CN103223001A - Microwave-supersonic wave cooperation method for extracting soy isoflavone in soy sauce residue - Google Patents
Microwave-supersonic wave cooperation method for extracting soy isoflavone in soy sauce residue Download PDFInfo
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- CN103223001A CN103223001A CN2013101495257A CN201310149525A CN103223001A CN 103223001 A CN103223001 A CN 103223001A CN 2013101495257 A CN2013101495257 A CN 2013101495257A CN 201310149525 A CN201310149525 A CN 201310149525A CN 103223001 A CN103223001 A CN 103223001A
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Abstract
The invention discloses a microwave-supersonic wave cooperation method for extracting soy isoflavone in soy sauce residue. The invention belongs to a soy isoflavone extraction method. According to the invention, soy sauce residue is crushed, and is subjected to petroleum ether degreasing; with a mass volume ratio of 1:35, the soy sauce residue is added into 60% ethanol; a pH value is regulated to 4-5; the mixture is placed in a microwave-supersonic wave cooperation extraction instrument. Ultrasonic wave (600W) is normally switched on, a microwave power is 500W, and intermittent extraction is carried out for 100s; the extract liquid is subjected to pump filtration and centrifugation, and a supernatant is obtained; and concentration and bake-drying are carried out, such that soy isoflavone crude product is obtained. As a result of examining, soy isoflavone extraction rate can reach 0.652%. The process is simple. Advantages of time saving, energy saving, high extraction rate, high product purity, high reproducibility, low pollution, and the like of microwave and ultrasonic wave are integrated. The method has wide popularization and application prospect.
Description
Technical field
The present invention relates to the method that microwave-ultrasonic synergistic extracts soybean isoflavone in the soy sauce slag, belong to the method for from the soy sauce slag, extracting soybean isoflavone.
Background technology
Soybean isoflavone is that a class is present in the trace active composition in the leguminous plant, comprises 12 kinds of compositions such as genistin, genistein, daidzin and daidzein.Scientific research shows that soybean isoflavone has a lot of important physical functions, and is closely related with health, except that having antitumor action, also aging, cardiovascular disease, osteoporosis and climacteric syndrome is had prevention and therapeutical effect.
The primary raw material of soy sauce brewing is Semen sojae atricolor, Semen Viciae fabae, soybean cake or bean cake, Semen Pisi sativi, wheat bran, Semen Tritici aestivi and Sal etc., produces a large amount of depleted soy sauce slags after brewageing fermentation, extracting soy sauce.Its moisture, salinity, fat content height also contain a certain amount of protein, fiber, flavone, phospholipid etc.Limited to its development and use at present, mainly as the batching of feedstuff or fertilizer, added value is low, is an important directions of soy sauce slag development and use to the extraction separation and the higher value application of its effective ingredient such as soybean isoflavone etc.
At present, the extracting method of soybean isoflavone mainly contains solvent extraction, supercritical CO
2Extraction, ultrasonic assisted extraction method, microwave-assisted extraction method.Conventional solvent extraction method time consumption and energy consumption consumes a large amount of solvents, and economy and Environmental costs are very high.Supercritical CO
2Fluid extraction is compared with the conventional solvent extraction method, and extraction ratio height, energy consumption are low, but higher to equipment requirements.The cavitation of ultrasound wave by producing between sample and solvent improves mass transfer rate, have save time, low-temperature energy-saving, extraction ratio and the high advantage of product purity.The microwave-assisted extraction method mainly is to utilize the temperature effects of microwave and Electromagnetic Environmental Effect to improve extraction efficiency, compare with traditional extraction process, can reach and strengthen and the purpose of optimizing heat and mass, have advantages such as selectivity height, extraction efficiency height, operating time weak point, favorable reproducibility, pollution are little.
Summary of the invention
The purpose of this invention is to provide a kind of method of from the soy sauce slag, extracting soybean isoflavone.Utilize microwave and hyperacoustic collaborative extraction effect, given full play to the advantage of two kinds of extracting method, thereby further improve the extraction ratio of soybean isoflavone in the soy sauce slag.
