CN101570556A - Method for extracting secoisolariciresinol diglucoside from flax seeds or husks, extract obtained and use thereof - Google Patents
Method for extracting secoisolariciresinol diglucoside from flax seeds or husks, extract obtained and use thereof Download PDFInfo
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Abstract
The invention relates to a method for extracting secoisolariciresinol diglucoside from degummed flax seeds or husks, an extract containing the secoisolariciresinol diglucoside and use thereof. The method comprises crushing the degummed flax seeds or husks, degreasing, ultrasonic-microwave synergistic extracting, separating, depressurizing and concentrating, and drying to obtain the extract containing the secoisolariciresinol diglucoside. The method has high extraction rate for secoisolariciresinol diglucoside and high economical efficiency, and the extract is widely applied to bakery products, beverages, snack foods and the like and has great market potential.
Description
[technical field]
The present invention relates to Food science field and oil crops processing technique field.More specifically, the rich shell that the present invention relates to degummed flax seeds or degummed flax seeds partly is the method that raw material extracts secoisolariciresinol diglycoside, relates to and contains secoisolariciresinol diglycoside extract and uses thereof.
[background technology]
Flax (Linum usitatissimum L) claim flax again, belongs to the flax family (Linaceae) linum, is one of the most ancient crop.Linseed oil is the seed in the fruit of flax railway carriage or compartment, and each railway carriage or compartment really contains seed 6-10 grain.The linseed oil shell is hard, shell-containing rate 42%-50%, kernel-containing rate 50%-58%.In recent decades, the bioactive ingredients in the linseed oil is found by the investigator gradually and is familiar with that the development and use of foodstuffs industry bound pair linseed oil show more and more stronger interest.At first be to be rich in linolenic linseed oil, they have very big help to the control of cardiovascular disorder.Next is a rich dietary fiber in the linseed oil, wherein most important parts is the food fibre of solubility a---flaxseed gum, it is a kind of natural crossing polysaccharide, has high viscosity, strong retentiveness, good emulsifying property, foaminess and stability, but blood fat reducing, and have reducing weight and beautifying features and nutrition health protection effect.Closely during the last ten years, the phytoestrogen constituents, particularly open loop secoisolariciresinoldiglucoside diglucoside (SDG) that is rich in the linseed oil receives investigator's concern.The content of SDG in linseed oil is far above other crops, also be topmost lignan in the linseed oil simultaneously, to alleviating menopausal symptom, inhibition human body mammary cancer, prostate cancer, the rectum cancer, useful effect is all brought into play in aspects such as assisting therapy lupus nephritis and diabetes.In addition, secoisolariciresinol diglycoside still is a kind of good natural antioxidants.Because the multiple bioactive ingredients that is rich in the linseed oil, American National ICR (NCI) is classified linseed oil one of as 6 kinds of plants for anticancer research objects, and its development and use have become the focus of development functionality food and food ingredients.
Yet owing to lack scientific understanding and processing means, the development and use of China's linseed oil are in for a long time than the primary level.Up to now, how linseed oil is as the oil expression raw material, and usually as feed, utilization ratio is lower for the grouts after the oil expression.How to make full use of three kinds of main biologically active substance-linseed oil, flaxseed gum and secoisolariciresinol diglycosides in the linseed oil, become the focus of current comprehensive utilization flax resource.
From the end of the nineties to the beginning of this century, the farm crop in research centre, Canada Saskatoon utilize the University of Helsinki of North Dakota State University, Sweden University of Agricultural Sciences and the Finland of portion, University of Saskachewan, University of Toronto, the U.S. carrying out extensive studies aspect linseed oil processing and the secoisolariciresinol diglycoside exploitation, the particularly research aspect the secoisolariciresinol diglycoside biological activity, for its development and use and dietary supplementation lay a good foundation.
