CN105124132A - Method for ultrasonic-assisted weak base extraction of proteins in cold-pressed sesame cake meal - Google Patents
Method for ultrasonic-assisted weak base extraction of proteins in cold-pressed sesame cake meal Download PDFInfo
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Abstract
The invention belongs to the technical field of deep processing of oil, and particularly relates to a method for ultrasonic-assisted weak base extraction of proteins in cold-pressed sesame cake meal. The method specifically comprises the following steps: recovering oil in sesame cake meal through subcritical extraction; then, crushing the sesame cake meal after oil extraction, and removing impurities; extracting sesame seed proteins through two times of ultrasonic-assisted base processes; centrifuging a protein extracting solution, taking supernatant, and acid-precipitating the proteins; performing centrifugation to obtain the precipitated proteins; and performing ultrafiltration and drying so as to obtain finished products of sesame seed proteins. Compared with a conventional alkali-solution and acid-isolation method, the method disclosed by the invention has the advantages of high quality of products, little pollution, high efficiency, and the like. Through the adoption of the method disclosed by the invention, an oil production byproduct, namely the low-temperature sesame cake meal, is produced into sesame seed proteins with a high added value, so that the comprehensive utilization of resources is realized, the economic benefits are improved, and the method disclosed by the invention is of positive socioeconomic significance.
Description
Technical field
The invention belongs to Oil processing byproduct comprehensive to utilize and vegetable protein extractive technique field, be specifically related to a kind of adopt ultrasonic assistant mild alkaline treatment cold press sesame cake meal, and sink through acid, the method for albumen in alcohol wash, UF membrane acquisition sesame cake meal.
Background technology
China is sesame production and supplyment big country, and within 2013, China's Sesame Seed Yield is 590,000 tons, because supply falls short of demand, and every year need from external import sesame about 400,000 tons.At present, the sesame of China 80% is used for oil expression, the annual sesame cake meal producing more than 500,000 tons.Sesame protein is one of main component in sesame cake meal, accounts for 50%.Sesame protein nutritive value is higher, and its essential amino acids content accounts for 30% of total amino acid total amount, and essential amino acid is except lysine and isoleucine content are lower than except FAO/WHO standard, and other amino acid all can meet human body requirements.In addition, large quantity research proves: hydrolysis sesame protein can produce anti-oxidation peptide, ace inhibitory peptide, chelated mineral peptide isoreactivity peptide.Therefore, sesame protein is with a wide range of applications at food, medicine, cosmetic field, is the protein resource with processing and utilization value.
The production technology of tradition sesame protein is that the molten acid of alkali is sunk, namely the character of sesame protein based on alkali-soluble protein is utilized, alkaline solution (more than pH10) is adopted to be extracted from grouts by sesame protein, centrifuging and taking supernatant subsequently, add acid solution and its pH is dropped to sesame protein isoelectric point, obtain sesame protein.The advantage that technique is simple although the method has, production capacity is large, uses strong acid and strong base both to reduce the quality of sesame protein in producing, too increases equipment and pollution treatment is invested.Therefore, be necessary to carry out improving to above-mentioned technique and reform.
Summary of the invention
The object of the invention is to overcome prior art defect, provides a kind of ultrasonic assistant weak base to extract the method for albumen in cold press sesame cake meal, the method has that production efficiency is high, environmental protection, product purity advantages of higher.
For achieving the above object, the present invention adopts following technical scheme:
Ultrasonic assistant weak base extracts a method for albumen in cold press sesame cake meal, and it comprises the steps:
1) the subcritical de-oiling pretreatment of cold press sesame cake meal:
After the pulverizing of cold press sesame cake meal, pack, put into subcritical abstraction tank, add liquefaction organic solvent and extract as subcritical fluids, to be extracted in grouts Residual oil lower than 1%, then the liquefaction organic solvent that decompression distillation removing is remaining, the sesame cake meal of removing liquefaction organic solvent is for subsequent use;
Wherein, cold press sesame cake meal is crushed to 20-60 orders.Sack can be Nylon Bag, cotton bag, cloth bag, and its order number is more than 200 orders; The condition of decompression distillation is specially: in-0.08--0.12MPa, 40-70 DEG C of distillation 20-100min.
