Summary of the invention
The present invention is directed to the state of the art that prior art is prepared about mutton taste flavor material, it is enzymolysis liquid that the present invention makes full use of corn protein powder, turns waste into wealth, by utilizing fatty controlled oxidization-thermal response system, adopt suet controlled oxidization to prepare mutton taste flavor material, there is the extensively value be suitable for.
The main technical schemes that the present invention adopts:
The present invention utilizes enzymatic isolation method to prepare corn protein powder enzymolysis liquid, with zein enzymolysis liquid, oxidation suet and wood sugar for primary raw material, interpolation sodium chloride, vitamin B1, cysteine hydrochloride, methionine carry out Maillard reaction and prepare Novel sheep meat flavour flavor material, not only prepare the natural mutton taste flavor material with strong Mutton Flavor, also for the deep processing and utilization of corn protein powder provides an effective way, the added value of corn protein powder is added.
The present invention specifically provides a kind of preparation method of mutton taste flavor material, and concrete preparation method is as follows:
(1) preparation of zeins: corn to be decoloured destarch through pretreatment, obtain the corn protein powder that protein content is higher, cross 80 mesh sieve, adopt ethanol immersion to prepare zeins, in g:mL, corn protein powder and 80% ethanol according to solid-liquid ratio 1:8, after 60 DEG C of water-bath lixiviate 5h, through the centrifugal 15min process of 3500r/min, get supernatant, through isoelectric precipitation, prepare zeins by freeze drying or heated-air drying;
(2) preparation of zeins enzymolysis liquid: take the zeins in step (1), take zeins as substrate, by concentration 1.5%, temperature 55 DEG C, pH 11.5 enzymolysis of concentration of substrate 10%, alkali protease, enzymolysis 5.0h under this condition, wherein, the vigor of alkali protease is 12.93 × 10
4u, pH scope 9.5-10.5, temperature range 40-55 DEG C, prepare zeins enzymolysis liquid, for subsequent use;
(3) preparation of corn protein powder enzymolysis liquid: take corn protein powder prepared by step (1), take corn protein powder as substrate, by concentration of substrate be 6%, basic protein enzyme concentration 3.0%, temperature 55 DEG C, pH 10.0 enzymolysis, enzymolysis 2.0h under this condition, wherein, the basic protein enzyme activity selected is 12.93 × 10
4u, pH scope 9.5-10.5, temperature range 40-55 DEG C, prepare corn protein powder enzymolysis liquid, for subsequent use;
(4) suet controlled oxidization: suet heating is made fusing, forms vortex through stirring, and adopts reflux condensation mode and temperature to control to carry out suet oxidation; The process conditions of suet controlled oxidization are: controlled oxidization time 4.0h, and controlled oxidization temperature is 135 DEG C, and throughput is 0.30m
3/ (Kg.h), under these process conditions, the PV value (peroxide value) recording this suet is 349.342 meq/Kg, AV value (anisidine value) be 192.658, S value (acid number) is 2.108 mgKOH/g, prepares oxidation suet;
(5) preparation of mutton taste flavor material: % by weight percentage, the oxidation suet utilizing above-mentioned steps to prepare and corn protein powder enzymolysis liquid or zeins enzymolysis liquid are primary raw material, add in corn protein powder enzymolysis liquid 88% or zeins enzymolysis liquid simultaneously the oxidation suet of 5%, 1.3% L-cysteine hydrochloride, the VB1 of 0.5%, methionine, 2% sodium chloride and the 3%D-wood sugar of 0.2% carry out Maillard reaction, reaction temperature is 120 DEG C, the initial pH of reaction is 6.5, reaction time is 2h, prepares mutton taste flavor material.
Simultaneously, the present invention specifically provides a kind of mutton taste flavor material, prepare according to the above-mentioned suet controlled oxidization preparation method provided, % by weight percentage, mutton taste flavor material contain 5% oxidation suet, 1.3% L-cysteine hydrochloride, 0.5% VB1,0.2% methionine, 2% sodium chloride, 3%D-wood sugar and 88% corn protein powder enzymolysis liquid.
Further.The present invention also provides another kind of mutton taste flavor material, prepare according to the above-mentioned suet controlled oxidization preparation method provided, % by weight percentage, mutton taste flavor material contain 5% oxidation suet, 1.3% L-cysteine hydrochloride, 0.5% VB1,0.2% methionine, 2% sodium chloride, 3%D-wood sugar and 88% zeins enzymolysis liquid.
