CN104186915A - Preparation method of oil soybean meal protein and application of oil soybean meal protein in beef sausage - Google Patents
Preparation method of oil soybean meal protein and application of oil soybean meal protein in beef sausage Download PDFInfo
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Abstract
The invention discloses a preparation method of oil soybean meal protein and an application of oil soybean meal protein in a beef sausage. The preparation method of the oil soybean meal protein comprises the following steps: carrying out supercritical oil extraction on cyperus esculentus, caking, crushing, screening, degreasing and adopting three times of ultrasonic auxiliary alkali leaching processes, wherein the first alkaline leaching process adopts the ratio of materials to liquid of 1 to 17, the ultrasound time of 26 minutes and the pH value of 9.6, and the second and the third alkaline leaching processes adopt the ratio of the materials to the liquid of 1 to 10, the pH value of 9.6, and the ultrasound time of 26 minutes; rotating by 3000 r/minute, centrifuging for 15 minutes, combining an alkali leaching liquid obtained in three times, carrying out acid precipitation for 1 hour under the condition that the pH value is 4.2, rotating by 3000 r/minute, centrifuging for 15 minutes, washing protein milk for 30 minutes by using 40-DEG C water with a weight of 5 times of the protein milk, washing for three times, and freezing and drying to obtain the oil soybean meal protein. The preparation method of the oil soybean meal protein and the application of the oil soybean meal protein in the beef sausage have the benefits that the yield of the applied beef sausage is improved by 21.59 percent, which is improved by 11.52 percent compared with the applied beef sausage added with soybean protein; the chewiness, the hardness, elasticity and other sausage gel indicators of the beef sausage can be obviously improved, and the application is wide.
Description
Technical field
The preparing technical field of the dregs of beans albumen the present invention relates to.Specifically, the present invention relates to a kind of preparation of oily Sha's dregs of beans albumen and the preparing technical field of application thereof.
Background technology
Oil Sha beans (
cyperus esculentus L.), having another name called chufa, Chufa, is a kind of Cyperus C4 of Cyperaceae plant.The English popular name of oil Sha beans has
cyperus esculentus, Chufa Flatsedge, Tigernut Sedge, Yellow Nutsedge, Yellow Nutgrass, Yellow Umbrella-sedgewith
earthalmonddeng.Oil Sha beans are a kind of very general perennial weeds in history at torrid areas and Mediterranean Region.Oil Sha beans can produce underground stem tuber like nut, are called as the vegetables of the stem tuber of " underground almond ".Oil Sha beans are a kind of healthy food, it was reported that oily Sha's beans energy prevention of cardiac, and thrombosis, reduces the risk of colon cancer and can activate blood circulation.Oil Sha beans stem tuber contains abundant starch, fat, sucrose and protein energy source, phosphorus and potassium mineral matter, vitamin C and vitamin E.Oil Sha beans output is the highest in current oil crops, thereby countries in the world agricultural experts are referred to as the king of oil crops.Oil Sha beans are also the ideal food of people Lai Shuoshi to diabetic and fat-reducing.Oil Sha beans are widely used in animal feed and human consumption.
Fewer to oily Sha's beans research at present, and mainly concentrate on the aspects such as oily Sha's beans starch, cyperus esculentus oil, oily Sha's legumin extraction application.But for oily Sha's legumin evaluation of nutrition no one report.Have not yet to see the research report of the application of oily Sha's dregs of beans albumen in beef sausage.
Summary of the invention
For the state of the art that has no the application in beef sausage about the evaluation of nutrition of oily Sha's legumin and oily Sha's dregs of beans albumen in prior art, the technical issues that need to address of the present invention are just to overcome the defect of prior art, aim to provide a kind of preparation of oily Sha's dregs of beans albumen and the application in beef sausage thereof, oily Sha's dregs of beans albumen of preparation under equal conditions, oil Sha dregs of beans protein product is compared with the functional characteristic of soybean protein, the frothing capacity of oil Sha dregs of beans albumen is higher than the soybean protein of common employing, and the application in beef sausage obtains good significant technique effect.
Technical scheme provided by the invention:
The present invention is by the preparation of oily Sha's dregs of beans, degreasing, pulverize and sieve, ultrasonic auxiliary alkali immersion is carried, centrifugal, acid is heavy, oily Sha's dregs of beans albumen is prepared in washing, freeze drying; The present invention is raw material by take oily Sha's dregs of beans, studies the technique that ultrasonic auxiliary alkali formulation is prepared oily Sha's dregs of beans albumen; First determine the major influence factors of extraction process, further design Box-Behnken experiment, take protein extracting ratio as index, optimize the optimum process that alkali of oily Sha's dregs of beans albumen is carried, and study extraction time and the impact of washing process on oily Sha's dregs of beans albumen yield, thereby finally determine the preparation technology parameter of oily Sha's dregs of beans albumen; In oily Sha's dregs of beans of preparation, contain crude protein 8.54%, soluble sugar 30.11%, starch 34.23%, ash content 7.87%, fat 5.15%, moisture 4.03%, crude fibre 11.12%.The beef sausage that adds oily Sha's dregs of beans albumen of 2.5%, yield rate is 83.78%, compares blank group and has improved 21.59%, than the soybean protein of the most common employing, has improved 11.52%.Matter structure analysis result shows that the interpolation of oily Sha's dregs of beans albumen can improve the chewiness of beef sausage, hardness, and elasticity, the meat intestines gel indexs such as cohesion, are with a wide range of applications.
The present invention specifically provides a kind of oily Sha's dregs of beans albumen, specifically by following technique, prepares, and % is according to weight percent meter, and concrete preparation method's step is as follows:
By oily Sha's beans through overcritical carry oil after grouts, pulverized 40 order to 100 mesh sieves, prepare oily Sha's dregs of beans through degreasing, pulverize by ultrasonic auxiliary alkali liquid extracting technology, alkali is carried process using solid-liquid ratio and is counted in mass ratio 1:(15-25 for the first time), ultrasonic time 25min to 45min, pH value 9-11, the isoelectric point of oily Sha's dregs of beans albumen is pI=3.8-4.4; Five alkali of for the second time to the are carried solid-liquid ratio and are counted in mass ratio 1:10, pH value 9.6, ultrasonic time 26min, the centrifugal 15min of 3000r/min, merges alkali extract several times, the heavy 1h of acid under pH value 3.8-4.4 condition, the centrifugal 15min of 3000r/min, albumin milk, is washed 2-4 time through washing 30min with the water of 40 ℃ to 60 ℃ of 5 times of weight, through freeze drying, prepares oily Sha's dregs of beans albumen.