Aspect the extraction of secoisolariciresinol diglycoside, Bakke and Klosterman have proposed a strip adoption 95% ethanol and 1 when finding SDG, 4-dioxane (1: 1, v/v) extract technology (Bakke J E and Klosterman H J.A new diglucoside fromflaxseed.Proceedings of the North Dakota Academy of Science, 1956 (10): 18-22) of SDG as solvent.After this, Muir and Westcott propose to use a kind of fatty alcohol solution (methyl alcohol or ethanol) to extract the lignan precursor substance from flax seed degreased dreg, adopt basic hydrolysis to discharge lignan then, separation and purification obtains the pure product of SDG (Muir A D and Westcott N D.Process for extractingand purifying lignans and cinnamic acid derivatives from flaxseed.CA 2216979.1996-10-03) then.Subsequently, Westcott and Paton adopt similar method to extract the mixture of SDG and HMGA and styracin glucoside (Westcott N D and Paton D.Complex containing lignan from linseed oil, phenolic and aliphatic substances from flax andprocess for preparing.US 6,264,853.2001-07-24).Dobbins and Wiley then adopt aqueous acetone solution to extract SDG, and the method that adopts basic hydrolysis to discharge SDG then obtains secoisolariciresinol diglycoside (Dobbins T A and Wiley D B.A process for recovering secoisolariciresinoldiglycoside from de-fatted flaxseed.WO03084974 2003-10-16).Heintzman and Bennett (Heintzman R and Bennett M L.Process for extraction and stabilizationof phytoestrogens from flaxseed and product therefrom.US 20030060420.2003-03-27), (Pihlava J M such as Pihlava, Hyvarinen H, Ryhanen E L, et al.Processfor isolating and purifying secoisolariciresinol diglcoside from flaxseed.US2004030108.2004-02-12) all adopts ethanolic soln from the linseed meal of degreasing, to extract and obtain SDG.Shukla etc. (Shukla R, Hilaly A K and Moore K M.Process for obtaininglignan.US 6,767,565 2004-07-27) also propose to adopt the method for solvent extraction to prepare SDG.Abe etc. (Abe K, Iino T, Fujii W, et al.Process for producing SDG and foods anddrinks containing the same.US2005158435 2005-07-21) then adopt the ethanolic soln that adds alkali to extract SDG.Domestic at the early-stage aspect the extraction purifying of SDG.(Wu Meijuan such as Wu Meijuan, Li Yulin, Tang Luoxiang etc. by the method .CN1162438.2003-02-05 of linseed meal extraction, separation and purifying SDG) studied by the linseed meal extraction, separated and the method for purifying SDG, propose one and extract route with Muir and the similar SDG of Westcott method therefor.(Wang Hao such as Wang Hao, Xiong Fei, Wu Jiajun etc. the preparation method of flaxseed lignan total glycoside extract and application .CN1749262.2006-03-22 thereof) adopt low-alcohol solution from flaxseed meal or flax seed husk, to extract SDG equally, (Liu Dachuan such as Liu Dachuan, Pang Meixia, Wu Bo. Linseed Lignans---open loop secoisolariciresinoldiglucoside diglucoside Study on extraction process. Chinese oil, 2002,27 (5): 83-86) the solvent method extraction process of SDG is optimized.The present inventor is on the basis of organic solvent extraction, basic hydrolysis, also adopt the modified gel post to separate to extracting product, obtain highly purified open loop secoisolariciresinoldiglucoside diglucoside (Xu Shiying, Wang Zhang, Zhang Wenbin, Zhang Xiaoming, the clock virtue. a kind of method .CN200610038634 that from linseed oil, extracts purifying secoisolariciresinoldiglucoside diglucoside).