The technical solution used in the present invention is as follows: a kind of microwave-ultrasonic synergistic extracts the method for soybean isoflavone in the soy sauce slag, and concrete steps are as follows:
(1) the broken defat of soy sauce ground-slag: under the condition of 60 ℃ of temperature, freeze-day with constant temperature is lower than 10% to moisture with fresh soy sauce slag; The soy sauce slag of oven dry, behind the pulverizing 5min, cross 60 mesh sieves, must do the slag specimen product; Add the 5mL petroleum ether by the dried soy sauce slag of every gram, seal and remove petroleum ether after 12 hours; Remainder is put the ventilation natural drying, obtains the soy sauce residue after the defat.
(2) the adding dissolve with ethanol solution extracts the soybean isoflavone in the soy sauce slag, regulates between pH to 4～5 with the 0.1mol/L hydrochloric acid solution; The concentration of described alcoholic solution is 60%V/V, and the quality volume of soy sauce slag and alcoholic solution is 1:35;
(3) microwave-ultrasonic synergistic extracts: solution is put in the microwave-ultrasonic synergic solvent extraction instrument, and often opening under the condition at ultrasound wave is 600W, sets microwave power 500W, interrupted extraction 100s; Soy sauce slag that must extract and alcoholic acid mixed liquor;
(4) processing of soybean isoflavone extracting solution: soy sauce slag and alcoholic acid mixed liquor sucking filtration after will extracting, filtrate is got supernatant with the centrifugal 10min of the rotating speed of 4000r/min; Supernatant is rotary evaporation 10min under 70 ℃, 50r/min condition, concentrated solution, concentrated solution is put 80 ℃ of thermostatic drying chambers oven dry 12h, the soybean isoflavone crude product.
With gained soybean isoflavone crude product of the present invention, be dissolved in NaOH solution, adopt spectrophotography to survey its concentration, the extraction ratio that calculates soybean isoflavone in the gained soy sauce slag is 0.652%.With adopting the ultrasonic extraction extraction ratio is 0.411%, microwave extraction gained extraction ratio 0.506%, and its extraction ratio of comparing significantly improves.
The invention has the beneficial effects as follows: this technology has been concentrated the advantage of microwave, ultrasound wave two kinds of extracting method, can improve the extraction ratio of soybean isoflavone in the soy sauce slag; Technology is simple, cost economy, has broad prospect for its application.This method is quick, simple and easy to do, has overcome supercritical CO simultaneously
2The shortcoming that the fluid extraction method is high to equipment requirements.
The specific embodiment
Raw material is provided by Hengshun Wantong Food Making Co., Ltd., Xuzhou.
Fresh soy sauce slag is placed on 60 ℃ of Constant Temp. Ovens to be dried to moisture content and to be lower than 10%.Soy sauce slag after the oven dry is placed in the portable pulverizer, pulverizes 5min, crosses 60 mesh sieves, must do the slag specimen product.Accurately take by weighing the dried soy sauce slag of 2g and put into the 100mL beaker, add the 10mL petroleum ether, seal rim of a cup with sealing compound, soaked 12 hours, remove petroleum ether with liquid-transfering gun, remainder is put the soy sauce slag after the ventilation natural drying promptly gets defat.
The soy sauce slag 2g that accurately takes by weighing after the defat puts into the 100mL small beaker, adding 70mL concentration is 60% alcoholic solution, regulate with the 0.1mol/L hydrochloric acid solution between the pH value to 4-5 of sample, raw material is poured in the 250mL extraction flask, with microwave-ultrasonic synergic solvent extraction instrument, often open (600W) under the condition at ultrasound wave, microwave power is adjusted to 500W, interrupted extraction 100s.
With the sample sucking filtration, filtrate is got supernatant with the centrifugal 10min of the rotating speed of 4000r/min.Rotary evaporation 10min under 70 ℃, 50r/min condition, concentrated solution, concentrated solution is put 80 ℃ of thermostatic drying chambers oven dry 12h, the soybean isoflavone crude product.
With gained soybean isoflavone crude product, be dissolved in NaOH solution, adopt spectrophotography to survey its concentration, the extraction ratio that calculates soybean isoflavone in the gained soy sauce slag is 0.652%.