Meanwhile, the present invention specifically provides a kind of oily Sha's dregs of beans albumen, specifically by following optimum process, prepares, and % is according to weight percent meter, and concrete optimum preparation method's step is as follows:
By oily Sha's beans through overcritical carry oil after grouts, pulverized 40 mesh sieves, prepare oily Sha's dregs of beans through degreasing, pulverize by ultrasonic auxiliary three alkali lye extracting technologies, alkali is carried process using solid-liquid ratio and is counted in mass ratio 1:17 for the first time, ultrasonic time 26min, pH value 9.6, recovery rate 44.01%, the isoelectric point of oily Sha's dregs of beans albumen is pI=4.2; Second and third alkali is carried solid-liquid ratio and is counted in mass ratio 1:10, pH value 9.6, ultrasonic time 26min, the centrifugal 15min of 3000r/min, merges three times alkali extract, the heavy 1h of acid under pH value 4.2 conditions, the centrifugal 15min of 3000r/min, 40 ℃ of water washing 30min of 5 times of weight for albumin milk, wash 3 times, oily Sha's dregs of beans albumen that freeze drying obtains: purity 43.54%, yield 26.85%.
In oily Sha's dregs of beans that the present invention is prepared by the above-mentioned preparation technology who provides, contain crude protein 8.54%, soluble sugar 30.11%, starch 34.23%, ash content 7.87%, fat 5.15%, moisture 4.03%, crude fibre 11.12%.
Meanwhile, the application of the oily Sha's dregs of beans albumen that the invention provides above-mentioned preparation in beef sausage, the addition of oily Sha's dregs of beans albumen is 2%-3% according to weight ratio.
Further, the present invention confirms by test, adopt common methods to prepare oily Sha's dregs of beans albumen applies in beef sausage, yield rate is all significantly improved under the same conditions on year-on-year basis, than this area the soybean protein of common employing all increase significantly, by matter structure analysis result, show that the interpolation of oily Sha's dregs of beans albumen can improve the chewiness of beef sausage, hardness, elasticity, the meat intestines gel indexs such as cohesion, show that the application in beef sausage obtains good significant effect by oily Sha's dregs of beans albumen.
By implementing the concrete summary of the invention of the present invention, can reach following beneficial effect:
(1) by response surface method, optimize and determine optimum oily Sha's dregs of beans albumen preparation technology: oily Sha's dregs of beans through degreasing, pulverize by ultrasonic auxiliary alkali liquid extracting technology, alkali is carried process using solid-liquid ratio and is counted in mass ratio 1:(15-25 for the first time), ultrasonic time 25min to 45min, pH value 9-11, the isoelectric point of oily Sha's dregs of beans albumen is pI=3.8-4.4, five alkali of for the second time to the are carried solid-liquid ratio and are counted in mass ratio 1:10, pH value 9.6, ultrasonic time 26min, the centrifugal 15min of 3000r/min, merge alkali extract several times, the heavy 1h of acid under pH value 3.8-4.4 condition, the centrifugal 15min of 3000r/min, albumin milk with the water of 40 ℃ to 60 ℃ of 5 times of weight through washing 30min, wash 2-4 time, through freeze drying, prepare oily Sha's dregs of beans albumen, oil Sha dregs of beans albumen yield is up to 26.85%, oil Sha dregs of beans purity of protein reaches 43.54%, in oily Sha's dregs of beans of preparation, contain crude protein 8.54%, soluble sugar 30.11%, starch 34.23%, ash content 7.87%, fat 5.15%, moisture 4.03%, crude fibre 11.12%.
(2) oily Sha's dregs of beans protein ratio of being prepared by the present invention adopts modal soybean protein isolate to be more suitable for being added in beef sausage, addition and yield rate positive correlation, and coefficient correlation 0.961, P<0.01 is extremely remarkable.Can add oily Sha's dregs of beans albumen of 2-3% in beef sausage, the beef sausage of oily Sha's dregs of beans albumen of interpolation 2.5%, yield rate is 83.78%, compares blank group and has improved 21.59%, than soybean protein, has improved 11.52%.Matter structure analysis result shows that the interpolation of oily Sha's dregs of beans albumen can improve the chewiness of beef sausage, hardness, elasticity, the meat intestines gel indexs such as cohesion.
Accompanying drawing explanation
Fig. 1 is shown as Coomassie brilliant blue canonical plotting.
Fig. 2 is shown as the affect figure of solid-liquid ratio on oily Sha's dregs of beans protein extracting ratio.
Fig. 3 is shown as the affect figure of pH on oily Sha's dregs of beans protein extracting ratio.
Fig. 4 is shown as the affect figure of ultrasonic time on oily Sha's dregs of beans protein extracting ratio.
Fig. 5 is shown as the affect figure of ultrasonic power on oily Sha's dregs of beans protein extracting ratio.
Fig. 6 is shown as and pulverizes the affect figure of order number on oily Sha's dregs of beans protein extracting ratio.
Fig. 7 is shown as solid-liquid ratio and the response surface figure of ultrasonic time factor reciprocation on absorbance impact.
Fig. 8 is shown as solid-liquid ratio and PH factor reciprocation to the response surface figure on absorbance impact.
Fig. 9 is shown as ultrasonic time and PH factor reciprocation to the response surface figure on absorbance impact.
Figure 10 is shown as oily Sha's dregs of beans albumen isoelectric point determination result figure.
Figure 11 is shown as alkali and carries the affect figure of number of times on albumen yield.
Figure 12 is shown as the affect figure of washing times on oily Sha's dregs of beans albumen yield.
Figure 13 is shown as washing temperature affects figure to the yield of oily Sha's dregs of beans albumen.