Above-mentioned research all adopts organic solvent (lower alcohol or acetone) to extract the method for SDG.Although it is low to stir the extraction method cost, consuming time longer, solvent load is bigger, and extraction efficiency is low.Therefore, the investigator is constantly attempting some emerging technologies and is extracting SDG.(Cacace J E and MazzaG.Pressurized low polarity water extraction of lignans from whole flaxseed.Journal of Food Engineering such as Cacace, 2006,77:1087-1095) attempt adopting subcritical water from the degreasing linseed meal, to extract SDG, this accelerated solvent extracting method has been avoided the use of organic solvent, yield is also satisfactory, but the equipment input and the operational condition of this method are had relatively high expectations, and still are not suitable for industrial applications.The present inventor once adopted microwave-assisted to extract secoisolariciresinol diglycoside (Zhang Wenbin, Xu Shiying. Microwave-assisted Extraction of Flaxseed Lignan research. research and development of natural products .2006,18:286-290), obtained and be better than the conventional result who extracts, but solvent consumption is bigger, and extraction efficiency still remains to be improved.Carry out subsequently studies show that with material with extract solvent to thick attitude, carry out then that ultrasonic-microwave is collaborative to be extracted, can obtain even more ideal result.
In addition, consider the distribution of each component in the linseed oil and the characteristics of linseed oil structure, the contriver proposes a kind of comprehensive utilization linseed oil, the operational path of flax seed husk particularly, that is: adopt suitable technology that flaxseed gum, linseed oil, linseed oil albumen and flax seed husk are partly separated or enrichment, recycled (comprehensive development and utilization of flax seed husk, No. the 082nd, mirror word [religion SW2008]) then respectively.After linseed oil wet method unsticking, obtain the linseed mucilage thing, can produce flaxseed gum.Linseed oil after the unsticking can adopt wet separation benevolence shell, and the rich benevolence of gained partly can be used as the raw material of extracting linseed oil by water-enzyme process, and rich shell partly can be used as the raw material that extracts secoisolariciresinol diglycoside.The processing method of this comprehensive utilization linseed oil has been taken into account three kinds of main bioactive ingredients of linseed oil, and comprehensive utilization has important references value to linseed oil.
[summary of the invention]
[technical problem that will solve]
It is a kind of by the method for extracting secoisolariciresinol diglycoside in linseed oil or the shell that purpose of the present invention provides.
Another object of the present invention provides a kind of extract that contains secoisolariciresinol diglycoside.
Another object of the present invention provides the described purposes that contains the secoisolariciresinol diglycoside extract.
[technical scheme]
The purpose of this invention is to provide the collaborative method of extracting secoisolariciresinol diglycoside of a kind of ultrasonic-microwave, for the comprehensive development and utilization of linseed oil resource provides effective way.The present invention partly is a raw material with the rich shell of degummed flax seeds or degummed flax seeds, under ultrasonic-microwave synergistic extraction condition, adopt ethanolic soln that the lignan class material rapid extraction in the flax seed husk is come out, after concentrated and spraying drying, obtain the powder-product (seeing accompanying drawing 1) of high lignan content.Lignan extraction yield height of the present invention, process economy is good, and product can be widely used in baked goods, drink and snackfoods etc., and market potential is very big.
The present invention is achieved through the following technical solutions.
The present invention relates to a kind of by the method for extracting secoisolariciresinol diglycoside in linseed oil or the shell.This method comprises the steps:
(1) degummed flax seeds with the screening of 60 mesh sieves, obtains the degummed flax seeds powder after crushed.
In the present invention, described degummed flax seeds should be appreciated that it is to adopt common wet method method for degumming, and linseed oil (g/mL) condition under soaks 60min at 70 ℃ of temperature, pH 6.0, material-water ratio at 1: 7, repeats repeatedly to come unstuck, and the colloid that the linseed oil top layer exists is sloughed.Generally speaking, the residual glue content of described degummed flax seeds should be controlled at 1～2% (accounting for the linseed oil total mass), helps the development and use of next step benevolence shell separation and rich benevolence part and rich shell part like this.
The disintegrating apparatus that uses in this step is the various medicinal herb grinders of mass selling in the market, for example Wenling, Zhejiang machine works with trade(brand)name " herbal medicine pulverizing machine " product sold, Changxing, Zhengzhou machine works with trade(brand)name " ultra-fine micropowder machine " product sold, Shengzhou city new millennium disintegrating apparatus company limited with trade(brand)name " ultra micro aquatic feeds pulverizer " product sold or Fujian Fengli Machinery Technology Ltd. with trade(brand)name " heat-sensitive material supper micron mill " product sold.
