CN103223001B - 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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- CN103223001B CN103223001B CN201310149525.7A CN201310149525A CN103223001B CN 103223001 B CN103223001 B CN 103223001B CN 201310149525 A CN201310149525 A CN 201310149525A CN 103223001 B CN103223001 B CN 103223001B
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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 soy sauce residues, belong to the method for extracting soybean isoflavone from soy sauce residues.
Background technology
Soybean isoflavone is that a class is present in the trace active composition in leguminous plant, comprises 12 kinds of compositions such as genistin, genistein, daidzin and daidzein.Scientific research shows, soybean isoflavone has a lot of important physiological functions, closely related with health, except having antitumor action, also aging, cardiovascular disease, osteoporosis and climacteric syndrome is had to preventive and therapeutic action.
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 discarded soy sauce residues after brewageing fermentation, extracting soy sauce.Its moisture, salinity, fat content are high, also contain a certain amount of protein, fiber, flavone, phospholipid etc.Limited to its exploitation at present, mainly, as the batching of feedstuff or fertilizer, added value is low, to its effective ingredient as extraction separation and the higher value application of soybean isoflavone etc. be the important directions that soy sauce residues develops.
At present, the extracting method of soybean isoflavone mainly contains solvent extraction, supercritical CO
2extraction, ultrasonic assisted Extraction are followed the example of, 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 conventional solvent extraction method, and extraction ratio is high, energy consumption is low, but higher to equipment requirements.Ultrasound wave is by the cavitation producing between sample and solvent, improves mass transfer rate, have advantages of save time, low-temperature energy-saving, extraction ratio and product purity high.Microwave-assisted extraction method is mainly to utilize the temperature effects of microwave and Electromagnetic Environmental Effect to improve extraction efficiency, compared with traditional extraction process, can reach strengthening and optimize the object of heat and mass, the advantage such as have that selectivity is high, extraction efficiency is high, the operating time is short, favorable reproducibility, pollution are little.
Summary of the invention
The object of this invention is to provide a kind of method of extracting soybean isoflavone from soy sauce residues.Utilize the collaborative extraction effect of microwave and ultrasound, given full play to the advantage of two kinds of extracting method, thereby further improve the extraction ratio of soybean isoflavone in soy sauce residues.
The technical solution used in the present invention is as follows: a kind of microwave-ultrasonic synergistic extracts the method for soybean isoflavone in soy sauce residues, and concrete steps are as follows:
(1) soy sauce residues is pulverized defat: by fresh soy sauce residues, under the condition of temperature 60 C, freeze-day with constant temperature is to moisture lower than 10%; The soy sauce residues of drying, pulverize after 5min, cross 60 mesh sieves, obtain dry slag specimen product; Add 5mL petroleum ether by every gram of dry soy sauce residues, seal and remove petroleum ether after 12 hours; Remainder is put ventilation natural drying, obtains the soy sauce residue after defat.
(2) add dissolve with ethanol solution to extract the soybean isoflavone in soy sauce residues, between 0.1mol/L hydrochloric acid solution adjusting pH to 4～5; The concentration of described alcoholic solution is 60%V/V, and the quality volume of soy sauce residues and alcoholic solution is 1:35;
(3) microwave-ultrasonic synergistic extracts: solution is put in microwave-ultrasonic synergic solvent extraction instrument, and often opening under condition at ultrasound wave is 600W, sets microwave power 500W, interrupted extraction 100s; The soy sauce residues that must extract and the mixed liquor of ethanol;
(4) processing of soybean isoflavone extracting solution: by the soy sauce residues after extraction and the mixed liquor sucking filtration of ethanol, filtrate, with the centrifugal 10min of rotating speed of 4000r/min, is got supernatant; Supernatant is rotary evaporation 10min under 70 DEG C, 50r/min condition, obtains concentrated solution, and concentrated solution is put 80 DEG C of thermostatic drying chambers dries 12h, obtains soybean isoflavone crude product.
