CN106770395A - The dynamic (dynamical) method of starch retrogradation is studied using peak area is selected - Google Patents
The dynamic (dynamical) method of starch retrogradation is studied using peak area is selected Download PDFInfo
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Abstract
Utilized the invention discloses one kind and select peak area to study the dynamic (dynamical) method of starch retrogradation.Using granted patent, " method for preparing amylose having narrow molecular weight distribution range prepares four retrogradation amyloses to the present invention; will obtain four times retrogradation amylose crushed after being dried; survey X ray diffraction datas; using the drawing of origin softwares; using the peak area of 10 ° 20 ° of the angle of diffraction (2 θ) divided by the total diffraction peak areas of amylose crystal, multiplied by the percent crystallization in massecuite for obtaining with 100% the amylose crystal；Four amyloses of retrogradation of selection, it is dissolved in the alkali lye dissolving of 2 4mol/L, hydrochloric acid conditioning solution with 6 12mol/L is neutral, a period of time is stood under 4 80 DEG C of temperature conditionss, sampled according to a series of time periods, method after drying and crushing according to (3) determines the percent crystallization in massecuite of sample in series of time (t), then crystallization rate constant k and nucleation index n is calculated according to formula ln (ln (1 percent crystallization in massecuite))=lnk+nlnt, judges starch retrogradation speed and retrogradation nucleation type.
Description
Technical field
It is to be related to a kind of utilization to select peak area in particular the present invention relates to food field of deep
The method for studying starch retrogradation dynamic method.
Background technology
Starch retrogradation is substantially the process that starch molecule forms crystal, includes nucleation and core increase.With
In the ripe theory Avrammi equations that slaine and small organic molecule Crystallization process kineticses are studied
(ln (- ln (1- percent crystallization in massecuites))=lnk+nlnt) should be also applied for starch retrogradation dynamics research.But arrive
So far, the dynamic law of starch retrogradation is also successfully explored using this equation without document report.
Its main cause has two aspects, and one is that starch molecule amount distribution is too wide, different molecular weight distribution
Starch molecule retrogradation kinetics parameter it is inconsistent, research association admixed together make these parameters height rise and fall
It is indefinite；Two is that starch molecule amount is big, space structure is complicated, makes starch retrogradation process crystal growth mode not
Single, the crystal retrogradation nucleation index of different time sections is presented irregular change, and experimental result reappearance is not
It is high.
The content of the invention
The present invention is to prepare narrower straight chain, the amylopectin of range of molecular weight distributions using new granted patent
On the basis of, calculated by many experiments and data, it is found that the retrogradation of X-ray diffraction measure amylose is brilliant
Body 10 ° -20 ° of the angle of diffraction (2 θ) peak area divided by the total diffraction peak areas of amylose crystal,
Brought back to life in amylose different temperatures and time multiplied by the percent crystallization in massecuite for obtaining with 100% the amylose crystal
Journey gained crystal structure rate is presented regular change.Percent crystallization in massecuite is calculated in this way substitutes into Avrammi
More can accurately be calculated after equation amylose retrogradation nucleation index n and velocity constant k, so as to compared with
The thermodynamic nature that adequately reflection amylose is brought back to life.
The present invention is achieved through the following technical solutions：
Method (the patent No. ZL of amylose having narrow molecular weight distribution range " is prepared using granted patent
201110120286.3) amylose is prepared；By the alkali lye that this amylose concentration is 2-4mol/L
Dissolving, is neutral with the hydrochloric acid conditioning solution of 6-12mol/L, and " molecular weight distribution model is prepared with reference to patent
The method (patent No. ZL 201110120286.3) for enclosing narrower amylose prepares secondary retrogradation straight chain shallow lake
Powder；With secondary retrogradation amylose as raw material, three times, four retrogradation straight chains are prepared using identical method
Starch；The four retrogradation amylose crushed after being dried that will be obtained, survey X-ray diffraction data, utilize
Origin softwares chart, using the peak area of 10 ° -20 ° of the angle of diffraction (2 θ) divided by amylose crystal
Total diffraction peak areas, multiplied by the percent crystallization in massecuite for obtaining with 100% the amylose crystal；Four retrogradations of selection
Amylose, be dissolved in 2-4mol/L alkali lye dissolving, with the hydrochloric acid conditioning solution of 6-12mol/L
It is neutrality, a period of time is stood under 4-80 DEG C of temperature conditionss, sampled according to a series of time periods, dries
Spread out divided by amylose crystal is total according to the peak area using the angle of diffraction 10 ° -20 ° of (2 θ) after crushing
Peak area is penetrated, series of time (t) is determined multiplied by the method for the percent crystallization in massecuite for obtaining with 100% the amylose crystal
The percent crystallization in massecuite of interior sample, then calculates crystallization rate according to formula ln (- ln (1- percent crystallization in massecuites))=lnk+nlnt
Constant k and nucleation index n, judge starch retrogradation speed and retrogradation nucleation type (n less than 1 for once into
Core, is multiple nucleation more than 1).