(2) the degummed flax seeds powder that obtains of step (1) mixes with normal hexane with the ratio of 10-20 weight part according to 1 weight part, in the normal temperature encloses container, under agitation carry out degreasing 1-3h then with normal hexane, carry out centrifugation again, the residue that obtains washs with normal hexane, carry out centrifugation again, its residue is a degreasing degummed flax seeds powder, under reduced pressure handles then and removes residual normal hexane.
In the present invention, described encloses container is the stainless steel reaction pot.For example Wuxi City Xishan avenge unrestrained chemical industry equipment factory with trade(brand)name " stainless steel reaction pot " product sold, Wuxi City clear spring chemical industry equipment factory with trade(brand)name " stainless steel reaction pot " product sold, Wuxi City political circle petrochemical equipment company limited with trade(brand)name " electric heating reacting kettle " product sold or company of Shanghai Farfly Energy Technology Co., Ltd with trade(brand)name " stirred autoclave " product sold.
Described centrifugation is used present at the whizzer of the rotating speed of selling on the market more than 2500r/m, and for example Hunan instrument whizzer instrument company limited, Jintan City, Jiangsu Province Medical Instruments factory, day U.S. Science and Technology Ltd. and Anting Scientific Instrument Factory, Shanghai are with trade(brand)name " table model high speed centrifuge " product sold.
Usually, the residual fat content of described degreasing degummed flax seeds powder should be controlled at 1～2%, helps the development and use of next step benevolence shell separation and rich benevolence part and rich shell part like this.
Described under reduced pressure the processing means this a kind of like this processing that is removed by volatilization of normal hexane under pressure 1～5kPa.
(3) be the aqueous ethanolic solution that the ratio of 4-8 weight part adds 30-60% (v/v) concentration according to every weight part in the degreasing degummed flax seeds powder that obtains toward step (2), mix; At total ultrasonic power 50-300W/g, total microwave input power is 150-600W/g, carries out the collaborative extraction of ultrasonic-microwave under the condition of microwave power 50-1000W/s.
In the present invention, described ultrasonic wave microwave cooperating is handled and is used at present at the ultrasonic-microwave synergistic extraction equipment of the power of selling on the market more than 90W, for example Shanghai Xintuo Microwave Instruments Co., Ltd. with trade(brand)name " ultrasonic-microwave synergistic extraction/the reaction instrument " product sold, French PR OLABO company with trade(brand)name " MAXIDIGEST MX 350 " product sold and U.S. Hach company with trade(brand)name " Digesdahl counteract appearance " product sold.
In the present invention, the collaborative extraction of described ultrasonic-microwave should be appreciated that it is to adopt ultrasonic simultaneously and microwave action extracts target substance from raw material.
(4) the collaborative extract of the ultrasonic-microwave of step (3) carries out centrifugally, reclaims supernatant liquor, adds aqueous ethanolic solution in the centrifugal residue to wash, and carries out centrifugally again, and the merging supernatant liquor obtains being rich in the clear liquid of secoisolariciresinol diglycoside.
The centrifugation apparatus that this step is used is identical with foregoing centrifugation apparatus.
(5) the secoisolariciresinol diglycoside clear liquid that is rich in that step (4) obtains carries out concentrating under reduced pressure, reclaims ethanol for recycling.
In the present invention, described concentrating under reduced pressure means to remove under pressure 1～5kPa and is rich in concentrated that secoisolariciresinol diglycoside clear liquid solvent is carried out.
Described concentrating under reduced pressure equipment is the equipment of selling on market at present, for example Hang Zhouhui close mechanical means company limited with the sharp grand light industry and machinery in trade(brand)name " vacuum decompressioning and concentrating tank " product sold, Jiangyin golden hair drying plant company limited, Jiangyin City Su Xin drying plant company limited or Wenzhou City company limited with trade(brand)name " spherical vacuum concentration pot " product sold.
