CN107300568A - The method for measuring new fresh mushroom glass transition temperature - Google Patents
The method for measuring new fresh mushroom glass transition temperature Download PDFInfo
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- CN107300568A CN107300568A CN201710412027.5A CN201710412027A CN107300568A CN 107300568 A CN107300568 A CN 107300568A CN 201710412027 A CN201710412027 A CN 201710412027A CN 107300568 A CN107300568 A CN 107300568A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N25/00—Investigating or analyzing materials by the use of thermal means
- G01N25/02—Investigating or analyzing materials by the use of thermal means by investigating changes of state or changes of phase; by investigating sintering
- G01N25/12—Investigating or analyzing materials by the use of thermal means by investigating changes of state or changes of phase; by investigating sintering of critical point; of other phase change
Abstract
The invention discloses a kind of method for measuring new fresh mushroom glass transition temperature, step includes：Drying mushroom is milled to mushroom powder；The mushroom sample of different water cut processed；The glass transition temperature of dsc measurement mushroom containing non-f reezing water；The glass transition temperature of dsc measurement mushroom containing freeze water；Obtain glass transition temperature curve；Obtain frozen temperature；Build the state diagram that frozen temperature, glass transition temperature curve and maximum Freeze concentration state constitute mushroom；It is determined that freezing outlet temperature value T under maximum Freeze concentration statem', thus point does vertical line in state diagram, and with the glass transition temperature curve intersection, intersection point is mushroom feature glass transition temperature.Because the moisture content of new fresh mushroom is higher, its glass transition temperature can not be directly obtained with DSC apparatus measures, and by the method for state diagram, mushroom feature glass transition temperature can be obtained indirectly.
Description
Technical field
The invention belongs to food processing technology field, it is related to the storage and processing of fruit or vegetables, more particularly to one kind
The method for measuring new fresh mushroom glass transition temperature.
Background technology
According to the literature, Chinese mushroom production accounts for more than the 70% of world wide production.Mushroom is rich in multiple nutritional components
And functional components, the effects such as with antitumor, reducing blood lipid, it is described as " queen in mushroom ".Because new fresh mushroom moisture content is up to
More than 90%, easily rotted after adopting, so as to cause very big economic loss to production and storing.It is logical both at home and abroad at present
Frequently with dry or Refrigeration Technique preservation mushroom, however, in both processing or storage, easily forming non-equilibrium nothing and determining
Form, unstability when causing the mushroom to preserve.Therefore, glassy state storage theory is applied in the processing and storage of mushroom,
Theoretical foundation and technical support are provided to the stability for raising mushroom quality.
Glass transition temperature can be used as processing or the standard of storage-stable.When glass transition occurs for system,
Endothermic curve occurs one " step " that glass transition is not a point, but a regional extent.According to amorphous state without fixed
It, by the difference of temperature province can be divided into three kinds of mechanical states by the feature that the mechanical property of shape polymer is varied with temperature：
Glassy state, elastomeric state (also known as rubbery state) and viscous state.Transformation between glassy state and rubbery state is referred to as glass transition, right
The transition temperature answered is glass transition temperature Tg.When food is preserved below glass transition temperature, the molecule of system
Diffusion rate is smaller, thus food be in glassy state when be not susceptible to chemical reaction, can extend the shelf life.On the contrary, when storage temperature
When degree is more than glass transition temperature, system is in rubbery state, and molecular mobility increase causes the adverse reaction of some in food
Occur.Therefore, in food processing or storage, it should try one's best and be maintained under glassy state.When the moisture content of food is relatively low, its
Glass transition temperature can be obtained directly by apparatus measures, i.e. Tg.And when the moisture content of food is higher, due to freezing speed
Rate is relatively slow, is extremely difficult to accurately maximum Freeze concentration state；And, can not be direct due to the limitation of instrumental sensitivity
Experiment measurement is obtained, but feature glass transition temperature (T can be obtained by state diagramg') value.The state diagram description of food
Relation between the different conditions of food and the moisture content of material and temperature, it can predict stability during food storage,
And suitable temperature and humidity condition can be provided for the freezing and dry processing of food.State diagram, which is generally comprised, freezes song
Line, glass transition temperature curve and maximum Freeze concentration state.For new fresh mushroom, because its moisture content is higher
(0.90g/g wet basis), the method for availability status figure obtains mushroom feature glass transition temperature, i.e. Tg′.This method is calibrated
Really, because Tg' it is corresponding be glass transition temperature under maximum Freeze concentration state.
