CN102206538B - Method for extracting grease and flavone from soy sauce residues - Google Patents
Method for extracting grease and flavone from soy sauce residues Download PDFInfo
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- CN102206538B CN102206538B CN 201110107005 CN201110107005A CN102206538B CN 102206538 B CN102206538 B CN 102206538B CN 201110107005 CN201110107005 CN 201110107005 CN 201110107005 A CN201110107005 A CN 201110107005A CN 102206538 B CN102206538 B CN 102206538B
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Abstract
The invention discloses a method for extracting grease and flavone from soy sauce residues, aims to provide a grease and flavone extracting method which is simple, low in cost, short in purification time and high in grease and flavone extraction ratios, and belongs to the technical field of extraction. In the technical key point, the method sequentially comprises the following steps of: 1) drying the soy sauce residues and grinding; 2) adding a solvent into the soy sauce residues obtained in the step 1), and performing ultrasonic extraction at a time; 3) performing centrifugal separation on substances obtained after the ultrasonic extraction in the step 2), and collecting the soy sauce residues and solution respectively; 4) recycling a solvent in the solution obtained in the step 3), and drying by distillation to obtain the grease; 5) drying the soy sauce residues obtained in the step 3), adding the solvent, and performing the ultrasonic extraction at a time; 6) filtering the substances obtained after the ultrasonic extraction in the step 5), and collecting the obtained filtrate and filter residues respectively; and 7) recycling the solvent in the filtrate obtained in the step 6), and drying by distillation to obtain the flavone.
Description
Technical field
The present invention discloses a kind of grease extraction process, specifically, is the method for extracting grease and flavones from soy sauce residues, belongs to the extractive technique field.
Background technology
In China, about 5,000,000 tons of soy sauce output, as produce soy sauce byproduct---the output of soy sauce residues is also large, be about 1,500,000 tons, and its market scale every year is with 10% speed increase.The main nutrient composition of soy sauce residues (butt) is as follows: moisture content 12%, crude protein 21.40%, fat 18.10%, robust fibre 23.90%, nitrogen-free extract 9.10%, mineral substance 15.50%, huge crude protein, fat, robust fibre, nitrogen-free extract, mineral substance like this, if deal with improperly, not only cause the huge wasting of resources, and also cause certain pollution for environment.
At present, development and use research is mainly reflected in the following aspects to soy sauce residues: 1, exploitation is directly used in peasant's fertilizer that tills the land as the organic fertilizer soy sauce residues, can make the soil salinization, has a strong impact on again water quality.China legendary god of farming group Beijing bio tech ltd has been developed a kind of bio-organic fertilizer live bacteria agent, and it is to utilize soy sauce residues and urban and rural domestic refuse through 1-2 week fermentation, is converted into the green non-pollution ecological organic fertilizer; 2, extract foodstuff fibre, food fibre is extensively admitted to the physiological action of human body, be called as " the 7th nutrient substance ", have preventing constipation and the rectum cancer, reduction serum cholesterol, regulate the blood pressure and blood lipoid metabolism, prevention gallbladdergallstonecholetithiasis, fat-reducing and the effect such as anticancer; 3, soy sauce residues recycling fermented sauce, because soy sauce residues is nutritious, its protein content surpasses 10%, suitably adds auxiliary material, by multiple bacteria compound fermentation, generation is a large amount of to the favourable material that makes soy sauce, and generates multiple flavour substances; 4, producing the bright agent of hiding, residue of soya and acid-sludge are combined produce tasty agents, is the another new way of development and use soy sauce residues; 5, be developed as biological flocculant, the characteristics such as efficient, nontoxic and non-secondary pollution receive much concern biological flocculant in recent years because of it, but have limited its suitability for industrialized production and application because preparation cost is too high; 6, extract the antioxidant such as isoflavones, flavonoid compound is that occurring in nature exists one of other aldehydes matter of maximum kind, and flavones is because its water-fast characteristics just become the aglucon type in brewing process, and major part remain in still in the soy sauce residues; 7, the squeezing get oil take soybean as the soy sauce residues of raw material gained in lipid content higher.