(6) the concentrating under reduced pressure residue that obtains of step (5) carries out spraying drying and obtains a kind of secoisolariciresinol diglycoside extract that contains.
A preferred embodiment of the invention can use degummed flax seeds to gall broken resulting rich shell extracting section secoisolariciresinol diglycoside through emery wheel.The step of using described rich shell extracting section secoisolariciresinol diglycoside is identical with the step that use degummed flax seeds noted earlier is extracted secoisolariciresinol diglycoside.
According to another kind of preferred implementation of the present invention, in step (2), the residue that obtains is that 5-20 weight part normal hexane washs with normal hexane according to every weight part residue.
According to another kind of preferred implementation of the present invention, described centrifugation is to carry out centrifugal 15-25min under rotating speed 2500-3500r/m.
Preferably, described centrifugation is to carry out centrifugal 20min under rotating speed 3000r/m.
According to another kind of preferred implementation of the present invention, step (3) is carried out the collaborative extraction of ultrasonic-microwave 10-30 minute.Preferably, step (3) is carried out the collaborative extraction of ultrasonic-microwave 20 minutes.
According to another kind of preferred implementation of the present invention, in step (4), add described residue weight 3-6 30%-60% (v/v) ethanolic soln doubly and wash.
According to another kind of preferred implementation of the present invention, described concentrating under reduced pressure residue inlet temperature 160-180 ℃ with air outlet temperature 80-90 ℃ condition under carry out spraying drying or use temperature 80-90 ℃ hot blast carries out drying.
Adopt the method for the invention can obtain containing the secoisolariciresinol diglycoside extract, its secoisolariciresinol diglycoside content is (to see accompanying drawing 2) in described extract gross weight more than 10%.
Secoisolariciresinol diglycoside content adopts HPLC to measure, and for example uses the Waters2690 liquid chromatograph, selects Symmetry C8 (150mm * 2.1mmi.d., 5 μ m) reverse-phase chromatographic column, the sweep limit of PAD is set in 200～400nm, 30 ℃ of column temperatures, sampling volume 10 μ L.Moving phase is by two kinds of solution compositions: (A) 1% acetum (v/v), (B) methyl alcohol.The employing linear gradient elution (A: B, v/v), 0 min, 5: 95; 40min, 55: 45; 60min, 5: 95.Flow velocity 0.5mL/min.Positive ion and negative ion mode are adopted in mass spectroscopy simultaneously, and operating parameter is:
Ionic means EIS
-EIS
+Unit
Capillary voltage 3.88 3.87 kV
120 120 ℃ of ion source temperatures
300 300 ℃ of desolventizing temperature degree
Mass range 300-800 300-800 m/z
Photomultiplier cell voltage 650 650 V
The pressure 2.6e-3 2.6e-3 Pa of analyzer room
Carrier gas speed 4.2 4.2 L/h
The invention still further relates to the described purposes of secoisolariciresinol diglycoside extract in baked goods, drink and snackfoods batching that contain.
[beneficial effect]
The present invention extracts secoisolariciresinol diglycoside with the ultrasonic-microwave synergizing method, and its beneficial effect is as follows:
(1) adopt the collaborative secoisolariciresinol diglycoside that extracts of ultrasonic-microwave, the yield height is compared raising more than 1 0% than existing microwave extract method, and the time is short, and along with the exploitation of industrially scalable equipment, industrial applications prospect of the present invention is bright and clear;
(2) adopt lower solvent/material ratio, the target product extraction yield is high and save solvent, kills two birds with one stone;
(3) adopting the rich shell of degummed flax seeds or degummed flax seeds rich shell part, particularly degummed flax seeds is raw material partly, has taken into account the utilization of other components in the linseed oil, realizes the linseed oil high-efficiency comprehensive utilization, helps increasing economic efficiency and protecting environment.
(4) extraction that can be other food function factors of the method that proposes of the present invention provides useful reference.