Suet controlled oxidization index is respectively AV value (anisidine value), PV value (peroxide value) and S value (acid number); The product of suet controlled oxidization should have higher anisidine value, suitable high peroxide value, and this is favourable to follow-up thermal response; The acid number of oxidation suet should control in lower scope, otherwise suet can produce serious rancid flavor.
In the present invention, AV value (anisidine value), PV value (peroxide value) and S value (acid number) adopt GB/T 24304-2009, GB/T 5538-2005 and GB/T 5530-2005 [7-9] to measure respectively. using PV value (peroxide value), AV value (anisidine value), S value (acid number) as the index of suet controlled oxidization, in conjunction with sensory evaluation scoring and odor characteristic, the Optimal technique process finally determining suet controlled oxidization is: controlled oxidization time 4.0h, controlled oxidization temperature is 135 DEG C, and throughput is 0.30m
3/ (Kg.h); Adopt the preparation technology of Orthogonal Optimization Test to mutton taste flavor material to be optimized, the optimal conditions obtaining mutton taste flavor material Maillard reaction is: reaction temperature is 120 DEG C, and the initial pH of reaction is 6.5, and the reaction time is 2h.
It is well known technical scheme that the present invention adopts ethanol immersion to extract zeins, those skilled in the art can prepare extraction zeins according to prior art, but, the present invention preferentially adopts concentration of substrate 6%, basic protein enzyme concentration is 3.0%, temperature be 55 DEG C, pH is 10.0, enzymolysis 2.0h under this condition, obtains the hydrolyzate of corn protein powder.
By implementing the concrete summary of the invention of the present invention, following effect can be reached:
The present invention utilizes enzymatic isolation method to prepare corn protein powder enzymolysis liquid, with zein enzymolysis liquid, oxidation suet and wood sugar for primary raw material, interpolation sodium chloride, vitamin B1, cysteine hydrochloride, methionine carry out Maillard reaction and prepare Novel sheep meat flavour flavor material, this novel meat flavor material has fat perfume (or spice), meat is fragrant and roasting fragrant, full and the natural sense of tool, both the mouthfeel of people can have been met, be unlikely to again people is got fat, simultaneously also for the deep processing and utilization of corn protein powder provides an effective way, add the added value of corn protein powder.
Detailed description of the invention
, for embodiment, the present invention is described below, but the present invention is not limited to following embodiment.In addition, in following explanation, if no special instructions, % all refers to m/m mass percent.
In the present invention, equipment and material have:
Suet: commercially available; Corn protein powder enzymolysis liquid: laboratory is made by oneself; It is pure that sodium thiosulfate, KI, P-nethoxyaniline, Potassium Hydrogen Phthalate, potassium bichromate, soluble starch, glacial acetic acid, isooctane, absolute ether etc. are analysis
H HS electric-heated thermostatic water bath; 90-1 type constant temperature blender with magnetic force; Constant temperature indicating controller; Glass rotameter; The outer visible spectrophotometer of UV-2000 ultraviolet; AB204-S type analysis sky equality
The all reagent selected in the present invention and instrument are all well known selecting, but do not limit enforcement of the present invention, and 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 one: suet controlled oxidization prepares the determination of mutton taste flavor material formula
The formula of mutton taste flavor material, by test of many times and experiment, is determined to adopt corn protein powder enzymolysis liquid, D-wood sugar, L-cysteine hydrochloride, methionine, VB1, sodium chloride and oxidation suet.By the optimal case of the Orthogonal Optimization Test determination mutton taste flavor material of 6 factor 3 levels.The factor level table of orthogonal test and the results are shown in Table 1-3.