Because the raw material of sauce fermentation is soybean, can change into glycerine and lipid acid after soybean oil is processed by fermentation, sneaks in the soy sauce and glycerine is water-soluble, lipid acid is retained in the soy sauce residues because of water insoluble, so croude fatty acids content is high in the soy sauce residues.The content of grease reaches gross weight more than 1/3 in the dried soy sauce residues, and than high nearly 1 times of fat content in the soybean, the height of fat content if do not carry out first degreasing, can affect the extraction of the components such as food fibre, flavones.Therefore, before other compositions of soy sauce residues were studied, the especially extraction of food fibre and flavones will be carried out first skimming treatment, prepared for further developing the soy sauce residues resource.
Chinese patent CN 1539937A, for the extracting bean oil from soy sauce residues provides a kind of method, but there is complex manufacturing technology in the patent No. 031143490, and needs to adopt high pressure, brings certain trouble to production like this; Chinese patent CN101385532A, application number 200710121815.5 provide a kind of method of utilizing biphasic solvent catalysis soy sauce residues, but the required time is long, are about 2 to 6 hours, like this inefficiency, and follow-up solvent treatment trouble.
Summary of the invention
For the problems referred to above, the present invention discloses a kind of method of extracting fast grease and flavones from soy sauce residues.
Purpose of the present invention provides a kind of method from soy sauce residues extraction grease and flavones, in turn includes the following steps:
Above-mentioned a kind of method from soy sauce residues extraction grease and flavones, the described dry soy sauce residues of step 1) are that soy sauce residues is placed 50 ℃～70 ℃ bakings of baking oven, 10～14h.
Above-mentioned a kind ofly extracting the method for grease and flavones, step 2 from soy sauce residues) to add quality be 5 to 15 times of dried soy sauce residues quality to described solvent.
Above-mentioned a kind ofly extracting the method for grease and flavones, step 2 from soy sauce residues) described solvent is one of them of sherwood oil, acetone, Virahol; Preferred Virahol.
Above-mentioned a kind ofly extract the method for grease and flavones, step 2 from soy sauce residues) during described ultrasonic extraction, extracting temperature is 45 ℃～60 ℃, ultrasonic treatment time is 10min～40min.
Above-mentioned a kind of method from soy sauce residues extraction grease and flavones, the described solvent adding of step 5) quality are 10 to 40 times of dried soy sauce residues quality.
Above-mentioned a kind of method from soy sauce residues extraction grease and flavones, the described solvent of step 5) is concentration 40%～80% ethanol.
Above-mentioned a kind of method from soy sauce residues extraction grease and flavones, during the described ultrasonic extraction of step 5), extracting temperature is 30 ℃～70 ℃, ultrasonic treatment time is 5min～30min.
Compared with prior art, method provided by the present invention is simple, and at the bottom of the cost, the purification time is short, grease and flavones extraction yield are high, Effective Raise working efficiency, use solvent species few, but need not to separate just direct circulation utilization, be conducive to environment protection.
With reference to GB/T5009.37-2003, the extraction yield of the method disclosed in the present grease is higher than 30%(in the soy sauce residues butt), the color of the grease that gets is darker; Be about 2900～3750meq/kg with peroxide value, the grease of recovery is more applicable for the production of Chemicals such as biofuel or extraction lipid acid; The extracted amount of the flavones of gained is higher than 2.4mg/g.