The specific embodiment
Below, for embodiment, the present invention is described, still, the present invention is not limited to following embodiment, and the % substantially relating in the present invention is weight percent meter without specializing.
The main raw and auxiliary material and the instrument and equipment that adopt: oily Sha's dregs of beans albumen: laboratory self-control; The imperial fish oil of gold: commercial; Soybean protein isolate: food stage; Beef, sheep intestines, sheep oil, seasoning matter: commercial; FSH-2A is adjustable high-speed homogenization mulser: Jintan City Medical Instruments factory, NDJ-1 viscosimeter: Jintan City instrument plant; TDL-5-A type centrifuge: Town in Shanghai is enjoyed scientific instrument factory; UV-2000 spectrophotometer: You Keni Shanghai Instrument Ltd.; HH-S2 digital display thermostat water bath: Jintan City Medical Instruments factory; FW-100 high speed Universalpulverizer; KXL high temperature disappears and boils stove, assembling nitrogen apparatus; TDL-5-A type centrifuge: Town in Shanghai is enjoyed scientific instrument factory; Freeze drier: Beijing Bo Yikang laboratory apparatus Co., Ltd; UV-2000 spectrophotometer: You Keni Shanghai Instrument Ltd.; HH-S2 digital display thermostat water bath: Jintan City Medical Instruments factory; FW-100 high speed Universalpulverizer; Chamber type electric resistance furnace: Shenyang City's electric furnace factory KXL high temperature disappears and boils stove, assembling nitrogen apparatus etc.
All raw and auxiliary materials of selecting in the present invention, selected all reagent and instrument are all well known selecting, but do not limit enforcement of the present invention, other reagent more well known in the art and equipment are all applicable to the enforcement of the following embodiment of the present invention.
embodiment mono-: the preparation of oily Sha's dregs of beans albumen
% is according to weight percent meter, solid-liquid ratio is according to weight ratio meter, by oily Sha's beans through overcritical carry oil after grouts, pulverized 40 order to 100 mesh sieves, prepare oily Sha's dregs of beans through degreasing, pulverize by ultrasonic auxiliary alkali liquid extracting technology, alkali is carried process using solid-liquid ratio and is counted in mass ratio 1:(15-25 for the first time), ultrasonic time 25min to 45min, pH value 9-11, the isoelectric point of oily Sha's dregs of beans albumen is pI=3.8-4.4; Five alkali of for the second time to the are carried solid-liquid ratio and are counted in mass ratio 1:10, pH value 9.6, ultrasonic time 26min, the centrifugal 15min of 3000r/min, merges alkali extract several times, the heavy 1h of acid under pH value 3.8-4.4 condition, the centrifugal 15min of 3000r/min, albumin milk, is washed 2-4 time through washing 30min with the water of 40 ℃ to 60 ℃ of 5 times of weight, through freeze drying, prepares oily Sha's dregs of beans albumen.
In oily Sha's dregs of beans that the present invention is prepared by the above-mentioned preparation technology who provides, contain crude protein 8.54%, soluble sugar 30.11%, starch 34.23%, ash content 7.87%, fat 5.15%, moisture 4.03%, crude fibre 11.12%.
embodiment bis-: the preparation of oily Sha's dregs of beans albumen
% is according to weight percent meter, solid-liquid ratio is according to weight ratio meter, by oily Sha's beans through overcritical carry oil after grouts, pulverized 40 mesh sieves, prepare oily Sha's dregs of beans through degreasing, pulverize by ultrasonic auxiliary three alkali lye extracting technologies, alkali is carried process using solid-liquid ratio and is counted in mass ratio 1:17 for the first time, ultrasonic time 26min, pH value 9.6, recovery rate 44.01%, the isoelectric point of oily Sha's dregs of beans albumen is pI=4.2; Second and third alkali is carried solid-liquid ratio and is counted in mass ratio 1:10, pH value 9.6, ultrasonic time 26min, the centrifugal 15min of 3000r/min, merges three times alkali extract, the heavy 1h of acid under pH value 4.2 conditions, the centrifugal 15min of 3000r/min, 40 ℃ of water washing 30min of 5 times of weight for albumin milk, wash 3 times, oily Sha's dregs of beans albumen that freeze drying obtains: purity 43.54%, yield 26.85%.
embodiment tri-: Coomassie brilliant blue Specification Curve of Increasing
1.1 Coomassie brilliant blue Specification Curve of Increasings: the bovine serum albumin of preparation 100 μ g/mL, get respectively 0mL, 0.1mL, 0.2mL, 0.3mL, 0.4mL, 0.5mL, in 0.6mL and test tube, with 0.15M NaCl solution, mend to 1mL, after add 5mL to prepare in advance Coomassie brilliant blue solution, after standing 10min, in 595nm, measure light absorption value, drawing standard curve.
1.2 oily Sha's dregs of beans protein extracting ratio and yield
Crude protein content * 100% in protein content ÷ raw material in oil Sha dregs of beans protein extracting ratio=extract
Oil Sha dregs of beans albumen yield=(protein sample weight * crude protein content) ÷ (raw material weight * crude protein content)
Crude protein content in oil Sha's dregs of beans and oily Sha's legumin powder all adopts Kjeldahl's method N * 6.25, and the protein content in extract adopts Coomassie brilliant blue method to measure.
1.3 calibration curves and regression equation: the Coomassie brilliant blue calibration curve that experiment is drawn, in 0-60 μ g/mL concentration ranges, linear good, R2 is 0.9922.
embodiment tetra-: the optimum preparation condition of oily Sha's dregs of beans albumen
1.1 oily Sha's dregs of beans albumen are prepared experiment of single factor
1.1.1 the impact of liquid ratio on oily Sha's dregs of beans protein extracting ratio: accurately take 20g degreasing oil Sha's bean cake powder (40 order) 5 parts, liquid ratio with 1:5,1:10,1:15,1:20,1:25 adds deionized water respectively, at pH, be 9, ultrasonic temperature is ultrasonic 25 min under the condition of 40 ℃, then centrifuging and taking supernatant, by Coomassie brilliant blue method, survey the light absorption value at its 595 nm places, place, each level is established three parallel laboratory tests, get its mean value, the oily Sha's dregs of beans protein extracting ratio of take is index, analyzes the impact that liquid material comparison albumen leaches recovery rate.