The content of the invention
The problem of for being previously mentioned, the invention provides a kind of method for measuring new fresh mushroom glass transition temperature, step
Suddenly include：
1) it is freeze-dried
New fresh mushroom is drying using the method progress of freeze-drying, drying mushroom is then milled to mushroom powder；
2) the mushroom sample of different water cut processed
Obtained mushroom powder is placed in the closed container equipped with different saturated salt solutions, is then placed within insulating box
Balance, carries out adsorption experiment, and the mushroom sample of different water cut is made；
3) dsc measurement contains the glass transition temperature of non-f reezing water (moisture content is relatively low) mushroom
Double scanning imaging systems：Take moisture content be not higher than 0.2 mushroom sample drop to -85 from 25 DEG C with 5 DEG C/min speed~-
120 DEG C, 10min is kept, then 60 DEG C are warming up to 5 DEG C/min speed, then -85 are dropped to from 60 DEG C of speed with 5 DEG C/min
~-120 DEG C, 60 DEG C then are warming up to 5 DEG C/min speed again, the glass of the sample of mushroom containing non-f reezing water is gone out by dsc measurement
Glass transition temperature initial value, glass transition temperature midrange and Tg endpoint value；
4) dsc measurement contains the glass transition temperature of freeze water (moisture content is higher) mushroom
The heat flow curve of mushroom is tentatively obtained using DSC scanning imaging systems first, glass transition temperature is found and freezes end
Point temperature (Tm') position, then further using cycle of annealing measure glass transition temperature；
41) preliminary scan program：Mushroom sample of the moisture content higher than 0.2 is taken to drop to -85 from 25 DEG C of speed with 5 DEG C/min
~-120 DEG C, 10min is kept, then 40 DEG C is raised to from -85~-120 DEG C with 5 DEG C/min speed again, goes out to contain by dsc measurement
Glass transition temperature initial value, glass transition temperature midrange and the Tg endpoint of freeze water mushroom sample
Value, solidification point and freeze outlet temperature value Tm′；
42) cycle of annealing：
Dsc measurement cycle of annealing is that mushroom sample drops to -85~-120 DEG C from 25 DEG C of speed with 5 DEG C/min, then with 5
DEG C/min speed is raised to (Tm' -1) certain time DEG C, is kept；Then again with 5 DEG C/min speed from (Tm' -1) DEG C -85 are dropped to
~-120 DEG C, then it is raised to 40 DEG C with 5 DEG C/min speed so that glass transition reaches maximum Freeze concentration state and elimination
Exothermic peak；
5) glass transition temperature curve is obtained
Mushroom glass transition temperature is simulated with the change of moisture content, and vitrifying is obtained using nonlinear regression and fitting
Transition temperature curve；
6) frozen temperature is obtained
Mushroom solidification point is simulated with the change of moisture content, and it is bent to obtain solidification point using nonlinear regression and fitting
Line；
7) state that frozen temperature, glass transition temperature curve and maximum Freeze concentration state constitute mushroom is built
Figure；
8) determine to freeze outlet temperature value T under maximum Freeze concentration statem', and marked on frozen temperature
The point for freezing outlet temperature value under maximum Freeze concentration state, thus puts and does vertical line, with the glass transition temperature curve
Intersecting, intersection point is mushroom feature glass transition temperature.
Preferred scheme is：Mushroom glass transition temperature uses Gordon-Taylor (GT) equation with the change of moisture content
Simulation, glass transition temperature curve is obtained using Origin softwares (version 8.6) nonlinear regression and fitting.
Preferred scheme is：Mushroom solidification point uses Clausius-Clapeyron equation simulations with the change of moisture content,
Frozen temperature is obtained using Origin softwares (version 8.6) nonlinear regression and fitting.
Preferred scheme is：In cycle of annealing, (T is raised to 5 DEG C/min speedm' -1) 30min or 60min DEG C, is kept.
Preferred scheme is：The glass transition temperature of dsc measurement mushroom containing non-f reezing water is using double scanning imaging system measurements.
Preferred scheme is：It is more than 0.94 sample for water activity, distilled water can be added directly into equipped with mushroom
In the measuring cup of powder, 24h is balanced at 4 DEG C.