Embodiment
Embodiment 1
A kind of method of extracting grease and flavones from soy sauce residues, in turn include the following steps: the soy sauce residues that will wet first is ground into fine powder after putting into 50 ℃ oven for drying 14 h, the Virahol that soy sauce residues quality after adding is dried again is 13 times, then adopt ultrasonic extraction once, extracting temperature is 50 ℃, and ultrasonic treatment time is 30min; Collect respectively liquid and the degreasing soy sauce residues that obtains after the centrifugation, solvent is reclaimed in first evaporation again, and a small amount of solvent of residue in the water bath method liquid namely gets grease again.With the degreasing soy sauce residues oven dry of gained, then add 50% ethanol of 20 times of degreasing soy sauce residues in the degreasing soy sauce residues again, adopt ultrasonic extraction once, extracting temperature is 60 ℃, and ultrasonic treatment time is 15min; After normal pressure filters, collect respectively filtrate and the filter residue that obtains, the solvent in the filtrate is steamed in water-bath, namely gets flavones.
The degreasing soy sauce residues cooling of gained is dried by the fire 0.5h again to constant weight, weighs, and the grease extraction yield that calculates gained is that 35%(is in the soy sauce residues butt), the color of grease is darker; With reference to GB/T5009.37-2003, grease obtained acid value is 323.96mg/g, and peroxide value is 3104.35 meq/kg.
With rutin as standard substance, adopt aluminum nitrate determination of color flavones content, flavones content is expressed as in the extract of every gram soy sauce residues powder dry weight the quite amount (mg/g) of rutin, general flavone content (mg) in soy sauce residues flavones extraction yield (mg/g)=extracting solution/used soy sauce ground-slag amount (g), the extracted amount of the flavones of gained is about 2.4710mg/g.
Embodiment 2
A kind of method of extracting grease and flavones from soy sauce residues, in turn include the following steps: the soy sauce residues that will wet is first pulverized after putting into 70 ℃ oven for drying 10 h, the Virahol that soy sauce residues quality after adding is dried again is 15 times, then adopt ultrasonic extraction once, extracting temperature is 60 ℃, and ultrasonic treatment time is 10min; Collect respectively liquid and the solid that obtains after the centrifugation, solvent is reclaimed in first evaporation, and a small amount of solvent of residue in the water bath method liquid namely gets grease again.The solid of gained is being dried to get the degreasing soy sauce residues, adding 40% ethanol of 40 times of degreasing soy sauce residues in the degreasing soy sauce residues again, adopting ultrasonic extraction once, extracting temperature is 70 ℃, and ultrasonic treatment time is 5min; After normal pressure filters, collect respectively filtrate and the filter residue that obtains, the solvent in the water bath method filtrate namely gets flavones.
The degreasing soy sauce residues cooling of gained is dried by the fire 0.5h again to constant weight, weighs, and the grease extraction yield that calculates gained is that 31.25%(is in the soy sauce residues butt), the color of grease is darker; With reference to GB/T5009.37-2003, grease obtained acid value is 330.69mg/g, and peroxide value is 3397.56 meq/kg.
With rutin as standard substance, adopt aluminum nitrate determination of color flavones content, flavones content is expressed as the amount (mg/g) of the suitable rutin of flavones in the extract of every gram soy sauce residues powder dry weight, general flavone content (mg) in soy sauce residues flavones extraction yield (mg/g)=extracting solution/used soy sauce ground-slag amount (g), the flavones extracted amount of gained is about 2.4710mg/g.
Embodiment 3
A kind of method of extracting grease and flavones from soy sauce residues, in turn include the following steps: the soy sauce residues that will wet is first pulverized after putting into 60 ℃ oven for drying, and oven dry approximately needs 12 h, adds acetone again, wherein, the adding quality of acetone is 5 times of the soy sauce residues quality after drying; Then adopt ultrasonic extraction once, extracting temperature is 45 ℃, and ultrasonic treatment time is 40min; Collect respectively liquid and the solid that obtains after the centrifugation, solvent is reclaimed in first evaporation, uses a small amount of solvent of residue in the water bath method liquid again, namely gets grease; The solid of gained at 109 ℃ of oven dry 2h, is namely got the degreasing soy sauce residues, add 50% ethanol of 20 times of degreasing soy sauce residues quality in the degreasing soy sauce residues, adopt ultrasonic extraction once, extracting temperature is 50 ℃, and ultrasonic treatment time is 10min; After normal pressure filters, collect respectively filtrate and the filter residue that obtains, the solvent in the water bath method filtrate namely gets flavones.