The factor level table of table 1 Mutton Flavor material formula
Table 2 mutton taste flavor material is filled a prescription six factor three horizontal quadrature table and results
Table 3 mutton taste flavor material formulation optimization analysis of variance table
Factor |
Variance quadratic sum |
The free degree |
F ratio |
F critical value |
Conspicuousness |
A/ is oxidized suet |
558.111 |
2 |
313.898 |
19.000 |
* |
B/D-wood sugar |
10.111 |
2 |
5.687 |
19.000 |
|
C/ sodium chloride |
32.111 |
2 |
18.060 |
19.000 |
|
D/ VB
1 |
103.444 |
2 |
58.180 |
19.000 |
* |
E/L-cysteine hydrochloride |
147.111 |
2 |
82.740 |
19.000 |
* |
F/ methionine |
52.111 |
2 |
29.309 |
19.000 |
* |
Error |
1.78 |
2 |
|
|
|
The Orthogonal Optimization Test result optimized from Mutton Flavor material formula and intuitive analysis table 2, R value size is: A (oxidation suet) >E (L-cysteine hydrochloride) >D (VB1) >F (methionine) >C (sodium chloride) >B (D-wood sugar), the analysis of variance table 3 of the Orthogonal Optimization Test result optimized from Mutton Flavor material formula, oxidation suet, L-cysteine hydrochloride, the flavor effect of ratio to Mutton Flavor material of VB1 and methionine is remarkable.Known by table 2, the optimum combination of the formula of mutton taste flavor material Maillard reaction is A2E2D2F1C2B3, i.e. the oxidation suet of 5%, the L-cysteine hydrochloride of 1.3%, the VB1 of 0.5%, the methionine of 0.2%, 2% sodium chloride, 3%D-wood sugar and 88% corn protein powder enzymolysis liquid.
Being combined as most of the formula of mutton taste flavor material Maillard reaction: the oxidation suet of 5%, the L-cysteine hydrochloride of 1.3%, the VB1 of 0.5%, the methionine of 0.2%, 2% sodium chloride, 3%D-wood sugar and 88% corn protein powder enzymolysis liquid.
embodiment two: the preparation method of mutton taste flavor material
See accompanying drawing 1, utilize fatty controlled oxidization-thermal response system, adopt suet controlled oxidization to prepare the method for mutton taste flavor material, concrete preparation method's step is as follows:
(1) preparation of zeins: corn to be decoloured destarch through pretreatment, obtain the corn protein powder that protein content is higher, cross 80 mesh sieve, adopt ethanol immersion to prepare zeins, in g:mL, corn protein powder and 80% ethanol according to solid-liquid ratio 1:8, after 60 DEG C of water-bath lixiviate 5h, through the centrifugal 15min process of 3500r/min, get supernatant, through isoelectric precipitation, prepare zeins by freeze drying or heated-air drying;
(2) preparation of zeins enzymolysis liquid: take the zeins in step (1), take zeins as substrate, by concentration 1.5%, temperature 55 DEG C, pH 11.5 enzymolysis of concentration of substrate 10%, alkali protease, enzymolysis 5.0h under this condition, wherein, the vigor of alkali protease is 12.93 × 10
4u, pH scope 9.5-10.5, temperature range 40-55 DEG C, prepare zeins enzymolysis liquid, for subsequent use;
(3) preparation of corn protein powder enzymolysis liquid: take corn protein powder prepared by step (1), take corn protein powder as substrate, by concentration of substrate be 6%, basic protein enzyme concentration 3.0%, temperature 55 DEG C, pH 10.0 enzymolysis, enzymolysis 2.0h under this condition, wherein, the basic protein enzyme activity selected is 12.93 × 10
4u, pH scope 9.5-10.5, temperature range 40-55 DEG C, prepare corn protein powder enzymolysis liquid, for subsequent use;
(4) suet controlled oxidization: suet heating is made fusing, forms vortex through stirring, and adopts reflux condensation mode and temperature to control to carry out suet oxidation; The process conditions of suet controlled oxidization are: controlled oxidization time 4.0h, and controlled oxidization temperature is 135 DEG C, and throughput is 0.30m
3/ (Kg.h), under these process conditions, the PV value (peroxide value) recording this suet is 349.342 meq/Kg, AV value (anisidine value) be 192.658, S value (acid number) is 2.108 mgKOH/g, prepares oxidation suet;
(5) preparation of mutton taste flavor material: % by weight percentage, the oxidation suet utilizing above-mentioned steps to prepare and corn protein powder enzymolysis liquid or zeins enzymolysis liquid are primary raw material, add in corn protein powder enzymolysis liquid 88% or zeins enzymolysis liquid simultaneously the oxidation suet of 5%, 1.3% L-cysteine hydrochloride, the VB1 of 0.5%, methionine, 2% sodium chloride and the 3%D-wood sugar of 0.2% carry out Maillard reaction, reaction temperature is 120 DEG C, the initial pH of reaction is 6.5, reaction time is 2h, prepares mutton taste flavor material.
Two kinds of mutton taste flavor material are prepared as follows according to the above-mentioned employing suet controlled oxidization preparation method provided:
% by weight percentage, mutton taste flavor material contain 5% oxidation suet, 1.3% L-cysteine hydrochloride, 0.5% VB1,0.2% methionine, 2% sodium chloride, 3%D-wood sugar and 88% corn protein powder enzymolysis liquid.