[description of drawings]
Fig. 1, the collaborative secoisolariciresinol diglycoside process flow sheet that extracts of ultrasonic-microwave
Fig. 2, contain the HPLC analysis of spectra of secoisolariciresinol diglycoside extract
[embodiment]
Embodiment 1
Adopt the wet method method for degumming, under the condition of 70 ℃ of temperature, pH 6.0, material-water ratio 1: 7 (g/mL), soak 60min, repeat to come unstuck 4 times, obtain degummed flax seeds.After 60 ℃ of warm air dryings, the pulverizer that adopts Wenling, Zhejiang machine works to sell with trade(brand)name " herbal medicine pulverizing machine " is pulverized, and sieves with 60 mesh sieves.Take by weighing 500g degummed flax seeds powder, add normal hexane 6000mL, normal temperature snows and stir 2h in the encloses container that Wuxi City Xishan wave chemical industry equipment factory sells with trade(brand)name " stainless steel reaction pot ", the whizzer that uses Anting Scientific Instrument Factory, Shanghai to sell with trade(brand)name " table model high speed centrifuge " carries out centrifugation 20min with 3000r/m, the residue that obtains washs with the 5000mL normal hexane again, carry out centrifugation 20min with 3000r/m again, reclaim residue, the degreasing degummed flax seeds powder that obtains is at 70 ℃ of following ventilation 1h of temperature, normal hexane is wherein removed in volatilization, and degreasing this moment degummed flax seeds powder quality is 300g.The aqueous ethanolic solution that adds 1200mL 40% (v/v) concentration in the degreasing degummed flax seeds powder, mixing.In the device that Shanghai Xintuo Microwave Instruments Co., Ltd. sells with trade(brand)name " ultrasonic-microwave synergistic extraction/the reaction instrument ", 15min acts synergistically under the condition of ultrasonic power 300W, microwave power 1000W.And then carry out centrifugation 20min with 3000r/m, and reclaim supernatant liquor, in residue, add 1200mL 40% (v/v) aqueous ethanolic solution, the washing residue carries out centrifugation 20min with 3000r/m again, merges supernatant liquor, obtains being rich in the clear liquid of secoisolariciresinol diglycoside.This merging clear liquid carries out concentrating under reduced pressure under pressure 2kPa, reclaim ethanol for recycling.The spray-dryer that residue uses no cylinder continent spray-drier factory to sell with trade(brand)name " Highspeedcentrifugingandsprayingdrier ", under the condition of 160 ℃ of air intakes, 90 ℃ of air-out, carry out spraying drying, obtain 32g secoisolariciresinol diglycoside extract, adopt the HPLC analytical method, the SDG content of measuring the secoisolariciresinol diglycoside extract in specification sheets under the condition that illustrates is 10.8%.
Embodiment 2
Adopt the wet method unsticking, 70 ℃ of temperature, pH 6.0, material-water ratio 1: 7 (g/mL), soak 60min, unsticking number of times 4 times at every turn, obtain degummed flax seeds.After galling broken and the classification of waterpower whirlpool, emery wheel obtains rich shell part.Reclaim rich shell part 60 ℃ of following warm air dryings, adopt Fujian Fengli Machinery Technology Ltd. to pulverize then, cross 60 mesh sieves with the pulverizer of trade(brand)name " heat-sensitive material supper micron mill ".Take by weighing 100g degummed flax seeds shell powder, add normal hexane 1000mL, normal temperature snows and stir 3h in the encloses container that Wuxi City Xishan wave chemical industry equipment factory sells with trade(brand)name " stainless steel reaction pot ", adopt Hunan instrument whizzer instrument company limited with centrifugal (3000r/m in the whizzer of trade(brand)name " table model high speed centrifuge " sale, 20min) separate, again with 500mL normal hexane washing residue, centrifugal (3000r/m, 20min), reclaim residue, obtain degreasing degummed flax seeds powder, 70 ℃ of following ventilation 1h, normal hexane is wherein removed in volatilization, and this moment, powder quality was 75g.The ethanolic soln 600mL that in degreasing degummed flax seeds powder, adds 40% (v/v) concentration, mixing.At ultrasonic power 90W, microwave power is under the condition of 200W, adopts in the device of Shanghai Xintuo Microwave Instruments Co., Ltd. with trade(brand)name " ultrasonic-microwave synergistic extraction/the reaction instrument " sale and acts on 500s.Centrifugal (3000r/m 20min), reclaims supernatant liquor, adds 500mL 40% (v/v) ethanolic soln in residue, the washing residue, and (3000r/m 20min), merges supernatant liquor to recentrifuge, obtains being rich in the clear liquid of secoisolariciresinol diglycoside.Concentrating under reduced pressure in the device that Jiangyin City Su Xin drying plant company limited sells with trade(brand)name " spherical vacuum concentration pot " reclaims ethanol for recycling.80 ℃ of warm air dryings obtain flax seed husk powder 10.5g, adopt HPLC to analyze, and determine wherein to contain open loop secoisolariciresinoldiglucoside diglucoside 15.6%.