By gained soybean isoflavone crude product of the present invention, be dissolved in NaOH solution, adopt its concentration of Spectrophotometric Determination, the extraction ratio that calculates soybean isoflavone in gained soy sauce residues is 0.652%.Be 0.411% with adopting ultrasonic extraction extraction ratio, microwave extraction gained extraction ratio 0.506%, its extraction ratio of comparing significantly improves.
The invention has the beneficial effects as follows: this technique has been concentrated the advantage of microwave, ultrasound wave two kinds of extracting method, can improve the extraction ratio of soybean isoflavone in soy sauce residues; Technique is simple, cost economy, has wide popularizing application prospect.The method is quick, simple and easy to do, has overcome supercritical CO simultaneously
2the shortcoming that fluid extraction method is high to equipment requirements.
Detailed description of the invention
Raw material is provided by Hengshun Wantong Food Making Co., Ltd., Xuzhou.
Fresh soy sauce residues is placed on to 60 DEG C of Constant Temp. Ovens and is dried to moisture content lower than 10%.Soy sauce residues after oven dry is placed in portable pulverizer, pulverizes 5min, crosses 60 mesh sieves, obtains dry slag specimen product.Accurately take the dry soy sauce residues of 2g and put into 100mL beaker, add 10mL petroleum ether, seal rim of a cup with sealing compound, soak 12 hours, remove petroleum ether with liquid-transfering gun, remainder is put ventilation natural drying and is obtained the soy sauce residues after defat.
The soy sauce residues 2g accurately taking after defat puts into 100mL small beaker, adding 70mL concentration is 60% alcoholic solution, regulate with 0.1mol/L hydrochloric acid solution between pH value to 4-5 of sample, raw material is poured in 250mL extraction flask, with microwave-ultrasonic synergic solvent extraction instrument, often open (600W) under condition at ultrasound wave, microwave power is adjusted to 500W, interrupted extraction 100s.
By sample sucking filtration, filtrate, with the centrifugal 10min of rotating speed of 4000r/min, is got supernatant.Rotary evaporation 10min under 70 DEG C, 50r/min condition, obtains concentrated solution, and concentrated solution is put 80 DEG C of thermostatic drying chambers dries 12h, obtains soybean isoflavone crude product.
By gained soybean isoflavone crude product, be dissolved in NaOH solution, adopt its concentration of Spectrophotometric Determination, the extraction ratio that calculates soybean isoflavone in gained soy sauce residues is 0.652%.
Claims (1)
1. microwave-ultrasonic synergistic extracts a method for soybean isoflavone in soy sauce residues, and concrete steps are as follows:
(1) soy sauce residues pulverize defat: by fresh soy sauce residues under the condition of temperature 60 C, freeze-day with constant temperature to moisture content lower than 10%; The soy sauce residues of drying, pulverize after 5min, cross 60 mesh sieves, obtain dry slag specimen product; Add 5mL petroleum ether by every gram of dry soy sauce residues, seal and remove petroleum ether after 12 hours; Remainder is put ventilation natural drying, obtains the soy sauce residue after defat.
(2) add dissolve with ethanol solution to extract the soybean isoflavone in soy sauce residues, between 0.1mol/L hydrochloric acid solution adjusting pH to 4～5; The concentration of described alcoholic solution is 60%V/V, and the quality volume of soy sauce residues and alcoholic solution is 1:35;
(3) microwave-ultrasonic synergistic extracts: solution is put in microwave-ultrasonic synergic solvent extraction instrument, and often opening under condition at ultrasound wave is 600W, sets microwave power 500W, interrupted extraction 100s; The soy sauce residues that must extract and the mixed liquor of ethanol;
(4) processing of soybean isoflavone extracting solution: by the soy sauce residues after extraction and the mixed liquor sucking filtration of ethanol, filtrate, with the centrifugal 10min of rotating speed of 4000r/min, is got supernatant; Supernatant is rotary evaporation 10min under 70 DEG C, 50r/min condition, obtains concentrated solution, and concentrated solution is put 80 DEG C of thermostatic drying chambers dries 12h, obtains moisture content lower than 5% soybean isoflavone crude product.
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| 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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