From accompanying drawing 2 results, find out, solid-liquid ratio on the extraction impact of oily Sha's dregs of beans albumen significantly, increase along with solid-liquid ratio, there is the stripping of more oily Sha's dregs of beans albumen, recovery rate raises, and during to 1:15, recovery rate tends to be steady, consider the purity of financial cost and oily Sha's dregs of beans albumen, selection 1:(15-25) solid-liquid ratio be the suitableeest solid-liquid ratio.
1.1.2 the impact of pH value on oily Sha's dregs of beans albumen leaching rate: accurately take 20g degreasing oil Sha's bean cake powder (40 order) 5 parts, the distilled water that adds respectively 300 mL, ultrasonic temperature be 30 ± 5 ℃, pH be 7,8., ultrasonic 25min under 9,10,11 condition, other operations are the same.
By accompanying drawing 3 results are clear, find out, pH is large on the impact of oily Sha's dregs of beans protein extracting ratio, rising along with pH, the recovery rate ascendant trend of oil Sha dregs of beans albumen is very steep, illustrate that pH is large on the recovery rate impact of oily Sha's dregs of beans albumen, when pH is greater than 9, although recovery rate is still increasing, consider that concentration of lye is too large, starch and some sugar can be dissolved in wherein, are that purity of protein reduces, and concentration of lye too greatly also has some ANFs generations simultaneously, being unfavorable for nutrient health, is optimum pH scope therefore select pH9-11.
1.1.3 the impact of ultrasonic time on oily Sha's dregs of beans protein extracting ratio: accurately take 20g degreasing oil Sha's bean cake powder (40 order) 7 parts, the deionized water that adds respectively 300mL, difference ultrasonic 10 min, 15 min, 20 min, 25 min, 30 min under the condition that is 9 at the ultrasonic temperature of 30 ± 5 ℃, pH, 35min, 45min is centrifuging and taking supernatant then, and other operations are the same.
By accompanying drawing 4, found out, the extraction positive correlation of ultrasonic time and oily Sha's dregs of beans albumen, when ultrasonic time reaches 25min, the extraction rate reached of oily Sha's dregs of beans albumen, to 44% left and right, has again subsequently to a certain degree and declines, and after 35 minutes, curve tends to be steady.This be due to, ultrasonic time is long, some starch molecules also thereupon stripping affect protein extracting ratio, simultaneously, ultrasonic time is long, and slight sex change occurs oily Sha's dregs of beans albumen, and oily Sha's dregs of beans protein micromolecular is assembled again, be difficult to separated with starch, therefore choose ultrasonic time 25min to 45min as fit value.
1.1.4 the impact of ultrasonic power on oily Sha's dregs of beans protein extracting ratio: accurately take 20g degreasing oil Sha's bean cake powder (40 order) 7 parts, at solid-liquid ratio 1:15, pH9, ultrasonic time 25min, under the condition that ultrasonic temperature is 30 ± 5 ℃, respectively with 160w, 200w, 240w, 280w, 320w, 360w, under 400w constant power condition, carry out oily Sha's dregs of beans protein extraction, centrifuging and taking supernatant, other operations are the same.
By accompanying drawing 5, be found that, ultrasonic power is not remarkable on the impact of oily Sha's dregs of beans albumen, considers energy-conservationly, and choosing 160w to 400w is operating power.
1.1.5 pulverize the impact of order number on oily Sha's dregs of beans albumen leaching rate: accurately take 20g degreasing oil Sha bean cake powder (40 orders, 60 orders, 80 orders, 100 orders) each portion, the distilled water that adds respectively 300 mL, ultrasonic 25min under the condition that is 9 at pH, ultrasonic temperature is 30 ± 5 ℃.Then centrifuging and taking supernatant, other operations are the same.
By accompanying drawing 6 results, within the scope of 40-100 objects, oily Sha's dregs of beans protein extracting ratio is without significant difference, along with the increase recovery rate rising of order number.Repeatedly pulverize and sieve complex steps, and can cause significant loss to a certain extent, therefore select 40 order to 100 objects oil Sha bean cake powders for extracting raw material.
2.1 principal element screenings
According to experiment of single factor result, utilize the Two-1evel experimental design screening in design-expeter8.06 software to pulverize order number, solid-liquid ratio, pH, ultrasonic time, the major influence factors in the factors such as ultrasonic power.Specifically referring to table 1 and table 2.
Table 1: two horizontal factor screening design tables
? | -1 | 1 |
Solid-liquid ratio | 1:5 | 1:15 |
Ultrasonic time min | 10 | 25 |
Ultrasonic power w | 240 | 360 |
Pulverize order number | 40 | 100 |
PH value | 7 | 11 |
Note :-1 represents the minimum level of response in experiment of single factor, and 1 represents the level that response is the highest
Table: 2: two level design screening principal element results
? | Solid-liquid ratio | Ultrasonic time min | Ultrasonic power W | Pulverize order number | PH value | Recovery rate % |
1 | -1 | -1 | -1 | 1 | 1 | 9.27 |
2 | 1 | -1 | -1 | -1 | -1 | 7.11 |
3 | -1 | 1 | -1 | -1 | 1 | 22.23 |
4 | 1 | 1 | -1 | 1 | -1 | 15.58 |
5 | -1 | -1 | 1 | 1 | -1 | 6.62 |
6 | 1 | -1 | 1 | -1 | 1 | 28.97 |
7 | -1 | 1 | 1 | -1 | -1 | 12.82 |
8 | 1 | 1 | 1 | 1 | 1 | 44.05 |
Table 3: each factor variance analytical table
Soruces of variation | The free degree | All square | F value | Prob>F |
Solid-liquid ratio | 1 | 250.54 | 22.42 | 0.0418* |
Ultrasonic time | 1 | 228.02 | 20.41 | 0.0457* |
Ultrasonic power | 1 | 183.07 | 16.38 | 0.0560 |
Pulverize order number | 1 | 2.41 | 0.22 | 0.6881 |
pH | 1 | 486.56 | 43.55 | 0.0222* |
Note * represents remarkable p<0.05
By table 3 result, found out, the secondary factors that affects oily Sha's dregs of beans recovery rate is that pH> solid-liquid ratio > ultrasonic time > ultrasonic power > pulverizes order number, pH wherein, solid-liquid ratio, ultrasonic time is remarkable on the recovery rate impact of oily Sha's dregs of beans albumen, therefore select pH, solid-liquid ratio, ultrasonic time is that principal element is carried out BBD response surface optimal design, determines the optimal level of each factor.
embodiment five: the optimum preparation condition of oily Sha's dregs of beans albumen
1.1 response surface methods are optimized oily Sha's dregs of beans albumen preparation technology
According to experiment of single factor and Two-1evel experimental design result, select after suitable factor and horizontal extent according to the center combination principle design experiment of Box-Behnken, optimize protein extraction technique.