Claims (1)
1. a microwave-ultrasonic synergistic extracts the method for soybean isoflavone in the soy sauce slag, and concrete steps are as follows:
(1) the broken defat of soy sauce ground-slag: under the condition of 60 ℃ of temperature, freeze-day with constant temperature to moisture content is lower than 10% with fresh soy sauce slag; The soy sauce slag of oven dry, behind the pulverizing 5min, cross 60 mesh sieves, must do the slag specimen product; Add the 5mL petroleum ether by the dried soy sauce slag of every gram, seal and remove petroleum ether after 12 hours; Remainder is put the ventilation natural drying, obtains the soy sauce residue after the defat.
(2) the adding dissolve with ethanol solution extracts the soybean isoflavone in the soy sauce slag, regulates between pH to 4～5 with the 0.1mol/L hydrochloric acid solution; The concentration of described alcoholic solution is 60%V/V, and the quality volume of soy sauce slag and alcoholic solution is 1:35;
(3) microwave-ultrasonic synergistic extracts: solution is put in the microwave-ultrasonic synergic solvent extraction instrument, and often opening under the condition at ultrasound wave is 600W, sets microwave power 500W, interrupted extraction 100s; Soy sauce slag that must extract and alcoholic acid mixed liquor;
(4) processing of soybean isoflavone extracting solution: soy sauce slag and alcoholic acid mixed liquor sucking filtration after will extracting, filtrate is got supernatant with the centrifugal 10min of the rotating speed of 4000r/min; Supernatant is rotary evaporation 10min under 70 ℃, 50r/min condition, concentrated solution, concentrated solution is put 80 ℃ of thermostatic drying chambers oven dry 12h, moisture content be lower than 5% soybean isoflavone crude product.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103739583A (en) * | 2014-01-10 | 2014-04-23 | 广东美味鲜调味食品有限公司 | Method for extracting soy isoflavone from soybean sauce dreg by using ODS (Ozone Depleting Substance) and HSCCC (High Speed Counter Current Chromatography) |
| CN103755674A (en) * | 2014-01-10 | 2014-04-30 | 广东美味鲜调味食品有限公司 | Method for extracting soy isoflavone from soy sauce residue by using amino silica gel cooperated with high-speed counter current chromatography (HSCCC) |
| CN106053373A (en) * | 2016-08-09 | 2016-10-26 | 安徽青松食品有限公司 | Detection method of soy isoflavone in soybean milk |
| CN107261551A (en) * | 2017-08-10 | 2017-10-20 | 湖南源绿科技有限公司 | The method of the ultrasonic combined efficient leaching device of microwave and effective component extracting |
| CN111875571A (en) * | 2020-07-23 | 2020-11-03 | 长沙理工大学 | Method for extracting soybean isoflavone from soy sauce residues |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103739583A (en) * | 2014-01-10 | 2014-04-23 | 广东美味鲜调味食品有限公司 | Method for extracting soy isoflavone from soybean sauce dreg by using ODS (Ozone Depleting Substance) and HSCCC (High Speed Counter Current Chromatography) |
| CN103755674A (en) * | 2014-01-10 | 2014-04-30 | 广东美味鲜调味食品有限公司 | Method for extracting soy isoflavone from soy sauce residue by using amino silica gel cooperated with high-speed counter current chromatography (HSCCC) |
| CN103739583B (en) * | 2014-01-10 | 2016-06-08 | 广东美味鲜调味食品有限公司 | The collaborative HSCCC of a kind of ODS extracts the method for soybean isoflavone in soy sauce residues |
| CN103755674B (en) * | 2014-01-10 | 2016-06-08 | 广东美味鲜调味食品有限公司 | The collaborative HSCCC of amination silica gel extracts the method for soybean isoflavone in soy sauce residues |
| CN106053373A (en) * | 2016-08-09 | 2016-10-26 | 安徽青松食品有限公司 | Detection method of soy isoflavone in soybean milk |
| CN107261551A (en) * | 2017-08-10 | 2017-10-20 | 湖南源绿科技有限公司 | The method of the ultrasonic combined efficient leaching device of microwave and effective component extracting |
| CN111875571A (en) * | 2020-07-23 | 2020-11-03 | 长沙理工大学 | Method for extracting soybean isoflavone from soy sauce residues |
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