To constant weight, drying temperature is 60-80 for the amylose drying that the step (1) and (2) obtain
DEG C, smashing fineness crosses 80 mesh and shines net.
When determining X-ray diffraction data in step (3), the angle of diffraction (2 θ) is scanned from 0 ° to 60 °,
Step-length is 0.05, and interval time is 2s, obtains the total diffraction peak areas of amylose crystal.
The step (1) prepare the raw material of amylose for sweet potato starch, farina, cornstarch,
Any one in wheaten starch, barley starch, bean starch.
The present invention has the following technical effect that：
The method of the present invention can ensure amylose retrogradation percent crystallization in massecuite in starch retrogradation dynamics research is studied
Correlation is presented in the range of certain hour with the starch retrogradation time, makes amylose retrogradation process kineticses
Can be furtherd investigate using Avrammi equations, clearly be accurately reflected amylose macromolecular retrogradation nucleation
The possibility mode increased with core.The inventive method is simple to operate, low cost.Conventional X-ray diffraction is direct
The method for determining common starch percent crystallization in massecuite or heat absorption enthalpy being determined using differential scan calorimeter, can not obtain
The stronger data of correlation between retrogradation time and retrogradation rate.
Specific embodiment
Below in conjunction with specific embodiment, the present invention is described in detail.
Embodiment 1
(1) 100 grams of sweet potato starch is mixed and made into the starch milk that concentration is 10%, 90 DEG C of gelatinizations with water
Pressure cooker is put into after 30min carries out HIGH PRESSURE TREATMENT, and high pressure temperature is 105-120 DEG C, and high-voltage time is
30min, carried out after taking-up it is aging obtain semi-solid retrogradation resistant starch, aging temperature be 15 DEG C, it is aging
Time is 6h.
(2) the retrogradation resistant starch for obtaining step (1) is digested using alpha-amylase, enzymatic hydrolysis condition
For：The retrogradation resistant starch obtained per 100g steps (1) adds the amylase 1200U, hydrolysis temperature to be
90-100 DEG C, enzymolysis time is 10min, then using 3000 revs/min of centrifugations, is precipitated with three times
Volume washes three centrifugation acquisition purifying retrogradation resistant starches afterwards.
(3) it is the NaOH of 2mol/L that the purifying retrogradation resistant starch that will be obtained after enzymolysis uses concentration
Aqueous dissolution.2 times of n-butanols of volume of alkali lye are added in retrogradation resistant starch after alkali lye dissolving, it
Afterwards, amylose is obtained after 3000 revs/min of centrifugal dryings.It is raw material with the sweet potato amylose for obtaining, weight
Multiple (1)-(3) step, obtains secondary retrogradation sweet potato amylose, same method repeat to obtain three times,
Four retrogradation sweet potato amyloses.
(4) the four retrogradation amylose crushed after being dried that will be obtained, survey X-ray diffraction data, utilize
Origin softwares chart, using the peak area of 10 ° -20 ° of the angle of diffraction (2 θ) divided by amylose crystal
Total diffraction peak areas, multiplied by the percent crystallization in massecuite for obtaining with 100% the amylose crystal；Four retrogradations of selection
Amylose, be dissolved in 2mol/L alkali lye dissolving, in being with the hydrochloric acid conditioning solution of 6mol/L
Property, a period of time is stood under 4 DEG C of temperature conditionss, taken according to 3,6,13,16,21,24h time periods
Sample, it is brilliant divided by amylose according to the peak area using the angle of diffraction 10 ° -20 ° of (2 θ) after drying and crushing
The total diffraction peak areas of body, system is determined multiplied by the method for the percent crystallization in massecuite for obtaining with 100% the amylose crystal
The percent crystallization in massecuite of sample in row time (t), respectively 29.2%, 31.7%, 31.7%, 31.9%, 34.5%,
36.9%, then according to formula ln (- ln (1- percent crystallization in massecuites))=lnk+nlnt calculate crystallization rate constant k and
Nucleation index n, respectively 0.7,0.6,7.8,0.8 and 0.01,0.01,0.77,0.06, sweet potato
Straight chain retrogradation nucleation is a nucleation.