Table 4: response surface factor level table
Level | X 1Solid-liquid ratio | X 2Ultrasonic time (min) | X 3pH |
-1 | 10 | 20 | 8 |
0 | 15 | 25 | 9 |
1 | 20 | 30 | 10 |
Center repeats to test 3 times.
Table 5: response surface experimental program and result
Sequence number | Solid-liquid ratio (X 1) | Ultrasonic time (X 2,min) | pH(X 3) | Y recovery rate (%) |
1 | 10 | 20 | 9 | 36.54 |
2 | 20 | 20 | 9 | 38.63 |
3 | 10 | 30 | 9 | 37.23 |
4 | 20 | 30 | 9 | 40.97 |
5 | 15 | 25 | 8 | 33.53 |
6 | 15 | 25 | 8 | 33.69 |
7 | 20 | 25 | 10 | 39.61 |
8 | 20 | 25 | 10 | 42.49 |
9 | 15 | 20 | 8 | 33.34 |
10 | 15 | 30 | 8 | 33.48 |
11 | 15 | 20 | 10 | 40.04 |
12 | 15 | 30 | 10 | 41.88 |
13 | 15 | 25 | 9 | 43.47 |
14 | 15 | 25 | 9 | 43.01 |
15 | 15 | 25 | 9 | 43.75 |
Table 6: regression model coefficient and the results of analysis of variance
Table 7: variance analysis 2
By: 6,7 analysis results are found out, F=84.45 > F
0.05(9,9)=3.18, p < 0.0001, shows that regression model is remarkable.Lose and intend a F=2.63 < F
0.05(9,3)=8.81, p=0.2844 > 0.05, not remarkable, illustrate that this models fitting degree is good, test error is little, can be used as forecast model.X wherein
1, X
2, X
3, X
1x
3, X
12, X
22, X
327 are significantly, remain two not remarkable.By table 6,7 analysis results, found out this model R
2=0.9935, illustrate that model is linear good, prediction R
2(Pred-R
2)=0.9134 and modified R
2(Adj R
2)=0.9817 approaches, and illustrates that this model has good precision of prediction, and Adeq Precision23.772>4, illustrates that this model has extremely strong response signal, represents that this model prediction precision is high.
Through software computational analysis, obtain matching regression equation, oily Sha's dregs of beans protein extraction response surface model:
Y=-333.528+1.538X
1+4.325X
2+64.72X
3+0.016X
1X
2+0.136X
1X
3+0.085X
2X
3-0.098X
1 2-0.104?X
2 2-3.618?X
3 2
Comprehensively analyze, the recurrence of this oil Sha dregs of beans protein extraction model is remarkable, loses a plan F value very little and not remarkable, shows that this model theory predicted value and true experimental data are without significant difference, and models fitting is effective, and experimental error is little.Therefore can to experimental result, carry out analyses and prediction with the true point of this regression equation modeling experiment.
From accompanying drawing 7,8 and accompanying drawing 9, can reflect intuitively reciprocation and the impact on response of this each factor of model.Wherein the significant interaction of pH and solid-liquid ratio, illustrates, can see that matching response curved surface has maximum in solid-liquid ratio and pH figure, by software, fit equation is asked to local derviation, can draw model maximum, solid-liquid ratio 1:16.59, ultrasonic time 25.95min, pH 9.56 prediction recovery rates 44.69%.Through in conjunction with practical operation condition, be modified to solid-liquid ratio 1:17, ultrasonic time 26min, pH9.6
By confirmatory experiment, carry out three times and repeat, show that the recovery rate under this optimal conditions is 44.01% ± 0.38%, close with the analogue value, relative error 0.68% <1%, illustrates that Regression Model Simulator is better.The predicted maximum of the regression equation of gained and validation value are very approaching, illustrate that regression equation can reflect the impact of the factor of respectively screening truly, and model and the actual conditions of foundation are more identical.Therefore, to put forward the condition of oily Sha's dregs of beans albumen be desirable to alkali of response surface method optimization.Therefore determine that optimum Extraction technique is solid-liquid ratio 1:17, ultrasonic time 26min, pH value 9.6.
Conclusion: optimized an alkali by response surface method and put forward extraction process: optimum process is solid-liquid ratio 1:17, ultrasonic time 26min, pH9.6, recovery rate 44.01%.
embodiment six: the optimum preparation condition of oily Sha's dregs of beans albumen
The sour heavy isoelectric point of 1.1 oily Sha's dregs of beans albumen preparation technology is determined: fixed extraction technique, and solid-liquid ratio 1:15, pH9, ultrasonic 30min, determines the heavy pH of acid by measuring residual protein content in the heavy rear supernatant of acid.
From accompanying drawing 10, find out, the isoelectric point of oily Sha's dregs of beans albumen is in 3.8-4.6 scopes, and when pH4.2, protein content is minimum after measured, therefore select pH3.8-4.4, is the heavy pH. of acid of oily Sha's dregs of beans albumen.
conclusion:determined the isoelectric pH 3.8-4.4 of oily Sha's dregs of beans albumen, optimum pH 4.2.