% by weight percentage, mutton taste flavor material contain 5% oxidation suet, 1.3% L-cysteine hydrochloride, 0.5% VB1,0.2% methionine, 2% sodium chloride, 3%D-wood sugar and 88% zeins enzymolysis liquid.
embodiment three: suet controlled oxidization prepares the optimization of process conditions of mutton taste flavor material
Utilize enzymolysis liquid to carry out Maillard reaction, determine comparatively optimal conditions according to sensory evaluation scores.Adopt the scheme that embodiment two provides, enzymolysis liquid is 90%, wood sugar is for being 3%, Cys is 2%, oxidation suet is 5%, under this condition, utilizes Orthogonal Optimization Test to be optimized Maillard reaction temperature, time and initial pH, using sensory evaluation scores as evaluation index, factor level table and the results are shown in Table 4 ~ 6.
The factor level table of table 4 reaction condition
Table 5 mutton taste flavor material condition Three factors-levels orthogonal arrage and result
Sequence number |
A temperature/DEG C |
B time/h |
C pH |
D is blank |
Score value |
1 |
110 |
1.0 |
6.0 |
-1 |
63 |
2 |
110 |
2.0 |
6.5 |
0 |
78 |
3 |
110 |
3.0 |
7.0 |
1 |
72 |
4 |
120 |
1.0 |
6.5 |
1 |
87 |
5 |
120 |
2.0 |
7.0 |
-1 |
92 |
6 |
120 |
3.0 |
6.0 |
0 |
82 |
7 |
130 |
1.0 |
7.0 |
0 |
68 |
8 |
130 |
2.0 |
6.0 |
1 |
69 |
9 |
130 |
3.0 |
6.5 |
-1 |
78 |
K1 |
71.000 |
72.667 |
71.333 |
77.667 |
|
K2 |
87.000 |
79.667 |
81.000 |
76.000 |
|
K3 |
71.667 |
77.333 |
77.333 |
76.000 |
|
R |
16.000 |
7.000 |
9.667 |
1.667 |
|
Table 6 mutton taste flavor material condition optimizing analysis of variance table
Factor |
Variance quadratic sum |
The free degree |
F ratio |
F critical value |
Conspicuousness |
Temperature |
491.556 |
2 |
88.473 |
19.000 |
* |
Time |
76.222 |
2 |
13.719 |
19.000 |
|
pH |
42.889 |
2 |
25.718 |
19.000 |
* |
Error |
5.560 |
2 |
|
|
|
From Orthogonal Optimization Test result and the intuitive analysis table 4 of Mutton Flavor material process optimization, R value: temperature >pH> temperature, namely being temperature to the factor that the flavor effect of mutton taste flavor material is maximum, is secondly pH and time; From the analysis of variance table 5 of the Orthogonal Optimization Test result of Mutton Flavor material process optimization, temperature and the flavor effect of pH to mutton taste flavor material remarkable.Known by table 6, the optimum combination of the condition of mutton taste flavor material Maillard reaction is A2C2B2, and namely reaction temperature is 120 DEG C, and the initial pH of reaction is 6.5, and the reaction time is 2h.
By the optimised process adopting single factor test and Orthogonal Optimization Test to determine alkali protease enzymolysis corn protein powder be concentration of substrate 6%, enzyme concentration is 3.0%, temperature is 55 DEG C, the time is 2.0h, pH is 10.0, carry out demonstration test under this condition, the degree of hydrolysis obtaining corn protein powder is 31.17%; The optimum combination of the condition of Maillard reaction is A2C2B2, and namely reaction temperature is 120 DEG C, and the initial pH of reaction is 6.5, and the reaction time is 2h.
embodiment four: the factor of influence single factor experiment of suet controlled oxidization
AV value (anisidine value), PV value (peroxide value) and S value (acid number) adopt existing known technology GB/T 24304-2009, GB/T 5538-2005 and GB/T 5530-2005 to measure respectively.
(1) temperature impact that suet is oxidized
See table 7 with to figure 2 depicts fixing throughput be 0.25m3/ (Kg.h), the controlled oxidization time is 3h, under temperature is respectively 100 DEG C, 115 DEG C, 125 DEG C, 135 DEG C, 145 DEG C, 155 DEG C and 165 DEG C of conditions, temperature is on the impact of suet oxidation index PV value (peroxide value), AV value (anisidine value) and S value (acid number).