2) sesame protein extracts:
A: step 1) gained sesame cake meal is crushed to 80-160 orders, add in salting liquid and be made into 5-15%(w/v) suspension and pH value is adjusted to 7.0-10.0, then proceed in circulating ultrasonic wave extraction apparatus, in 30-50 DEG C of first time ultrasonic extraction 20-50min under 200-800rpm mixing speed, ultrasonic extraction terminates, centrifugal (preferably the centrifugal 20-40min of 3000-5000rpm), gets supernatant, for subsequent use;
B: centrifugal gained precipitation in step a is added in salting liquid and is made into solid content 10-20%(w/v) suspension, and pH value is adjusted to 7.0-10.0, and then proceed in circulating ultrasonic wave extraction apparatus, the ultrasonic extraction of second time is carried out when ultrasonic extraction conditions is identical with first time, ultrasonic extraction terminates, centrifugal (preferably the centrifugal 20-40min of 3000-5000rpm), gets supernatant, for subsequent use;
C: combining step a and b gained supernatant, system pH is adjusted to 4.0-5.0 by acid adding, leaves standstill 30-60min, centrifugal (preferably the centrifugal 30-50min of 3000-5000rpm), collects sesame protein precipitation, for subsequent use;
Wherein, the alkali regulating pH used can be NaOH, potassium hydroxide etc., and acid used can be hydrochloric acid, sulfuric acid, phosphoric acid, acetic acid etc.; Acid paper mill wastewater is advisable at 1-5mol/L.
3) sesame protein purifying
Step c gained sesame protein precipitation is added water and is made into 2-6%(w/v) suspension, and pH is adjusted to 6.8-7.2, ultra-filtration and separation, ultrafiltration concentration liquid obtains sesame protein product after drying.
Concrete, in step 1), described liquefaction organic solvent is the mixture of butane, propane or butane and propane; Extraction conditions in subcritical abstraction tank is: 30-60 DEG C extract 3-5 times, and each extraction time is 20-40min, and every 1kg cold press sesame cake meal adds 2-5L liquefaction organic solvent and is advisable.
In step b and c, described salting liquid is the sodium-chloride water solution of concentration 0.2-0.8mol/L.
Step 2) a and b in, condition when ultrasonic wave extracts: the ultrasonic frequency of employing is 20KHz, 40KHz, 59KHz or 20KHz and 40KHz or 20KHz and 59KHz, or 40KHz and 59KHz, ultrasonic wave working method is impulse type, and its working time is 3-1:1 with intermittent time ratio.Ultrasonic intensity is often liter of solution effects 80-400W.
In step 3), for improving ultrafiltration effect, adopting two times of ultrafiltration, being again diluted with water to 2-6% by first time ultrafiltration gained concentrate and carrying out second ultrafiltration; In ultra-filtration process, adopt the milipore filter of molecular cut off 5000-10000Da, ultrafiltration pressure is 0.2-0.5MPa, and operating temperature is 20-40 DEG C.
In step 3), drying mode can be vacuum drying, vacuum freeze drying or spraying dry etc.; Vacuum drying operating condition is: pressure-0.08--0.10MPa, temperature 45-65 DEG C; The operating condition of vacuum freeze drying is: temperature-40--60
oc; Spray-dired operating condition is: 4-8% solid concentration, inlet temperature 160-200 DEG C, and outlet temperature is 60-80 DEG C, pressure 1.2-1.6MPa.
In step 3), after permeate and step c centrifugal gained supernatant that ultra-filtration and separation obtains merge, plate-frame filtering removes suspension, again adds salting liquid and is made into the suspension of 10-20% and adjusts pH to 7.0-10.0 and be reused for sesame protein extraction.