The impact on oily Sha's dregs of beans albumen yield of 1.2 extraction times and washing process
One time alkali is carried condition pH9.6, solid-liquid ratio 1:17 ultrasonic time 26min, and repeatedly alkali is put forward condition: solid-liquid ratio 1:10, pH value 9.6, ultrasonic power 160W, time 26min.Through accompanying drawing 11, find out that alkali is carried number of times more, albumen yield is larger, and after three times alkali is carried, albumen yield tends to be steady, and three times alkali leach protein yield improves 6% than an alkali leach protein yield.Therefore definite secondary to four time alkali is carried, it is three times that optimum alkali is carried number of times.
Through alkali repeatedly, carry, albumin milk after acid is heavy adds 5 times of weight water, through 40 ℃ of washing 30min, 1-5 times, result shows, albumen must take the lead in increasing along with the increase of number of times, after surpassing 3 times, start to decline, this is because washing times is too much, and albumin milk approaches pH and raises, part protein is also soluble in water, causes albumen yield to decline.Therefore selecting washing times is 2 times to 4 times, optimum 3 times.
Through three alkali, carry, the albumin milk after acid is heavy is through washing 30min, 3 times, 30-70 ℃ of washing temperature.Result shows, during washing, 40 ℃ to 60 ℃ albumen yield are high, and during 40 ℃ of washings, albumen yield is the highest, reach 26.6%, continue to heat up, albumen yield declines to some extent, and this is due to excess Temperature, albumen starts to occur sex change, and along with the increase of denaturation degrees, albumen yield declines to some extent.
Table 8: orthogonal array
A alkali is carried number of times | B washing times | C washing temperature ℃ |
1 | 2 | 30 |
2 | 3 | 40 |
3 | 4 | 50 |
Table: 9: quadrature result table
A alkali is carried number of times | B washing times | C washing temperature | Blank column | Albumen yield % | |
Experiment 1 | 1 | 1 | 1 | 1 | 22.37 |
Experiment 2 | 1 | 2 | 2 | 2 | 24.28 |
Experiment 3 | 1 | 3 | 3 | 3 | 21.42 |
Experiment 4 | 2 | 1 | 2 | 3 | 26.81 |
Experiment 5 | 2 | 2 | 3 | 1 | 26.49 |
Experiment 6 | 2 | 3 | 1 | 2 | 23.17 |
Experiment 7 | 3 | 1 | 3 | 2 | 26.22 |
Experiment 8 | 3 | 2 | 1 | 3 | 26.14 |
Experiment 9 | 3 | 3 | 2 | 1 | 26.17 |
k1 | 22.69 | 25.133 | 23.893 | 25.01 | ? |
k2 | 25.49 | 25.637 | 25.753 | 24.557 | ? |
k3 | 26.177 | 23.587 | 24.71 | 24.79 | ? |
Extreme difference | 3.487 | 2.05 | 1.86 | 0.453 |
Table 10: analysis of variance table
Factor | Sum of square of deviations | The free degree | F ratio | F critical value | Conspicuousness |
Alkali is carried number of times | 20.468 | 2 | 66.455 | 19 | * |
Washing times | 6.848 | 2 | 22.234 | 19 | * |
Washing temperature | 5.215 | 2 | 16.932 | 19 | ? |
Error | 0.31 | 2 |
Note: * represents that p<0.05 is remarkable
Owing to once extracting and still having some protein that are dissolved out to be wrapped up by the impurity in oily Sha's dregs of beans, fail completely out centrifugal, therefore adopt alkali, propose the impact of number of times on the rate of oily Sha's dregs of beans albumen, therefore design orthogonal experiment, pass through orthogonal test, design orthogonal table is in Table 9, the oily Sha's dregs of beans albumen yield of take is further optimized the preparation technology of oily Sha's dregs of beans albumen as index, in table 9,10, quadrature result is found out, A3B2C2 is optimum combination, be alkali and carry number of times 3 times, wash 3 times, 40 ℃ of washing temperature are theoretical optimum process.Through table 10 the results of analysis of variance, learn, factor alkali carries number of times and washing times is remarkable on oily Sha's dregs of beans albumen yield impact, is major influence factors.
Empirical tests test, obtains a result as the yield 26.85% of oily Sha's dregs of beans albumen, and oily Sha's dregs of beans purity of protein 43.54%, a little more than the peak in 9 experiments, therefore this Orthogonal Optimum Design is feasible.
conclusion:by above-mentioned Optimum Experiment, oil Sha dregs of beans albumen preparation technology is: adopt 2 to 5 alkali to put forward technique, alkali is carried pH9-11 for the first time, solid-liquid ratio 1:(15-25), ultrasonic time 25min to 45min, five alkali of for the second time to the are carried solid-liquid ratio 1:10, pH value 9.6, ultrasonic time 26min, the centrifugal 15min of 3000r/min, merge alkali extract several times, the heavy 1h of acid under pH value 3.8-4.4 condition, the centrifugal 15min of 3000r/min, albumin milk with the 5 times heavy water of 40 ℃ to 60 ℃ through washing 30min, wash 2-4 time, freeze drying prepares oily Sha's dregs of beans albumen.
Optimum process: adopt 3 alkali to put forward technique, alkali is carried solid-liquid ratio 1:17 for the first time, ultrasonic time 26min, pH value 9.6, extremely alkali is carried solid-liquid ratio 1:10, pH value 9.6 for the third time for the second time, ultrasonic time 26min, the centrifugal 15min of 3000r/min, merges repeatedly alkali extract, and the isoelectric point of oily Sha's dregs of beans albumen is pI=4.2; Determine that alkali carries number of times 3 times, 40 ℃ of washing temperature, wash 3 times, oily Sha's dregs of beans albumen yield 26.85%, oily Sha's dregs of beans purity of protein 43.54%.