Table 7 temperature affects result to PV, AV and S value
Temperature (DEG C) |
PV value/meq.Kg
-1 |
AV value |
S value/mgKOH.g
-1 |
Sensory evaluation scores |
Fragrance |
100 |
139.895 |
99.357 |
1.453 |
73 |
Light suet is fragrant |
115 |
193.578 |
113.274 |
1.487 |
72 |
Suet is fragrant |
125 |
246.251 |
165.239 |
1.603 |
75 |
Suet is fragrant |
135 |
367.679 |
185.537 |
2.449 |
89 |
Dense fat fragrance, light smell of mutton |
145 |
320.872 |
178.143 |
2.562 |
87 |
Suet fragrance, light smell of mutton |
155 |
298.543 |
157.349 |
8.573 |
78 |
Light penetrating odor |
165 |
287.876 |
148.974 |
12.305 |
70 |
Penetrating odor |
As can be seen from the result of table 7 and accompanying drawing 2, in 100 DEG C ~ 135 DEG C, PV and AV value increases with the rising of temperature, but the variation tendency of AV value is more slow, PV and AV value has a peak value 135 DEG C time; Within the scope of 135 DEG C ~ 165 DEG C, PV and AV value raises with temperature and reduces, and PV value significantly reduces, and the variation tendency of AV value is more slow; PV value obviously reduces, and this mainly raises due to temperature, and peroxide at high temperature easily decomposes, and not easily puts aside.AV value raises with temperature and slowly reduces, and its reason may be the rising along with temperature, and many carbonyls are polymerized to large molecule or are cracked into the small-molecule substance of highly volatile.In 100 DEG C ~ 145 DEG C, S value variation with temperature is comparatively slow, and in 145 DEG C ~ 165 DEG C, S value raises with temperature and increases sharply.Integrated sensory's scoring and odor characteristic can the initial setting comparatively suitable temperature with higher PV, AV and lower S value be 135 DEG C ~ 145 DEG C.
(2) time impact that suet is oxidized
See table 8 with to figure 3 depicts fixing throughput be 0.25m3/ (Kg.h), temperature is under 125 DEG C of conditions, controlled oxidization 0 h, 1 h, 2 h, 3 h, 4 h, 5 h and 6 h respectively, the time is on the impact of suet oxidation index PV value (peroxide value), AV value (anisidine value) and S value (acid number).
Table 8 time affects result to PV, AV and S value
Time/h |
PV value/meq.Kg
-1 |
AV value |
S value/mgKOH.g
-1 |
Sensory evaluation scores |
Fragrance |
0.0 |
5.086 |
4.249 |
0.521 |
58 |
Sheep smell of mutton |
1.0 |
89.274 |
12.436 |
0.972 |
67 |
Weak suet is fragrant |
2.0 |
163.351 |
98.783 |
1.375 |
73 |
Suet is fragrant |
3.0 |
226.251 |
155.239 |
1.503 |
87 |
Suet fragrance, light smell of mutton |
4.0 |
242.139 |
189.452 |
2.469 |
89 |
Suet fragrance, light smell of mutton |
5.0 |
335.748 |
247.137 |
8.932 |
76 |
Suet is fragrant, weak burnt odor |
6.0 |
486.652 |
251.328 |
11.435 |
70 |
Penetrating odor |
As can be seen from the result of table 8 and accompanying drawing 3, in 0h ~ 6h, PV, AV and S value increase in time and increasing, the variation tendency of PV and AV value in 0h ~ 4h is close, and in 4h ~ 6h, PV value increases rapidly, and the increase of AV value eases up.In 0h ~ 4h, S value changes in time and eases up, and in 4h ~ 6h, S value changes more violent in time.These variation tendencies mainly because along with the prolongation of oxidization time, cause the result that free fatty and peroxide increase.Integrated sensory's scoring and odor characteristic can be 3h ~ 4h initial setting comparatively suitable oxidation time with higher PV, AV and lower S value.
(3) throughput impact that suet is oxidized
See table 9 with to figure 4 depicts fixed temperature be 125 DEG C, the controlled oxidization time is 3 h, under throughput is respectively 0.15m3/ (Kg.h), 0.20m3/ (Kg.h), 0.25m3/ (Kg.h), 0.30m3/ (Kg.h), 0.35m3/ (Kg.h), 0.40m3/ (Kg.h), 0.45m3/ (Kg.h) condition, throughput is on the impact of suet oxidation index PV value (peroxide value), AV value (anisidine value) and S value (acid number).