Conventional X-ray diffraction is directly determined Ordinary Sweet Potatoes starch crystals rate or is surveyed using differential scan calorimeter
Surely absorb heat the method for enthalpy, X-ray diffraction measures the retrogradation percent crystallization in massecuite of sweet potato starch and is respectively under the same terms
12.5%th, 6.3%, 25.8%, 9.7%, 43.2%, 5.1%；Differential scan calorimeter is determined under the same terms
The retrogradation percent crystallization in massecuite that heat absorption enthalpy measures sweet potato starch is respectively 9.8%, 36.2%, 7.5%, 23.9%, 22.1%,
9.4%, can not obtain the stronger data of correlation between retrogradation time and retrogradation rate, it is impossible to use
Avrammi equation computational dynamics parameters.
Embodiment 2
(1) 100 grams of cornstarch is mixed and made into the starch milk that concentration is 10%, 90 DEG C of gelatinizations with water
Pressure cooker is put into after 30min carries out HIGH PRESSURE TREATMENT, and high pressure temperature is 105-120 DEG C, and high-voltage time is
30min, carried out after taking-up it is aging obtain semi-solid retrogradation resistant starch, aging temperature be 15 DEG C, it is aging
Time is 6h.
(2) the retrogradation resistant starch for obtaining step (1) is digested using alpha-amylase, enzymatic hydrolysis condition
For：The retrogradation resistant starch obtained per 100g steps (1) adds the amylase 1200U, hydrolysis temperature to be
90-100 DEG C, enzymolysis time is 10min, then using 3000 revs/min of centrifugations, is precipitated with three times
Volume washes three centrifugation acquisition purifying retrogradation resistant starches afterwards.
(3) it is the NaOH of 2mol/L that the purifying retrogradation resistant starch that will be obtained after enzymolysis uses concentration
Aqueous dissolution.2 times of n-butanols of volume of alkali lye are added in retrogradation resistant starch after alkali lye dissolving, it
Afterwards, amylose is obtained after 3000 revs/min of centrifugal dryings.It is raw material with the maize amylose for obtaining, weight
Multiple (1)-(3) step, obtains secondary retrogradation maize amylose, same method repeat to obtain three times,
Four retrogradation maize amyloses.
(4) the four retrogradation amylose crushed after being dried that will be obtained, survey X-ray diffraction data, utilize
Origin softwares chart, using the peak area of 10 ° -20 ° of the angle of diffraction (2 θ) divided by amylose crystal
Total diffraction peak areas, multiplied by the percent crystallization in massecuite for obtaining with 100% the amylose crystal；Four retrogradations of selection
Amylose, be dissolved in 2mol/L alkali lye dissolving, in being with the hydrochloric acid conditioning solution of 6mol/L
Property, a period of time is stood under 25 DEG C of temperature conditionss, according to 3,6,13,16,21, the 24h time periods
Sampling, according to the peak area using the angle of diffraction 10 ° -20 ° of (2 θ) divided by amylose after drying and crushing
The total diffraction peak areas of crystal, determine multiplied by the method for the percent crystallization in massecuite for obtaining with 100% the amylose crystal
The percent crystallization in massecuite of sample in series of time (t), respectively 30.6%, 30.4%, 31.3%, 31.3%, 31.7%,
32.9%, then according to formula ln (- ln (1- percent crystallization in massecuites))=lnk+nlnt calculate crystallization rate constant k and
Nucleation index n, respectively 0.6,0.6,0.4,1.5 and 0.05,0.02,0.14,0.19, corn
Straight chain retrogradation nucleation is a nucleation.
Conventional X-ray diffraction is directly determined common corn starch percent crystallization in massecuite or is surveyed using differential scan calorimeter
Surely absorb heat the method for enthalpy, X-ray diffraction measures the retrogradation percent crystallization in massecuite of cornstarch and is respectively under the same terms
2.3%th, 14.5%, 6.2%, 31.3%, 17.8%, 5.9%；Differential scan calorimeter is determined under the same terms
The retrogradation percent crystallization in massecuite that heat absorption enthalpy measures cornstarch is respectively 7.2%, 23.8%, 2.1%, 47.2%, 32.6%,
5.3%, can not obtain the stronger data of correlation between retrogradation time and retrogradation rate, it is impossible to use
Avrammi equation computational dynamics parameters.
Embodiment 3
(1) 100 grams of wheaten starch is mixed and made into the starch milk that concentration is 10%, 90 DEG C of gelatinizations with water
Pressure cooker is put into after 30min carries out HIGH PRESSURE TREATMENT, and high pressure temperature is 105-120 DEG C, and high-voltage time is
30min, carried out after taking-up it is aging obtain semi-solid retrogradation resistant starch, aging temperature be 15 DEG C, it is aging
Time is 6h.