embodiment seven: oily Sha's dregs of beans albumen and the comparison of soybean protein isolate functional character
As follows by oily Sha's dregs of beans albumen and this area modal soybean protein isolate functional character comparative test result prepared by the present invention, in Table 2
Table 11 oily Sha's dregs of beans albumen and the comparison of soybean protein isolate functional character
? | Dissolubility g/l | Foaming characteristic ml | Foaming stability mL | Emulsibility | Emulsibility is stable | Viscosity | Retentiveness | Hold oiliness |
Oil Sha dregs of beans albumen | 4.84 | 85 | 78 | 20% | 15% | 10mPa.s | 3.1g/g | 4.2g/g |
Soybean protein | 5.86 | 80 | 75 | 26% | 21% | 40mPa.s | 4.3g/g | 2.1g/g |
By table 11 result, found out, under equal conditions, oil Sha dregs of beans protein product is compared with the functional characteristic of the modal soybean protein in this area, the frothing capacity outline of oil Sha dregs of beans albumen is higher than soybean protein, holding oiliness can be apparently higher than soybean protein, all the other functional characteristics all lower than or approach soybean protein, the dissolubility of this and oily Sha's dregs of beans albumen has direct relation.
embodiment eight: the making of oily Sha's dregs of beans albumen application beef sausage
The 1.1 main technique routes that adopt: fresh beef → drip washing → dicing → pickling → cut half → bowel lavage → tying → boiling → packing → finished product beef sausage
1.2 beef sausage basic components: beef 70g, sheep oil 20g, protein 1-3g, salt 8g
1.3 key points for operation: dice: the square meat cubelets that beef are cut into 1cm; Pickle: by the meat cubelets that cut and spicy face, fennel powder, salt mixes by a certain percentage, pickles 2h; Cut half: add a certain amount of protein, be aided with frozen water and cut fast partly 30 minutes, meat gruel is placed to 4 degree refrigerators cooling; Bowel lavage: meat gruel is poured in clean sheep casing, and sealing, uses small pinhead exhaust; Boiling: boiling 30min in boiling water steam.
1.4 beef sausage yield rates calculate
Yield rate=(M/a-b) * 100%, in formula, M is beef sausage quality after boiling, and a is beef sausage quality before boiling, and b is casing quality
1.5 beef sausage subjective appreciations
By 10 Food Science professionals, form evaluation group, respectively beef sausage sample is marked, every index total points each 10 minutes, then calculates total points.Aesthetic quality's standards of grading are in Table 1.
table 12: sensory evaluation scores standard
Color and luster | Mouthfeel | Chewiness (kg) | Outward appearance | Scoring |
Cerise | Tasty and refreshing, exquisiteness, beef flavour is dense | >1.2 | Casing is bright and clean, complete | 10 |
Pale red | Fine and smooth smooth, beef flavour is dense | 1-1.2 | Bright and clean slightly poor, complete whole | 8 |
Canescence | Coarse, slightly meat grain sense, has micro-astringent taste | 0.8-1 | Bright and clean slightly poor, casing has slight crack | 6 |
Brown | There is the sense of obvious meat grain, the salty hardship of taste | 0.5-0.8 | Coarse, casing has obvious slight crack | 4 |
Brown | There is the sense of obvious powder meat grain, saline taste weight | <0.5 | Surface is soft coarse, obviously visible cube meat | 2 |
embodiment nine: oily Sha's dregs of beans albumen is applied in beef sausage
Determining of the optimum addition of 1.1 oily Sha's dregs of beans albumen
With soybean protein isolate, compare.With reference to the people's such as Liu Xiuhe result of study [37], the addition that adds oily Sha's dregs of beans albumen prepared by the present invention in beef sausage is 2-3%, and to adopt the addition of soybean protein isolate conventional in meat intestines be 2-3% in test in contrast.Therefore in beef sausage making experiment, the addition of oily Sha's dregs of beans albumen and soybean protein isolate is all got 2-3%, and carries out result of use comparison.
1.2 impacts of oily Sha's dregs of beans albumen addition on beef sausage yield rate, matter structure
Table 13: impact and the results of analysis of variance of different albumen additions on beef sausage yield rate, matter structure
? | Chew index Kg | Elasticity | Hardness Kg | Cohesion | Yield rate % |
Blank | 0.52±0.06 e | 0.73±0.005 d | 2.54±0.03 e | 0.28±0.01 e | 62.19±3.25 c |
1% oily Sha's dregs of beans albumen | 0.77±0.1 d | 0.76±0.01 c | 2.73±0.06 d | 0.37±0.005 c | 71.49±2.84 b |
1.5% oily Sha's dregs of beans albumen | 0.99±0.09 c | 0.82±0.02 a | 3.165±0.08 c | 0.38±0.01 c | 75.28±3.15 b |
2% oily Sha's dregs of beans albumen | 1.39±0.06 a | 0.78±0.01 bc | 3.736±0.08 a | 0.48±0.011 ab | 81.17±2.78 a |
2.5% oily Sha's dregs of beans albumen | 1.45±0.05 a | 0.79±0.01 b | 3.715±0.09 a | 0.5±0.01 a | 83.78±3.25 a |
3% oily Sha's dregs of beans albumen | 1.21±0.14 b | 0.79±0.02 b | 3.33±0.07 b | 0.46±0.01 b | 84.23±2.97 a |
2% soybean protein isolate | 0.92±0.11 cd | 0.79±0.005 b | 3.436±0.811 b | 0.34±0.015 d | 72.26±2.37 b |
Note: a, b, c, d level of signifiance p<0.05 SPSS 13.0 one-way analysis of variance multiple ratios are analyzed compared with LSD
Through SPSS correlation analysis, the addition positive correlation of beef sausage yield rate and oily Sha's dregs of beans albumen, coefficient correlation 0.961, P<0.01 is extremely remarkable.The addition that oily Sha's dregs of beans albumen is described has certain influence to the yield rate of beef sausage, from table 13 comparing result, add oily Sha's dregs of beans albumen 2% when above, the yield rate of beef sausage and texture index are all in rising trend, blank group and all the other 6 groups of significant differences, illustrate that adding protein can play quality and the yield rate that improves beef sausage, 2%, 2.5%, 3% addition for chew exponential sum hardness to affect difference not remarkable, because albumen adds too much, can affect the sense organ of beef sausage, therefore can select 2.5% for best when selecting addition.When oily Sha's dregs of beans albumen addition reaches 3%, the hardness of beef sausage declines to some extent, and this is due to oily Sha's dregs of beans albumen, to have strengthened the water absorbing capacity of beef sausage. and water can disappear to protein content increase the gel effect cause.