Beneficial effects of the present invention are as follows：
(1) because the moisture content of new fresh mushroom is higher, its glass transition temperature can not directly be obtained with DSC apparatus measures
Arrive, and by the method for state diagram, mushroom feature glass transition temperature can be obtained indirectly.
(2) glass transition temperature of mushroom can be as processing or the standard of storage-stable, when mushroom is in glass
When changing (glassy state) storage below transition temperature, its quality can be preferably kept, and bioactive substance in mushroom can be kept
Stability, so as to improve the nutritional quality of herb of Thinleaf GLossogyne products.
(3) when mushroom is preserved or processed under glassy state, the quality of herb of Thinleaf GLossogyne products can not only be improved, moreover it is possible to extend it
Storage period, so as to bring profit for mushroom processing enterprise.
(4) glass transition temperature of mushroom can as storage-stable criterion, when mushroom be in glassy state
Shi Pinzhi relatively stablize, therefore need not as far as possible reduction temperature and preservation freezing mushroom, it is only necessary to reach glassy state, so as to
Think that enterprise saves the energy.
(5) method of the invention is with low cost, simple to operate.
Brief description of the drawings
Fig. 1 is the state diagram of mushroom.
Embodiment
The present invention is described in further detail below, to make those skilled in the art being capable of evidence with reference to specification word
To implement.
It should be appreciated that such as " having ", "comprising" and " comprising " term used herein do not allot one or many
The presence or addition of individual other elements or its combination.
Embodiment 1
The method for present embodiments providing a kind of new fresh mushroom glass transition temperature of amount, step includes：
1) it is freeze-dried
New fresh mushroom is drying using the method progress of freeze-drying, drying mushroom is then milled to mushroom powder, it is cold
Lyophilized drying method can preferably keep the quality and nutritional ingredient of material, and can preferably protect compared with other drying means
Stay the structure of raw material；
2) the mushroom sample of different water cut processed
Obtained mushroom powder is placed in the closed container equipped with different saturated salt solutions, is then placed within insulating box
Balance, carries out adsorption experiment, and the mushroom sample of different water cut is made, and 0.94 sample is more than for water activity, can be by
Distilled water is added directly into the measuring cup equipped with mushroom powder, balances 24h at 4 DEG C, the moisture content of mushroom sample can basis
Of poor quality calculating of the sample before and after balance is obtained, and the water activity of the saturated salt solution is as shown in table 1；
3) glass transition temperature of dsc measurement mushroom containing non-f reezing water
The glass transition temperature of dsc measurement mushroom containing non-f reezing water is using double scanning imaging system measurements, in order to disappear
Except the enthalpy of the unformed sample release in first time scanning, scanned by second, can be than more clearly obtaining vitrifying
The step of step of transformation, glass transition temperature of dsc measurement mushroom containing non-f reezing water is：Moisture content is taken to be not higher than 0.2
Mushroom sample drops to -85 DEG C from 25 DEG C with 5 DEG C/min speed, keeps 10min, is then warming up to 60 with 5 DEG C/min speed
DEG C, then -85 DEG C are dropped to from 60 DEG C of speed with 5 DEG C/min, 60 DEG C then are warming up to 5 DEG C/min speed again, is surveyed by DSC
Measure the glass transition temperature initial value, glass transition temperature midrange and glass transition of the sample of mushroom containing non-f reezing water
Temperature end point value；
4) glass transition temperature of dsc measurement mushroom containing freeze water
The heat flow curve of mushroom is tentatively obtained using DSC scanning imaging systems first, glass transition temperature is found and freezes end
Point temperature (Tm') position, then further using cycle of annealing measure glass transition temperature；
41) preliminary scan program：Mushroom sample of the moisture content higher than 0.2 is taken to drop to -85 from 25 DEG C of speed with 5 DEG C/min
DEG C, 10min is kept, 40 DEG C are then raised to from -85 DEG C with 5 DEG C/min speed again, the sample of mushroom containing freeze water is gone out by dsc measurement
The glass transition temperature initial values of product, glass transition temperature midrange and Tg endpoint value, solidification point
With freeze outlet temperature value Tm′；
42) cycle of annealing：