It is a kind of new industry extracting method that ultrasonic assistant extracts, and it utilizes hyperacoustic mechanical effect, cavitation effect and fuel factor, and by increasing the movement velocity of medium molecule, the penetration power of increase medium improves the extraction efficiency of target substance.The present invention relies on ultrasonic assistant to extract and UF membrane coupling, under the condition reducing soda acid use amount and sewage discharge, and production high-quality sesame protein.Compared with traditional alkali extraction-acid precipitation, present invention process decreases use amount and the sewage discharge of chemical reagent, shortens the production time, improves product quality.The inventive method improves the utilization rate of sesame processing byproduct grouts, while increase dietary protein origin, extends machining chain, adds value-added content of product, have positive social economic value.
Compared with heavy with the molten acid of traditional alkali, advantage and the beneficial effect of the inventive method are as follows:
1, ultrasonic assistant weak base extracts sesame protein, because extraction conditions is gentle and use chemical reagent few, while raising sesame protein quality, also reduces equipment anticorrosion and pollution treatment cost.
2, UF membrane is adopted to carry out desalination to sesame protein in the present invention, energy-efficient and pollution-free; Meanwhile, be reused for protein extraction by after the permeate of UF membrane and centrifuged supernatant process, improve the utilization rate of water resource.
3, the sesame protein sex change of the present invention's production is few, purity is high, quality better, can be applicable to the fields such as medicine, food, cosmetics.
Accompanying drawing explanation
Fig. 1 is the process chart of the inventive method;
Fig. 2 adopts the sesame protein product that obtains of the inventive method, and in figure, (a) precipitates for centrifugal acquisition sesame protein, and (b) is the sesame protein powder after vacuum freeze drying.
Detailed description of the invention
Do to introduce in detail further to technical scheme of the present invention below in conjunction with embodiment, but protection scope of the present invention is not limited thereto.
embodiment 1:
Ultrasonic assistant weak base extracts a method for albumen in cold press sesame cake meal, and it comprises the steps:
1) the subcritical de-oiling pretreatment of cold press sesame cake meal:
Get cold press sesame cake meal 10kg, be crushed to 40 orders, load after in Nylon Bag, put into subcritical abstraction tank, be that 1kg:4L adds liquefied butane and extracts as subcritical fluids according to solid-liquid ratio, be extracted in grouts Residual oil lower than 1%(40 DEG C of extractions 3 times, extract 30min at every turn).Then at-0.10MPa, decompression distillation 60min removes remaining liquefied butane at 50 DEG C, the sesame cake meal of removing liquefied butane is for subsequent use;
2) sesame protein extracts:
A: get 1kg step 1) gained sesame cake meal and be crushed to 80 orders, then the sodium-chloride water solution of 9L0.3mol/L is added, and with 1mol/L NaOH, pH is adjusted to 9.5, proceed in circulating ultrasonic wave extraction apparatus subsequently, under 400rpm mixing speed, temperature 35 DEG C of conditions, adopt mode (20KHz and 40KHz ultrasonic power is 900W, and wherein 40KHz ultrasonic wave single working time and intermittent time are 10s and 5s) the first time ultrasonic extraction 30min of 20KHz and 40KHz ultrasonic wave coupling.After ultrasonic end, the centrifugal 30min of 4000rpm, collects first time and extracts supernatant, for subsequent use.
B: take centrifugal gained precipitation quality in step a, add 0.3mol/L sodium-chloride water solution and be made into 15%(w/v) suspension, and with 1mol/L NaOH, pH is adjusted to 9.5, proceeds to subsequently in circulating ultrasonic wave extraction apparatus.Carry out the ultrasonic extraction of second time when ultrasonic extraction conditions is identical with first time, ultrasonic extraction terminates, the centrifugal 30min of 4000rpm, collects second time and extracts supernatant, for subsequent use;
C: combining step a and b gained supernatant, system pH is adjusted to 4.3 by acid adding (3mol/L hydrochloric acid), leaves standstill the centrifugal 30min of 30min, 5000rpm, collects sesame protein precipitation, for subsequent use;
3) sesame protein purifying
By step c gained sesame protein precipitation add water be made into 3%(w/v) suspension, and pH is adjusted to 7.0, at room temperature 25 DEG C, the ultra-filtration and separation milipore filter of 10000Da (be with molecular cut off carry out ultrafiltration with 0.30Mpa operating pressure), when being concentrated to concentration and being 15%, add water and be again diluted to 3%, the same terms carries out second time ultrafiltration.Second time ultrafiltration gained concentrate in 65 DEG C ,-0.10Mpa carries out vacuum drying, finally obtain 398.56g white sesame protein powder, purity of protein is 86.5%.