The cooling of degreasing soy sauce residues is dried by the fire 0.5h again to constant weight, weighs, and calculating the grease extraction yield is that 30.15%(is in the soy sauce residues butt), the color of grease is darker; With reference to GB/T5009.37-2003, grease obtained acid value is 367.07mg/g, and peroxide value is 3726.46meq/kg.
With rutin as standard substance, adopt aluminum nitrate determination of color flavones content, flavones content is expressed as the amount (mg/g) of every gram soy sauce residues powder dry weight rutin suitable with the extract dry weight, general flavone content (mg) in soy sauce residues flavones extraction yield (mg/g)=extracting solution/used soy sauce ground-slag amount (g), the flavones extracted amount of gained is about 2.4120mg/g.
Embodiment 4
A kind of method of extracting grease and flavones from soy sauce residues, in turn include the following steps: the soy sauce residues that will wet is first put into 60 ℃ oven for drying 12 h pulverizing, the Virahol that soy sauce residues quality after adding is dried again is 5 times, then adopt ultrasonic extraction once, extracting temperature is 40 ℃, and ultrasonic treatment time is 40min; Collect respectively liquid and the solid that obtains after the centrifugation, the solvent in the water bath method liquid namely gets grease.The solid of gained is being dried to get the degreasing soy sauce residues, adding 70% ethanol of 10 times of degreasing soy sauce residues in the degreasing soy sauce residues, adopting ultrasonic extraction once, extracting temperature is 30 ℃, and ultrasonic treatment time is 30min; After normal pressure filters again, collect respectively filtrate and the filter residue that obtains, the solvent in the water bath method filtrate namely gets flavones.
The degreasing soy sauce residues cooling of gained is dried by the fire 0.5h again to constant weight, weighs, and the grease extraction yield that calculates gained is 31.35%(soy sauce residues butt meter), the color of grease is darker; With reference to GB/T5009.37-2003, grease obtained acid value 339.69mg/g, peroxide value is 3712.46meq/kg.
With rutin as standard substance, adopt aluminum nitrate determination of color flavones content, flavones content is expressed as the amount (mg/g) of every gram soy sauce residues powder dry weight rutin suitable with the extract dry weight, general flavone content (mg) in soy sauce residues flavones extraction yield (mg/g)=extracting solution/used soy sauce ground-slag amount (g), the flavones extracted amount of gained is about 2.4120mg/g.
Claims (2)
1. the method from soy sauce residues extraction grease and flavones is characterized in that, in turn includes the following steps:
1) dry soy sauce residues and pulverizing;
2) soy sauce residues to the step 1) gained adds solvent, and ultrasonic extraction once;
3) step with centrifugal separation 2) material after the ultrasonic extraction, and collect respectively degreasing soy sauce residues and the solution that obtains;
4) evaporate to dryness and recycling step 3) solvent in the solution of gained, namely get grease;
5) baking step 3) the degreasing soy sauce residues of gained, add again solvent and adopt ultrasonic extraction once;
6) filtration step 5) material after the ultrasonic extraction, and collect respectively filtrate and the filter residue that obtains;
7) evaporate to dryness and recycling step 6) solvent in the filtrate of gained, namely get flavones;
Wherein, the described dry soy sauce residues of step 1) is that soy sauce residues is placed 50 ℃～70 ℃ bakings of baking oven, 10～14h;
Step 2) to add quality be 5 to 15 times of dried soy sauce residues quality for described solvent;
Step 2) described solvent is one of them of sherwood oil, acetone, Virahol;
Step 2) during described ultrasonic extraction, extracting temperature is 45 ℃～60 ℃, and extraction time is 10min～40min;
The described solvent adding of step 5) quality is 10 to 40 times of dried degreasing soy sauce residues quality;
The described solvent of step 5) is concentration 40%～80% ethanol;
During the described ultrasonic extraction of step 5), extracting temperature is 30 ℃～70 ℃, and extraction time is 5min～30min.