The purpose of cycle of annealing is the step for increasing glass transition, reaches maximum Freeze concentration state and eliminates heat release
Peak, compares and is clearly observed glass transition, and annealing enables to ice crystal sufficient crystallising, and material molecule is reset, so that
Free volume is set to try one's best maximization, the step degree of heat enthalpy value when can finally make generation glass transition is relatively large, and DSC is surveyed
Amount cycle of annealing is that mushroom sample drops to -85 DEG C from 25 DEG C of speed with 5 DEG C/min, then is raised to (T with 5 DEG C/min speedm′-
1) 30min DEG C, is kept；Then again with 5 DEG C/min speed from (Tm' -1) DEG C -85 DEG C are dropped to, then with 5 DEG C/min speed liter
To 40 DEG C；
5) glass transition temperature curve is obtained
Mushroom glass transition temperature (sample containing non-f reezing water) is as shown in table 2 with the change of moisture content, can use
Gordon-Taylor (GT) equation simulation, vitrifying is obtained using Origin softwares (version 8.6) nonlinear regression and fitting
Transition temperature curve；
6) frozen temperature is obtained
Mushroom solidification point (containing water sample is freezed) is as shown in table 3 with the change of moisture content, and mushroom solidification point is with aqueous
The change of rate uses Clausius-Clapeyron equation simulations, utilizes Origin softwares (version 8.6) nonlinear regression
Fitting obtains frozen temperature, from table 3 it can be seen that Tm' reduced with the increase of total solid content, when solid material
Measure fraction Xs>During 0.30g/g wet basis, TmThe change of ' value is smaller, close to constant.Total solid content is 0.41 to 0.72g/
When between wet basis, the T of maximum Freeze concentration statem' average value is -33.4 DEG C；
7) state that frozen temperature, glass transition temperature curve and maximum Freeze concentration state constitute mushroom is built
Figure, as shown in Figure 1；
8) determine to freeze outlet temperature value under maximum Freeze concentration state, and mark on frozen temperature maximum
The point for freezing outlet temperature value under Freeze concentration state, thus point do vertical line, and the glass transition temperature curve intersection,
Intersection point is -53.2 DEG C of mushroom feature glass transition temperature.
Embodiment 2
The method for present embodiments providing a kind of new fresh mushroom glass transition temperature of amount, step includes：
1) it is freeze-dried
New fresh mushroom is drying using the method progress of freeze-drying, drying mushroom is then milled to mushroom powder, it is cold
Lyophilized drying method can preferably keep the quality and nutritional ingredient of material, and can preferably protect compared with other drying means
Stay the structure of raw material；
2) the mushroom sample of different water cut processed
Obtained mushroom powder is placed in the closed container equipped with different saturated salt solutions, 25 DEG C of perseverance is then placed within
Balanced 30 days in incubator, carry out adsorption experiment, the mushroom sample of different water cut is made, 0.94 sample is more than for water activity
Distilled water, can be added directly into the measuring cup equipped with mushroom powder by product, and 24h, the moisture content of mushroom sample are balanced at 4 DEG C
It can be obtained according to of poor quality calculating of the sample before and after balance, the water activity of the saturated salt solution is as shown in table 1；
3) glass transition temperature of dsc measurement mushroom containing non-f reezing water
The glass transition temperature of dsc measurement mushroom containing non-f reezing water is using double scanning imaging system measurements, in order to disappear
Except the enthalpy of the unformed sample release in first time scanning, scanned by second, can be than more clearly obtaining vitrifying
The step of step of transformation, glass transition temperature of dsc measurement mushroom containing non-f reezing water is：Moisture content is taken to be not higher than 0.2
Mushroom sample drops to -120 DEG C from 25 DEG C with 5 DEG C/min speed, keeps 10min, is then warming up to 60 with 5 DEG C/min speed
DEG C, then -120 DEG C are dropped to from 60 DEG C of speed with 5 DEG C/min, 60 DEG C then are warming up to 5 DEG C/min speed again, passes through DSC
The glass transition temperature initial value, glass transition temperature midrange and vitrifying for measuring the sample of mushroom containing non-f reezing water turn
Temperature end point values；
4) glass transition temperature of dsc measurement mushroom containing freeze water
The heat flow curve of mushroom is tentatively obtained using DSC scanning imaging systems first, glass transition temperature is found and freezes end