Table 9 throughput affects result to PV, AV and S value
Throughput/m
3.(Kg.h)
-1 |
PV value/meq.Kg
-1 |
AV value |
S value/mgKOH.g
-1 |
Sensory evaluation scores |
Fragrance |
0.15 |
107.562 |
89.237 |
0.0783 |
69 |
Weak suet is fragrant |
0.20 |
149.783 |
102.238 |
1.248 |
71 |
Weak suet is fragrant |
0.25 |
256.251 |
151.239 |
1.643 |
76 |
Suet is fragrant |
0.30 |
253.126 |
192.157 |
2.019 |
87 |
Pure and fresh suet is fragrant |
0.35 |
262.189 |
199.458 |
2.357 |
86 |
Suet is fragrant |
0.40 |
289.146 |
210.345 |
7.357 |
80 |
Weak burnt odor |
0.45 |
300.013 |
247.243 |
11.672 |
75 |
Burnt odor |
Can find out that PV and AV value is close with the variation tendency of throughput from the result of table 9 and accompanying drawing 4, but when throughput is 0.15m3/ (Kg.h) ~ 0.25m3/ (Kg.h), PV value is precipitous compared with AV value increase trend, when 0.25 m3/ (Kg.h) ~ 0.45m3/ (Kg.h), PV with AV value variation tendency is similar.This is mainly because degree of oxidation improves constantly, and peroxide constantly decomposes, and can cause the unstability of measurement result like this.Also be likely flow velocity increase, PV and PAV decrease reason may be, faster air velocity very easily cause minute bubbles formed large bubble make air in time participate in reaction and overflow from liquid.The variation tendency of S value is: in 0.15m3/ (Kg.h) ~ 0.35m3/ (Kg.h) scope, tend towards stability; When 0.35m3/ (Kg.h) ~ 0.45m3/ (Kg.h), increase rapidly.Integrated sensory's scoring and odor characteristic can the initial setting more suitable throughput with higher PV, AV and lower S value be in 0.25 m3/ (Kg.h) ~ 0.35m3/ (Kg.h) scope.
The technique being determined suet controlled oxidization by above-mentioned single factor experiment is: controlled oxidization time 4.0h, and controlled oxidization temperature is 135 DEG C, and throughput is 0.30m3/ (Kg.h); Under more excellent process conditions, carry out demonstration test, demonstration test result is: PV value is 349.342 meq/Kg, AV value be 192.658, S value is 2.108 mgKOH/g.
embodiment five: the factor of influence Orthogonal Optimization Test of suet controlled oxidization
On the basis of single factor experiment, choose temperature, time and throughput Three factors, carry out the Orthogonal Optimization Test of Three factors-levels, and result and intuitive analysis table and analysis of variance table are in table 10 ~ 13.
Table 10 orthogonal experiments and analysis
(note: Rx, Ry, Rz represent the extreme difference of peroxide value, anisidine value and acid number respectively)
The analysis of variance table of table 11 pair PV value
Factor |
Variance quadratic sum |
The free degree |
F ratio |
F critical value |
Conspicuousness |
Temperature |
47501.708 |
2 |
205.552 |
19.000 |
* |
Time |
1641.371 |
2 |
7.103 |
19.000 |
|
Throughput |
306.166 |
2 |
1.325 |
19.000 |
|
Error |
231.090 |
2 |
|
|
|
The analysis of variance table of table 12 pair AV value
Factor |
Variance quadratic sum |
The free degree |
F ratio |
F critical value |
Conspicuousness |
Temperature |
1795.257 |
2 |
14.652 |
19.000 |
|
Time |
900.915 |
2 |
7.353 |
19.000 |
|
Throughput |
3494.240 |
2 |
28.518 |
19.000 |
* |
Error |
122.530 |
2 |
|
|
|
The analysis of variance table of table 13 pair S value
Factor |
Variance quadratic sum |
The free degree |
F ratio |
F critical value |
Conspicuousness |
Temperature |
0.133 |
2 |
33.250 |
19.000 |
* |
Time |
0.749 |
2 |
187.250 |
19.000 |
* |
Throughput |
0.011 |
2 |
2.750 |
19.000 |
|
Error |
0.000 |
2 |
|
|
|
From result and intuitive analysis table and analysis of variance table 10-13, the optimum process of higher peroxide value (PV) is A2B3C3; The optimum process of higher anisidine value (AV) is: C2A2B2; The optimum process of lower acid number (S) is: B1A1C3; Consider requirement oxidation suet and there is higher PV, AV value and lower S value, the optimum combination determined is: A2B3C2, namely the preferred process condition of suet oxidation test is: controlled oxidization time 4.0h, and controlled oxidization temperature is 135 DEG C, and throughput is 0.30m3/ (Kg.h).Under more excellent process conditions, carry out demonstration test, demonstration test result is: PV value is 349.342 meq/Kg, AV value be 192.658, S value is 2.108 mgKOH/g.