Ultra-filtration and separation obtain permeate can merge with the centrifugal gained supernatant of step c after, plate-frame filtering removing suspension, add 0.3mol/L sodium-chloride water solution and be made into 15%(w/v) suspension and adjust pH to 9.5 be reused for sesame protein extraction.
The assay method of purity of protein adopts Kjeldahl's method, the mensuration (GB5009.5-2010) of Protein in Food.
embodiment 2:
Ultrasonic assistant weak base extracts a method for albumen in cold press sesame cake meal, and it comprises the steps:
1) the subcritical de-oiling pretreatment of cold press sesame cake meal:
Get cold press sesame cake meal 15kg, be crushed to 40 orders, load after in Nylon Bag, put into subcritical abstraction tank, be that 1kg:3L adds liquefied propane and extracts as subcritical fluids according to solid-liquid ratio, be extracted in grouts Residual oil lower than 1%(40 DEG C of extractions 5 times, extract 30min at every turn).Then at-0.10MPa, decompression distillation 80min removes remaining liquefied propane at 60 DEG C, the sesame cake meal of removing liquefied propane is for subsequent use;
2) sesame protein extracts:
A: get 1kg step 1) gained sesame cake meal and be crushed to 120 orders, then the sodium-chloride water solution of 9L0.6mol/L is added, and with 1mol/L NaOH, pH is adjusted to 10.0, proceed in circulating ultrasonic wave extraction apparatus subsequently, under 600rpm mixing speed, temperature 30 DEG C of conditions, adopt mode (20KHz and 59KHz ultrasonic power is respectively 800 and 1200W, and wherein 59KHz ultrasonic wave single working time and intermittent time are 12s and 4s) the first time ultrasonic extraction 25min of 20KHz and 59KHz ultrasonic wave coupling.After ultrasonic end, the centrifugal 30min of 4500rpm, collects first time and extracts supernatant, for subsequent use.
B: take centrifugal gained precipitation quality in step a, add 0.6mol/L sodium-chloride water solution and be made into 15%(w/v) suspension, and with 1mol/L NaOH, pH is adjusted to 10.0, proceeds to subsequently in circulating ultrasonic wave extraction apparatus.Carry out the ultrasonic extraction of second time when ultrasonic extraction conditions is identical with first time, ultrasonic extraction terminates, the centrifugal 30min of 4500rpm, collects second time and extracts supernatant, for subsequent use;
C: combining step a and b gained supernatant, system pH is adjusted to 4.5 by acid adding (3mol/L hydrochloric acid), leaves standstill the centrifugal 30min of 60min, 5000rpm, collect sesame protein precipitation (see in Fig. 2 a), for subsequent use;
3) sesame protein purifying
By step c gained sesame protein precipitation add water be made into 2%(w/v) suspension, and pH is adjusted to 7.0, at room temperature 30 DEG C, the ultra-filtration and separation milipore filter of 8000Da (be with molecular cut off carry out ultrafiltration with 0.40Mpa operating pressure), when being concentrated to concentration and being 12%, add water and be again diluted to 2%, the same terms carries out second time ultrafiltration.Second time ultrafiltration gained concentrate carries out vacuum freeze drying in-60 DEG C, finally obtain 429.34g white sesame protein powder (see in Fig. 2 b), purity of protein is 86.8%.