Point temperature (Tm') position, then further using cycle of annealing measure glass transition temperature；
41) preliminary scan program：Take mushroom sample of the moisture content higher than 0.2 drop to from 25 DEG C of speed with 5 DEG C/min-
120 DEG C, 10min is kept, 40 DEG C are then raised to from -120 DEG C with 5 DEG C/min speed again, gone out by dsc measurement fragrant containing freeze water
Glass transition temperature initial value, glass transition temperature midrange and the Tg endpoint value of mushroom sample, freeze
Temperature and freeze outlet temperature value Tm′；
42) cycle of annealing：
The purpose of cycle of annealing is the step for increasing glass transition, reaches maximum Freeze concentration state and eliminates heat release
Peak, compares and is clearly observed glass transition, and annealing enables to ice crystal sufficient crystallising, and material molecule is reset, so that
Free volume is set to try one's best maximization, the step degree of heat enthalpy value when can finally make generation glass transition is relatively large, and DSC is surveyed
Amount cycle of annealing is that mushroom sample drops to -120 DEG C from 25 DEG C of speed with 5 DEG C/min, then is raised to 5 DEG C/min speed
(Tm' -1) 60min DEG C, is kept；Then again with 5 DEG C/min speed from (Tm' -1) DEG C -120 DEG C are dropped to, then with 5 DEG C/min speed
Degree is raised to 40 DEG C；
5) glass transition temperature curve is obtained
Mushroom glass transition temperature is as shown in table 2 with the change of moisture content, can use Gordon-Taylor (GT) equation
Simulation, glass transition temperature curve is obtained using Origin softwares (version 8.6) nonlinear regression and fitting；
6) frozen temperature is obtained
Mushroom solidification point (containing water sample is freezed) is as shown in table 3 with the change of moisture content, and mushroom solidification point is with aqueous
The change of rate uses Clausius-Clapeyron equation simulations, utilizes Origin softwares (version 8.6) nonlinear regression
Fitting obtains frozen temperature, from table 3 it can be seen that Tm' reduced with the increase of total solid content, when solid material
Measure fraction Xs>During 0.30g/g wet basis, TmThe change of ' value is smaller, close to constant.Total solid content is 0.41 to 0.72g/
When between wet basis, the T of maximum Freeze concentration statem' average value is -33.4 DEG C；
7) state that frozen temperature, glass transition temperature curve and maximum Freeze concentration state constitute mushroom is built
Figure, as shown in Figure 1；
8) determine to freeze outlet temperature value under maximum Freeze concentration state, and mark on frozen temperature maximum
The point for freezing outlet temperature value under Freeze concentration state, thus point do vertical line, and the glass transition temperature curve intersection,
Intersection point is -53.2 DEG C of mushroom feature glass transition temperature.
Embodiment 3
The method for present embodiments providing a kind of new fresh mushroom glass transition temperature of amount, step includes：
1) it is freeze-dried
New fresh mushroom is drying using the method progress of freeze-drying, drying mushroom is then milled to mushroom powder, it is cold
Lyophilized drying method can preferably keep the quality and nutritional ingredient of material, and can preferably protect compared with other drying means
Stay the structure of raw material；
2) the mushroom sample of different water cut processed
Obtained mushroom powder is placed in the closed container equipped with different saturated salt solutions, 25 DEG C of perseverance is then placed within
Balanced 30 days in incubator, carry out adsorption experiment, the mushroom sample of different water cut is made, 0.94 sample is more than for water activity
Distilled water, can be added directly into the measuring cup equipped with mushroom powder by product, and 24h, the moisture content of mushroom sample are balanced at 4 DEG C
It can be obtained according to of poor quality calculating of the sample before and after balance, the water activity of the saturated salt solution is as shown in table 1；
3) glass transition temperature of dsc measurement mushroom containing non-f reezing water
The glass transition temperature of dsc measurement mushroom containing non-f reezing water is using double scanning imaging system measurements, in order to disappear
Except the enthalpy of the unformed sample release in first time scanning, scanned by second, can be than more clearly obtaining vitrifying
The step of step of transformation, glass transition temperature of dsc measurement mushroom containing non-f reezing water is：Moisture content is taken to be not higher than 0.2
Mushroom sample drops to -90 DEG C from 25 DEG C with 5 DEG C/min speed, keeps 10min, is then warming up to 60 with 5 DEG C/min speed