The technique being determined suet controlled oxidization by above-mentioned Orthogonal Optimization Test is: controlled oxidization time 4.0h, and controlled oxidization temperature is 135 DEG C, and throughput is 0.30m
3/ (Kg.h); Under more excellent process conditions, carry out demonstration test, demonstration test result is: PV value is 349.342 meq/Kg, AV value be 192.658, S value is 2.108 mgKOH/g.
embodiment six: the evaluation preparing mutton taste flavor material
1. subjective appreciation
Adopt the method for random sampling, form one 10 the scoring groups having each side representative figure to participate in, comprehensive grading is carried out to the flavor material that oxidation suet and Mei Lade break through, oxidation suet carries out comprehensive grading from color and luster (0-10 divides), odor type (0-30 divides), strong and weak (0-40 divides), remaining time (0-20 divides) and peculiar smell (-10-10 divides) five aspects, and Maillard reaction flavor material carries out comprehensive grading from color and luster (0-20 divides), odor type (0-30 divides), strong and weak (0-30 divides), remaining time (0-20 divides) four aspects.
2. the GC-MS of mutton taste flavor material analyzes
Headspace solid phase microextractiom is adopted to extract volatile ingredient, then with carrying out GC-MS analysis.
(1) extracting head is aging
By solid phase micro-extraction extraction head at the aging 10min of GC-MS injection port, injector temperature is 250 DEG C.
(2) SPME
Get 5mL sample and be placed in 25mL SPME Special sample bottle, cover tightly sample bottle cap, balance 10min in 50 DEG C of thermostat water baths after, the extracting head of solid phase micro-extraction device is inserted in sample bottle, release fiber head, make fiber head be placed in about 1cm above sample, headspace absorption 20min, regain fiber head subsequently, extract extracting head, extracting head is directly inserted GC-MS, release fiber head, 250 DEG C of desorb 10min, carry out GC-MS analysis.
(3) GC-MS condition
Chromatographic condition: capillary chromatographic column HP-5MS (30m × 0.25mm, 0.25 μm); Heating schedule: 40 DEG C keep 2min, are warming up to 220 DEG C, are warming up to 250 DEG C with 2 DEG C/min with 10 DEG C/min, keep 5min; Carrier gas (He) flow velocity is 1.0mL/min, injector temperature 250 DEG C; Splitless injecting samples.
Mass Spectrometry Conditions: electronics bombardment (EI) ion gun; Emitted energy 70eV; Ion source temperature 200 DEG C; Interface temperature 250 DEG C; ACQ mode: Scan; Sweep speed: 769u/s; Mass scan range: 33-450amu.
(4) data processing
Data processing: Data Processing in Experiment is completed by computer software, unknown compound is machine examination rope as calculated, composes storehouse (107k Compounds) and Wiley with NIST simultaneously and composes storehouse (320k Compounds, version 6.0) and match.
The GC-MS analysis result of mutton taste flavor material is in table 14.
Table 14 mutton taste flavor material GC-MS Components identification table
Sequence number |
Components Name |
Content |
1 |
(z)-9-hexadecene-1-alcohol |
1.99 |
2 |
1-heptadecanol |
3.32 |
3 |
Axerophthal |
10.06 |
4 |
2,3,6-tri chlorobenzaldehyde |
0.06 |
5 |
5,7-dimethyl-ALPHA-tetralone |
0.27 |
6 |
17-glycolic acid cortex (steroid) ketone |
6.68 |
7 |
Aldosterone |
0.59 |
8 |
1-(4-acetoxy-3-anisyl) ethyl ketone |
0.03 |
9 |
Equilin |
0.02 |
10 |
Metacortandracin |
0.41 |
11 |
Cortisone |
0.17 |
12 |
Stearic acid |
8.54 |
13 |
Palmitic acid |
0.19 |
14 |
Neocholan |
0.39 |
15 |
OA methyl esters |
58.12 |
16 |
Vitamin A acetic acid esters |
6.33 |
17 |
Tetradecylic acid 14 ester |
0.05 |
18 |
Methyl hexadecanoate |
0.29 |
19 |
2-pi-allyl-6-methylphenol |
0.22 |
20 |
12,13-dihydro-7H-dibenzo (A, G) carbazoles |
1.40 |
21 |
Other |
0.87 |
GC-MS analyze identify 20 flavor substances altogether, content come first 5 be respectively 58.12% OA methyl esters, the axerophthal of 10.06%, stearic acid, 17-glycolic acid cortex (steroid) ketone of 6.68%, the vitamin A acetic acid esters of 6.33% of 8.54%.