embodiment 3:
Ultrasonic assistant weak base extracts a method for albumen in cold press sesame cake meal, and it comprises the steps:
1) the subcritical de-oiling pretreatment of cold press sesame cake meal:
Get cold press sesame cake meal 10kg, be crushed to 20 orders, load after in cloth bag, put into subcritical abstraction tank, be that 1kg:4L adds liquefied butane and extracts as subcritical fluids according to solid-liquid ratio, be extracted in grouts Residual oil lower than 1%(40 DEG C of extractions 5 times, extract 30min at every turn).Then at-0.10MPa, decompression distillation 90min removes remaining liquefied butane at 65 DEG C, the sesame cake meal of removing liquefied butane is for subsequent use;
2) sesame protein extracts:
A: get 0.5kg step 1) gained sesame cake meal and be crushed to 160 orders, then the sodium-chloride water solution of 9.5L0.5mol/L is added, and with 1mol/L NaOH, pH is adjusted to 9.0, proceed in circulating ultrasonic wave extraction apparatus subsequently, under 500rpm mixing speed, temperature 40 DEG C of conditions, adopt 40KHz ultrasonic wave (40KHz ultrasonic power is 1800W, and ultrasonic wave single working time and intermittent time are 10s and 10s) first time ultrasonic extraction 30min.After ultrasonic end, the centrifugal 20min of 5000rpm, collects first time and extracts supernatant, for subsequent use.
B: take centrifugal gained precipitation quality in step a, add 0.5mol/L sodium-chloride water solution and be made into 15%(w/v) suspension, and with 1mol/L NaOH, pH is adjusted to 9.0, proceeds to subsequently in circulating ultrasonic wave extraction apparatus.Carry out the ultrasonic extraction of second time when ultrasonic extraction conditions is identical with first time, ultrasonic extraction terminates, the centrifugal 20min of 5000rpm, collects second time and extracts supernatant, for subsequent use;
C: combining step a and b gained supernatant, system pH is adjusted to 4.4 by acid adding (3mol/L hydrochloric acid), and room temperature leaves standstill 60min, the centrifugal 30min of 5000rpm, collects sesame protein precipitation, for subsequent use;
3) sesame protein purifying
By step c gained sesame protein precipitation add water be made into 2%(w/v) suspension, and pH is adjusted to 7.0, at room temperature 30 DEG C, the ultra-filtration and separation milipore filter of 5000Da (be with molecular cut off carry out ultrafiltration with 0.50Mpa operating pressure), when being concentrated to concentration and being 8%, add water and be again diluted to 2%, the same terms carries out second time ultrafiltration.Second time ultrafiltration gained concentrate spray-dried (solid concentration 8%, inlet temperature 180 DEG C, outlet temperature 80 DEG C, pressure 1.6MPa), finally obtain 174.27g white sesame protein powder, purity of protein is 86.65%.
Compared with traditional alkali extraction-acid precipitation, the inventive method have product quality high, pollute little, efficiency advantages of higher.Fats and oils processing accessory substance low temperature sesame cake meal is produced the sesame protein for high added value by the inventive method, has both achieved comprehensive utilization of resources, and has also increased economic benefit, and had positive social and economic significance.
Claims (7)
1. ultrasonic assistant weak base extracts a method for albumen in cold press sesame cake meal, it is characterized in that, comprises the steps:
1) the subcritical de-oiling pretreatment of cold press sesame cake meal:
After the pulverizing of cold press sesame cake meal, pack, put into subcritical abstraction tank, add liquefaction organic solvent and extract as subcritical fluids, to be extracted in grouts Residual oil lower than 1%, then the liquefaction organic solvent that decompression distillation removing is remaining, the sesame cake meal of removing liquefaction organic solvent is for subsequent use;
2) sesame protein extracts:
A: step 1) gained sesame cake meal is crushed to 80-160 orders, add in salting liquid be made into 5-15% suspension and pH value is adjusted to 7.0-10.0, then proceed in circulating ultrasonic wave extraction apparatus, in 30-50 DEG C of first time ultrasonic extraction 20-50min under 200-800rpm mixing speed, ultrasonic extraction terminates, centrifugal, get supernatant, for subsequent use;
B: gained precipitation centrifugal in step a is added in salting liquid the suspension being made into solid content 10-20%, and pH value is adjusted to 7.0-10.0, then proceed in circulating ultrasonic wave extraction apparatus, the ultrasonic extraction of second time is carried out when ultrasonic extraction conditions is identical with first time, ultrasonic extraction terminates, centrifugal, get supernatant, for subsequent use;
C: combining step a and b gained supernatant, system pH is adjusted to 4.0-5.0 by acid adding, leaves standstill 30-60min, centrifugal, collects sesame protein precipitation, for subsequent use;
3) sesame protein purifying
Step c gained sesame protein precipitation is added water be made into 2-6% suspension, and pH is adjusted to 6.8-7.2, ultra-filtration and separation, ultrafiltration concentration liquid obtains sesame protein product after drying.