The chewiness of beef sausage is significant difference with the difference of oily Sha's dregs of beans albumen addition, and positive control soybean protein isolate is not except remarkable with 1% oily Sha's dregs of beans albumen addition group difference, more remarkable with all the other each groups.Beef sausage yield rate, control group and soybean protein positive controls and the equal significant difference of oily Sha's dregs of beans albumen addition group, oil Sha dregs of beans 2%, 2.5%, 3% 3 group of yield rate difference to beef sausage is not remarkable, soybean protein isolate group and 1%, 1.5% group of difference of oily Sha's dregs of beans albumen are not remarkable, illustrate that under addition of the same race, oily Sha's dregs of beans albumen is better than soybean protein isolate to the yield rate of beef sausage.By SPSS simple correlation, analyze, know addition and yield rate positive correlation, coefficient correlation 0.961, P<0.01 is extremely remarkable.
As shown in Table 13, oily Sha's dregs of beans albumen of interpolation 2% and the beef sausage yield rate of soybean protein isolate are respectively 81.17% and 72.26%, and this additive effect that oily Sha's dregs of beans albumen is described is better than soybean protein isolate.And oily Sha's dregs of beans albumen addition of 2.5%, 3.0% makes beef sausage yield rate, be 83.78%, compare blank group and improved 21.59%.This illustrates that oily Sha's dregs of beans albumen is used as additive in beef sausage, can improve beef sausage yield rate, reduces fat loss.
1.3 organoleptic analysis
table 14: sensory evaluation scores result
Blank | 68±0.02d |
1% oily Sha's dregs of beans albumen | 72±0.01c |
1.5% oily Sha's dregs of beans albumen | 74±0.05bc |
2% oily Sha's dregs of beans albumen | 78±0.12ab |
2.5% oily Sha's dregs of beans albumen | 80±0.01a |
3% oily Sha's dregs of beans albumen | 70±0.02cd |
2% soybean protein isolate | 76±0.04b |
Note: a, b, c, d level of signifiance p<0.05 SPSS 13.0 one-way analysis of variance multiple ratios are analyzed compared with LSD
By table 14 sensory evaluation scores, can be found out, according to oily Sha's dregs of beans albumen addition of 2.5%, obtain the best result of 80 minutes, therefore determine that the optimum quantum of utilization of oily Sha's dregs of beans albumen is 2.5%.
conclusion:according to the oily Sha's dregs of beans protein ratio soybean protein isolate that adds 2-3%, be more suitable for being added in beef sausage, addition and yield rate positive correlation, coefficient correlation 0.961, P<0.01 is extremely remarkable.The beef sausage of oily Sha's dregs of beans albumen of interpolation 2.5%, yield rate is 83.78%, compares blank group and has improved 21.59%, than soybean protein, has improved 11.52%.Matter structure analysis result shows that the interpolation of oily Sha's dregs of beans albumen can improve the chewiness of beef sausage, hardness, elasticity, the meat intestines gel indexs such as cohesion.
Further, the present invention confirms by test, adopt common methods to prepare oily Sha's dregs of beans albumen applies in beef sausage, yield rate is all significantly improved under the same conditions on year-on-year basis, than this area the soybean protein of common employing all increase significantly, by matter structure analysis result, show that the interpolation of oily Sha's dregs of beans albumen can improve the chewiness of beef sausage, hardness, elasticity, the meat intestines gel indexs such as cohesion, show that the application in beef sausage obtains good significant effect by oily Sha's dregs of beans albumen.
Above-described embodiment is only for example of the present invention is clearly described, and the not restriction to embodiment.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here exhaustive without also giving all embodiments.And the apparent variation of being amplified out thus or change are still among protection scope of the present invention.
Claims (3)
1. oily Sha's dregs of beans albumen, is characterized in that, oily Sha's dregs of beans albumen prepares by following technique, and % is according to weight percent meter:
By oily Sha's beans through overcritical carry oil after grouts, pulverized 40 order to 100 mesh sieves, prepare oily Sha's dregs of beans through degreasing, pulverize by ultrasonic auxiliary alkali liquid extracting technology, alkali is carried process using solid-liquid ratio and is counted in mass ratio 1:(15-25 for the first time), ultrasonic time 25min to 45min, pH value 9-11, the isoelectric point of oily Sha's dregs of beans albumen is pI=3.8-4.4; Five alkali of for the second time to the are carried solid-liquid ratio and are counted in mass ratio 1:10, pH value 9.6, ultrasonic time 26min, the centrifugal 15min of 3000r/min, merges alkali extract several times, the heavy 1h of acid under pH value 3.8-4.4 condition, the centrifugal 15min of 3000r/min, albumin milk, is washed 2-4 time through washing 30min with the water of 40 ℃ to 60 ℃ of 5 times of weight, through freeze drying, prepares oily Sha's dregs of beans albumen.
2. a kind of oily Sha's dregs of beans albumen according to claim 1, is characterized in that, oily Sha's dregs of beans albumen prepares by following technique, and % is according to weight percent meter:
By oily Sha's beans through overcritical carry oil after grouts, pulverized 40 mesh sieves, prepare oily Sha's dregs of beans through degreasing, pulverize by ultrasonic auxiliary three alkali lye extracting technologies, alkali is carried process using solid-liquid ratio and is counted in mass ratio 1:17 for the first time, ultrasonic time 26min, pH value 9.6, recovery rate 44.01%, the isoelectric point of oily Sha's dregs of beans albumen is pI=4.2; Second and third alkali is carried solid-liquid ratio and is counted in mass ratio 1:10, pH value 9.6, ultrasonic time 26min, the centrifugal 15min of 3000r/min, merges three times alkali extract, the heavy 1h of acid under pH value 4.2 conditions, the centrifugal 15min of 3000r/min, 40 ℃ of water washing 30min of 5 times of weight for albumin milk, wash oily Sha's dregs of beans albumen that freeze drying obtains 3 times.
3. the application of oily Sha's dregs of beans albumen according to claim 1 in beef sausage, is characterized in that, in beef sausage, the addition of oily Sha's dregs of beans albumen is 2%-3% according to weight ratio.
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