solution;
C, the extracting solution among the step b is filtered with diatomite filter or butterfly chip filter centrifugal, remove the particle in the extracting solution;
D, with the extracting solution Al among the step c
2O
3, Al
2O
3+ TiO
2Or Al
2O
3+ ZnO
2For the inoranic membrane of membrane material carries out ultrafiltration, temperature 20-50 ℃, pressure is 0.1-0.3MPa, and flow velocity 2-3.5m/s removes small float and colloidal substance in the extracting solution;
E, the extracting solution of steps d is leached the ethanol of 50-80% in the extracting solution by polysulfones, polyether sulfone or Kynoar NF membrane, temperature is 20-50 ℃, and operating pressure is 0.4-0.8MPa, flow velocity 2-3.5m/s, concentrated, Recycled ethanol, wherein the molecular cut off of NF membrane is 200-1000MW;
F, the extracting solution after step e is concentrated are again through vacuum concentration, and temperature is 40-70 ℃, and vacuum is 0.05-0.08MPa, removes alcohol solvent, and can obtain content is the Flos lupuli (Flos Humuli Lupuli) total flavones of 30-40%.
2. method according to claim 1 is characterized in that the ultrafilter membrane pattern in the steps d is the tubular type of external-compression type or inner pressed, and membrane aperture is 0.1-0.2 μ m.
3. method according to claim 1 is characterized in that NF membrane is polysulfone membrane among the step e.
4. method according to claim 3, the molecular cut off that it is characterized in that step e NF membrane is 300-500MW.
5. method according to claim 1, the membranous type formula that it is characterized in that step e NF membrane are external-compression type or inner pressed tubular membrane or multichannel tube bank formula.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108498380A (en) * | 2018-05-30 | 2018-09-07 | 广州市康超信息科技有限公司 | A kind of hops facial mask and preparation method thereof |
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2012
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| CN101132807A (en) * | 2005-03-03 | 2008-02-27 | 札幌啤酒株式会社 | Antiallergic composition |
| CN1814094A (en) * | 2005-12-21 | 2006-08-09 | 宾晓辉 | Fat-reducing health-care product |
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|---|
| 白璐: "啤酒花浸膏加工工艺研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑 （月刊 ）》, no. 1, 31 January 2012 (2012-01-31), pages 024 - 83 * |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108498380A (en) * | 2018-05-30 | 2018-09-07 | 广州市康超信息科技有限公司 | A kind of hops facial mask and preparation method thereof |
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Application publication date: 20130109 |