GC-MS analyzes and identifies 20 flavor substances altogether, wherein alcohols 2 kinds, aldehydes 2 kinds, ketone 7 kinds, acids 3 kinds, ester class 4 kinds, each a kind of phenol, carbazole.
Carried out SPME-GC-MS analysis to mutton soup, formula I and formula II, qualification obtains 26 kinds of flavor substances, wherein alkanes 2 kinds, alcohols 3 kinds, aldehydes 2 kinds, ketone 8, acids 4 kinds, ester class 4 kinds, each a kind of benzene, phenol carbazole altogether; For determining the acceptability of formula I and formula II flavor material further, adopting the method for Comprehensive Evaluation, utilizing fuzzy matrix to carry out sense organ Comprehensive Assessment.The comprehensive evaluation result of fuzzy matrix shows to be respectively 69% and 72% to the ratio of liking of formula I and formula II, and formula II is better than formula I, and two kinds of formulas all can be used as the formula of mutton taste flavor material, economically consider, formula I is optimum formula; Formula I component be 5% oxidation suet, the L-cysteine hydrochloride of 1.3%, the VB1 of 0.5%, the methionine of 0.2%, 2% sodium chloride, 3%D-wood sugar and 88% corn protein powder enzymolysis liquid.
3. the fuzzy matrix assessment of mutton taste flavor material acceptability
The first step, carries out sensory evaluation one by one to the single factor test affecting flavor material acceptability, determine that people's factor of often planting ' is delithted with ', ' liking ', ' not liking ', ' not liking ' ratio.Second step, determine the weight of often kind of single factor test in this judge of acceptance, weight sum is 1.3rd step, is blurring mapping B=A.R, B illustrate the Receptive Comprehensive Evaluation result of people to flavor material.
By adopting the method for random sampling, form the evaluation group of each side representative figure of 30 people, and peculiar smell strong and weak to the color and luster of flavor material, odor type, local flavor is evaluated, by being delithted with, preferring, do not like and do not like determining grade, calculating probability respectively.
The probability be delithted with, preferred, do not like and do not like is respectively: A color and luster=[0.6 0.3 0.1 0],
A odor type=[0.4 0.2 0.3 0.1], A power=[0.4 0.3 0.2 0.1], A peculiar smell=[0.3 0.3 0.2 0.2]
Above-mentioned four monofactorial evaluation results are write as matrix:
Secondly, determine the weight of factor, the color and luster of flavor material, odor type, local flavor weight that is strong and weak and peculiar smell four factors is respectively 20%, 30%, 30% and 20%.Obtain weight A=[0.2 0.3 0.3 0.2]
Finally, Comprehensive Evaluation B=A is carried out.R
Namely there is the people of 42% to be delithted with, the people of 27% likes, the people of 21% does not like, the people of 10% do not like; The comprehensive evaluation result of fuzzy matrix shows that people like ratio to be 69% to it.
The comprehensive evaluation result of fuzzy matrix shows that the like ratio of people to the mutton taste flavor material of the formula I that the present invention determines is 69%.
Visible by above-described embodiment, the present invention utilizes enzymatic isolation method to prepare corn protein powder enzymolysis liquid, with zein enzymolysis liquid, oxidation suet and wood sugar are primary raw material, add sodium chloride, vitamin B1, cysteine hydrochloride, methionine carries out Maillard reaction and prepares Novel sheep meat flavour flavor material, this novel meat flavor material has fat perfume (or spice), meat is fragrant and roasting fragrant, full and the natural sense of tool, both the mouthfeel of people can have been met, be unlikely to again people is got fat, simultaneously also for the deep processing and utilization of corn protein powder provides an effective way, add the added value of corn protein powder.