2. a kind of method from soy sauce residues extraction grease and flavones according to claim 1 is characterized in that described solvent is Virahol.
1. the method from soy sauce residues extraction grease and flavones is characterized in that, in turn includes the following steps:
1) dry soy sauce residues and pulverizing;
2) soy sauce residues to the step 1) gained adds solvent, and ultrasonic extraction once;
3) step with centrifugal separation 2) material after the ultrasonic extraction, and collect respectively degreasing soy sauce residues and the solution that obtains;
4) evaporate to dryness and recycling step 3) solvent in the solution of gained, namely get grease;
5) baking step 3) the degreasing soy sauce residues of gained, add again solvent and adopt ultrasonic extraction once;
6) filtration step 5) material after the ultrasonic extraction, and collect respectively filtrate and the filter residue that obtains;
7) evaporate to dryness and recycling step 6) solvent in the filtrate of gained, namely get flavones;
Wherein, the described dry soy sauce residues of step 1) is that soy sauce residues is placed 50 ℃～70 ℃ bakings of baking oven, 10～14h;
Step 2) to add quality be 5 to 15 times of dried soy sauce residues quality for described solvent;
Step 2) described solvent is one of them of sherwood oil, acetone, Virahol;
Step 2) during described ultrasonic extraction, extracting temperature is 45 ℃～60 ℃, and extraction time is 10min～40min;
The described solvent adding of step 5) quality is 10 to 40 times of dried degreasing soy sauce residues quality;
The described solvent of step 5) is concentration 40%～80% ethanol;
During the described ultrasonic extraction of step 5), extracting temperature is 30 ℃～70 ℃, and extraction time is 5min～30min.
2. describedly according to claim 41 a kind ofly extract the method for grease and flavones from soy sauce residues, it is characterized in that described solvent is Virahol.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102965184B (en) * | 2012-12-07 | 2014-12-24 | 中国科学院过程工程研究所 | Method for simultaneously extracting oil fat and soy isoflavone from soy sauce residues |
| CN103173280B (en) * | 2013-03-06 | 2015-03-18 | 曹庸 | Continuous-phase-change soy sauce residue oil extraction method |
| CN103242155A (en) * | 2013-05-29 | 2013-08-14 | 江南大学 | Method for separating and extracting organic acids from sauce-residue anaerobic acidogenic mixed fermentation broth |
| CN105505572A (en) * | 2015-12-02 | 2016-04-20 | 仲恺农业工程学院 | Method for directly extracting crude fat from fresh sauce residue through ultrasonic intensification and application of crude fat |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1539937A (en) * | 2003-04-27 | 2004-10-27 | 张荣耀 | Oil press method form dregs of soy sauce |
| CN1871937A (en) * | 2006-01-20 | 2006-12-06 | 李锦记（新会）食品有限公司 | Method for extracting composite functional matter in soy sauce |
| CN101385532A (en) * | 2007-09-14 | 2009-03-18 | 中国科学院过程工程研究所 | Method for extracting nutritive matter from sauce residue |
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| CN101778572A (en) * | 2007-08-02 | 2010-07-14 | 荷兰联合利华有限公司 | compositions comprising polyphenol |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1539937A (en) * | 2003-04-27 | 2004-10-27 | 张荣耀 | Oil press method form dregs of soy sauce |
| CN1871937A (en) * | 2006-01-20 | 2006-12-06 | 李锦记（新会）食品有限公司 | Method for extracting composite functional matter in soy sauce |
| CN101385532A (en) * | 2007-09-14 | 2009-03-18 | 中国科学院过程工程研究所 | Method for extracting nutritive matter from sauce residue |
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