DEG C, then -90 DEG C are dropped to from 60 DEG C of speed with 5 DEG C/min, 60 DEG C then are warming up to 5 DEG C/min speed again, is surveyed by DSC
Measure the glass transition temperature initial value, glass transition temperature midrange and glass transition of the sample of mushroom containing non-f reezing water
Temperature end point value；
4) glass transition temperature of dsc measurement mushroom containing freeze water
The heat flow curve of mushroom is tentatively obtained using DSC scanning imaging systems first, glass transition temperature is found and freezes end
Point temperature (Tm') position, then further using cycle of annealing measure glass transition temperature；
41) preliminary scan program：Mushroom sample of the moisture content higher than 0.2 is taken to drop to -90 from 25 DEG C of speed with 5 DEG C/min
DEG C, 10min is kept, 40 DEG C are then raised to from -90 DEG C with 5 DEG C/min speed again, the sample of mushroom containing freeze water is gone out by dsc measurement
The glass transition temperature initial values of product, glass transition temperature midrange and Tg endpoint value, solidification point
With freeze outlet temperature value Tm′；
42) cycle of annealing：
The purpose of cycle of annealing is the step for increasing glass transition, reaches maximum Freeze concentration state and eliminates heat release
Peak, compares and is clearly observed glass transition, and annealing enables to ice crystal sufficient crystallising, and material molecule is reset, so that
Free volume is set to try one's best maximization, the step degree of heat enthalpy value when can finally make generation glass transition is relatively large, and DSC is surveyed
Amount cycle of annealing is that mushroom sample drops to -90 DEG C from 25 DEG C of speed with 5 DEG C/min, then is raised to (T with 5 DEG C/min speedm′-
1) 30min DEG C, is kept；Then again with 5 DEG C/min speed from (Tm' -1) DEG C -90 DEG C are dropped to, then with 5 DEG C/min speed liter
To 40 DEG C；
5) glass transition temperature curve is obtained
Mushroom glass transition temperature (sample containing non-f reezing water) is as shown in table 2 with the change of moisture content, can use
Gordon-Taylor (GT) equation simulation, vitrifying is obtained using Origin softwares (version 8.6) nonlinear regression and fitting
Transition temperature curve；
6) frozen temperature is obtained
Mushroom solidification point (containing water sample is freezed) is as shown in table 3 with the change of moisture content, and mushroom solidification point is with aqueous
The change of rate uses Clausius-Clapeyron equation simulations, utilizes Origin softwares (version 8.6) nonlinear regression
Fitting obtains frozen temperature, from table 3 it can be seen that Tm' reduced with the increase of total solid content, when solid material
Measure fraction Xs>During 0.30g/g wet basis, TmThe change of ' value is smaller, close to constant.Total solid content is 0.41 to 0.72g/
When between wet basis, the T of maximum Freeze concentration statem' average value is -33.4 DEG C；
7) state that frozen temperature, glass transition temperature curve and maximum Freeze concentration state constitute mushroom is built
Figure, as shown in Figure 1；
8) determine to freeze outlet temperature value under maximum Freeze concentration state, and mark on frozen temperature maximum
The point for freezing outlet temperature value under Freeze concentration state, thus point do vertical line, and the glass transition temperature curve intersection,
Intersection point is -53.2 DEG C of mushroom feature glass transition temperature.
The water activity of 1 25 DEG C of saturated salt solutions of table
The glass transition temperature of the mushroom of table 2 (containing non-f reezing water sample)
Note：TgiFor glass transition temperature initial value, TgmFor glass transition temperature midrange, TgeFor glass transition
Temperature end point value.
The glass transition temperature of the mushroom of table 3 (containing water sample is freezed) and maximum Freeze concentration state
Note：" n.d. " represents to be not detected by.
TgiFor glass transition temperature initial value, TgmFor glass transition temperature midrange, TgeFor glass transition temperature
End point values.TFFor solidification point, Tm' it is to freeze outlet temperature.
Although embodiment of the present invention is disclosed as above, it is not restricted in specification and embodiment listed
With it can be applied to various suitable the field of the invention completely, can be easily for those skilled in the art
Other modification is realized, therefore under the universal limited without departing substantially from claim and equivalency range, the present invention is not limited
In specific details and shown here as the legend with description.