Claims (9)
1, a kind of by the method for extracting secoisolariciresinol diglycoside in linseed oil or the shell, it is characterized in that this method comprises the steps:
(1) degummed flax seeds with the screening of 60 mesh sieves, obtains the degummed flax seeds powder after crushed;
(2) the degummed flax seeds powder that obtains of step (1) mixes with normal hexane with the ratio of 10-20 weight part according to 1 weight part, in the normal temperature encloses container, under agitation carry out degreasing 1-3h then with normal hexane, carry out centrifugation again, the residue that obtains washs with normal hexane, carry out centrifugation again, its residue is a degreasing degummed flax seeds powder, under reduced pressure handles then and removes residual normal hexane;
(3) be the aqueous ethanolic solution that the ratio of 4-8 weight part adds 30-60% (v/v) concentration according to every weight part in the degreasing degummed flax seeds powder that obtains toward step (2), mix; At total ultrasonic power 50-300W/g, total microwave input power is 150-600W/g, carries out the collaborative extraction of ultrasonic-microwave under the condition of microwave power 50-1000W/s;
(4) the collaborative extract of the ultrasonic-microwave of step (3) carries out centrifugally, reclaims supernatant liquor, adds aqueous ethanolic solution in the centrifugal residue to wash, and carries out centrifugally again, and the merging supernatant liquor obtains being rich in the clear liquid of secoisolariciresinol diglycoside;
(5) the secoisolariciresinol diglycoside clear liquid that is rich in that step (4) obtains carries out concentrating under reduced pressure, reclaims ethanol for recycling;
(6) the concentrating under reduced pressure residue that obtains of step (5) carries out spraying drying and obtains a kind of secoisolariciresinol diglycoside extract that contains.
2, method according to claim 1 is characterized in that using degummed flax seeds to gall broken resulting rich shell extracting section secoisolariciresinol diglycoside through emery wheel.
3, method according to claim 1 is characterized in that in step (2), and the residue that obtains is that 5-20 weight part normal hexane washs with normal hexane according to every weight part residue.
4, method according to claim 1 is characterized in that described centrifugation is to carry out centrifugal 15-25min under rotating speed 2500-3500r/m.
5, method according to claim 1 is characterized in that step (3) carries out that ultrasonic-microwave is collaborative to be extracted 10-30 minute.
6, method according to claim 1 is characterized in that in step (4), adds described residue weight 3-6 30%-60% (v/v) ethanolic soln doubly and washs.
7, method according to claim 1, it is characterized in that described concentrating under reduced pressure residue inlet temperature 160-180 ℃ with air outlet temperature 80-90 ℃ condition under carry out spraying drying or use temperature 80-90 ℃ hot blast carries out drying.
8, contain the secoisolariciresinol diglycoside extract according to what the described method of arbitrary claim among the claim 1-7 obtained, the secoisolariciresinol diglycoside content that it is characterized in that it is in described extract gross weight more than 10%.
9, the purposes of secoisolariciresinol diglycoside extract in baked goods, drink and snackfoods batching that contain according to claim 8.
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2009
- 2009-05-26 CN CN2009101434401A patent/CN101570556B/en not_active Expired - Fee Related
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