2. ultrasonic assistant weak base extracts the method for albumen in cold press sesame cake meal as claimed in claim 1, and it is characterized in that, in step 1), described liquefaction organic solvent is the mixture of butane, propane or butane and propane; Extraction conditions in subcritical abstraction tank is: 30-60 DEG C extract 3-5 times, and each extraction time is 20-40min, and every 1kg cold press sesame cake meal adds 2-5L liquefaction organic solvent.
3. ultrasonic assistant weak base extracts the method for albumen in cold press sesame cake meal as claimed in claim 1, and it is characterized in that, in step b and c, described salting liquid is the sodium-chloride water solution of concentration 0.2-0.8mol/L.
4. ultrasonic assistant weak base extracts the method for albumen in cold press sesame cake meal as claimed in claim 1, it is characterized in that, step 2) a and b in, condition when ultrasonic wave extracts: the ultrasonic frequency of employing is 20KHz, 40KHz, 59KHz or 20KHz and 40KHz or 20KHz and 59KHz, or 40KHz and 59KHz, ultrasonic wave working method is impulse type, and its working time is 3-1:1 with intermittent time ratio.
5. ultrasonic assistant weak base extracts the method for albumen in cold press sesame cake meal as claimed in claim 1, it is characterized in that, in step 3), for improving ultrafiltration effect, adopt two times of ultrafiltration, be again diluted with water to 2-6% by first time ultrafiltration gained concentrate and carry out second ultrafiltration; In ultra-filtration process, adopt the milipore filter of molecular cut off 5000-10000Da, ultrafiltration pressure is 0.2-0.5MPa, and operating temperature is 20-40 DEG C.
6. ultrasonic assistant weak base extracts the method for albumen in cold press sesame cake meal as claimed in claim 1, and it is characterized in that, in step 3), drying mode is vacuum drying, vacuum freeze drying or spraying dry; Vacuum drying operating condition is: pressure-0.08--0.10MPa, temperature 45-65 DEG C; The operating condition of vacuum freeze drying is: temperature-40--60
oc; Spray-dired operating condition is: 4-8% solid concentration, inlet temperature 160-200 DEG C, and outlet temperature is 60-80 DEG C, pressure 1.2-1.6MPa.
7. ultrasonic assistant weak base extracts the method for albumen in cold press sesame cake meal as claimed in claim 1, it is characterized in that, in step 3), after the permeate that ultra-filtration and separation obtains and the centrifugal gained supernatant of step c merge, plate-frame filtering removing suspension, again add salting liquid be made into 10-20% suspension and adjust pH to 7.0-10.0 be reused for sesame protein extract.
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| CN110357938A (en) * | 2019-08-30 | 2019-10-22 | 中国热带农业科学院香料饮料研究所 | A method of extracting albumen from Jack-fruit seeds |
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| EP3957188A4 (en) * | 2020-06-25 | 2022-09-07 | Queensbucket. Co., Ltd. | Method for preparing sesame oil meal extract and food composition comprising same as active ingredient for preventing or alleviating colitis |
| JP2022541355A (en) * | 2020-06-25 | 2022-09-26 | クイーンズバケット カンパニー，リミテッド | Method for producing sesame oil cake extract and food composition for preventing or improving colitis containing same as active ingredient |
| CN115191510A (en) * | 2022-06-10 | 2022-10-18 | 中国农业大学 | Low-temperature preparation method of pumpkin seed protein isolate and obtained product |
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