Claims (6)
1. a kind of method for measuring new fresh mushroom glass transition temperature, it is characterised in that step includes：
1) it is freeze-dried
New fresh mushroom is drying using the method progress of freeze-drying, drying mushroom is then milled to mushroom powder；
2) the mushroom sample of different water cut processed
Obtained mushroom powder is placed in the closed container equipped with different saturated salt solutions, is then placed within insulating box and puts down
Weighing apparatus, carries out adsorption experiment, and the mushroom sample of different water cut is made；
3) dsc measurement contains the glass transition temperature of non-f reezing water (moisture content is relatively low) mushroom
Double scanning imaging systems：The mushroom sample for taking moisture content to be not higher than 0.2 drops to -85~-120 with 5 DEG C/min speed from 25 DEG C
DEG C, 10min is kept, then 60 DEG C are warming up to 5 DEG C/min speed, then -85 are dropped to from 60 DEG C of speed with 5 DEG C/min~-
120 DEG C, 60 DEG C then are warming up to 5 DEG C/min speed again, the vitrifying of the sample of mushroom containing non-f reezing water is gone out by dsc measurement
Transition temperature initial value, glass transition temperature midrange and Tg endpoint value；
4) dsc measurement contains the glass transition temperature of freeze water (moisture content is higher) mushroom
The heat flow curve of mushroom is tentatively obtained using DSC scanning imaging systems first, glass transition temperature is found and freezes terminal temperature
Spend (Tm') position, then further using cycle of annealing measure glass transition temperature；
41) preliminary scan program：Take mushroom sample of the moisture content higher than 0.2 drop to -85 from 25 DEG C of speed with 5 DEG C/min~-
120 DEG C, 10min is kept, then 40 DEG C are raised to from -85~-120 DEG C again with 5 DEG C/min speed, gone out by dsc measurement containing jelly
Bear water the glass transition temperature initial value, glass transition temperature midrange and Tg endpoint of mushroom sample
Value, solidification point and freeze outlet temperature value Tm′；
42) cycle of annealing：
Dsc measurement cycle of annealing is that mushroom sample drops to -85~-120 DEG C from 25 DEG C of speed with 5 DEG C/min, then with 5 DEG C/min
Speed be raised to (Tm' -1) certain time DEG C, is kept；Then again with 5 DEG C/min speed from (Tm' -1) DEG C -85~-120 are dropped to
DEG C, then it is raised to 40 DEG C with 5 DEG C/min speed so that glass transition reaches maximum Freeze concentration state and eliminates heat release
Peak；
5) glass transition temperature curve is obtained
Mushroom glass transition temperature is simulated with the change of moisture content, and glass transition is obtained using nonlinear regression and fitting
Temperature curve；
6) frozen temperature is obtained
Mushroom solidification point is simulated with the change of moisture content, and frozen temperature is obtained using nonlinear regression and fitting；
7) state diagram that frozen temperature, glass transition temperature curve and maximum Freeze concentration state constitute mushroom is built；
8) determine to freeze outlet temperature value T under maximum Freeze concentration statem', and mark on frozen temperature maximum jelly
The point for freezing outlet temperature value under enrichment stage is tied, thus point does vertical line, with the glass transition temperature curve intersection, handed over
Point is mushroom feature glass transition temperature.
2. the method for the new fresh mushroom glass transition temperature of measurement according to claim 1, it is characterised in that mushroom glass
Change transition temperature and use Gordon-Taylor (GT) equation simulation with the change of moisture content, utilize Origin softwares
(version8.6) nonlinear regression and fitting obtains glass transition temperature curve.
3. the method for the new fresh mushroom glass transition temperature of measurement according to claim 1, it is characterised in that mushroom freezes
Temperature uses Clausius-Clapeyron equation simulations with the change of moisture content, utilizes Origin softwares (version 8.6)
Nonlinear regression and fitting obtains frozen temperature.
4. the method for the new fresh mushroom glass transition temperature of measurement according to claim 1, it is characterised in that cycle of annealing
In, (T is raised to 5 DEG C/min speedm' -1) 30min or 60min DEG C, is kept.
5. the method for the new fresh mushroom glass transition temperature of measurement according to claim 1, it is characterised in that dsc measurement
The glass transition temperature of the mushroom containing non-f reezing water is using double scanning imaging system measurements.
6. the method for the new fresh mushroom glass transition temperature of measurement according to claim 1, it is characterised in that for moisture
Activity is more than 0.94 sample, can be added directly into distilled water in the measuring cup equipped with mushroom powder, and 24h is balanced at 4 DEG C.
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