(2) the retrogradation resistant starch for obtaining step (1) is digested using alpha-amylase, enzymatic hydrolysis condition
For：The retrogradation resistant starch obtained per 100g steps (1) adds the amylase 1200U, hydrolysis temperature to be
90-100 DEG C, enzymolysis time is 10min, then using 3000 revs/min of centrifugations, is precipitated with three times
Volume washes three centrifugation acquisition purifying retrogradation resistant starches afterwards.
(3) it is the NaOH of 2mol/L that the purifying retrogradation resistant starch that will be obtained after enzymolysis uses concentration
Aqueous dissolution.2 times of n-butanols of volume of alkali lye are added in retrogradation resistant starch after alkali lye dissolving, it
Afterwards, amylose is obtained after 3000 revs/min of centrifugal dryings.It is raw material with the wheat amylose for obtaining, weight
Multiple (1)-(3) step, obtains secondary retrogradation maize amylose, same method repeat to obtain three times,
Four retrogradation maize amyloses.
(4) the four retrogradation amylose crushed after being dried that will be obtained, survey X-ray diffraction data, utilize
Origin softwares chart, using the peak area of 10 ° -20 ° of the angle of diffraction (2 θ) divided by amylose crystal
Total diffraction peak areas, multiplied by the percent crystallization in massecuite for obtaining with 100% the amylose crystal；Four retrogradations of selection
Amylose, be dissolved in 2mol/L alkali lye dissolving, in being with the hydrochloric acid conditioning solution of 6mol/L
Property, a period of time is stood under 70 DEG C of temperature conditionss, according to 3,6,13,16,21, the 24h time periods
Sampling, according to the peak area using the angle of diffraction 10 ° -20 ° of (2 θ) divided by amylose after drying and crushing
The total diffraction peak areas of crystal, determine multiplied by the method for the percent crystallization in massecuite for obtaining with 100% the amylose crystal
The percent crystallization in massecuite of sample in series of time (t), respectively 32.7%, 33.2%, 33.3%, 33.7%, 34.9%,
36.9%, then according to formula ln (- ln (1- percent crystallization in massecuites))=lnk+nlnt calculate crystallization rate constant k and
Nucleation index n, respectively 0.7,0.4,0.4,1.2 and 3.26,0.15,0.18,0.13, wheat
It is multiple nucleation before straight chain retrogradation nucleation 6h, is a nucleation after 6h.
Conventional X-ray diffraction is directly determined common wheat starch crystals rate or is surveyed using differential scan calorimeter
Surely absorb heat the method for enthalpy, X-ray diffraction measures the retrogradation percent crystallization in massecuite of wheaten starch and is respectively under the same terms
6.7%th, 36.8%, 5.2%, 46.1%, 12.4%, 9.8%；Differential scan calorimeter is determined under the same terms
The retrogradation percent crystallization in massecuite that heat absorption enthalpy measures wheaten starch is respectively 8.3%, 38.2%, 6.7%, 43.3%, 14.6%,
8.2%, can not obtain the stronger data of correlation between retrogradation time and retrogradation rate, it is impossible to use
Avrammi equation computational dynamics parameters.
Claims (4)
1. a kind of utilization selects peak area to study the dynamic (dynamical) method of starch retrogradation, it is characterised in that：
Comprise the steps：
(1) using granted patent " method for preparing amylose having narrow molecular weight distribution range " specially
Profit ZL 201110120286.3, prepares amylose；
(2) by the alkali lye dissolving that the amylose concentration in (1) is 2-4mol/L, 6-12 is used
The hydrochloric acid conditioning solution of mol/L is neutrality, and the method for reusing step (1) prepares secondary retrogradation
Amylose；With secondary retrogradation amylose as raw material, prepared by the method for being continuing with step (1)
Three retrogradation amyloses, four retrogradation amyloses；
(3) the four retrogradation amylose crushed after being dried that will be obtained, survey X-ray diffraction data,
Charted using origin softwares, using the peak area of 10 ° -20 ° of the angle of diffraction (2 θ) divided by straight chain
The total diffraction peak areas of starch crystal, multiplied by the percent crystallization in massecuite for obtaining with 100% the amylose crystal；
(4) four amyloses of retrogradation are selected, the alkali lye dissolving of 2-4mol/L is dissolved in, is used
The hydrochloric acid conditioning solution of 6-12mol/L is neutrality, and a period of time is stood under 4-80 DEG C of temperature conditionss,
Sampled according to 3,6,13,16,21,24h time periods, according to the method for (3) after drying and crushing
The percent crystallization in massecuite of sample in series of time (t) is determined, then ((1- is crystallized-ln according to formula ln
Rate))=lnk+nlnt calculate crystallization rate constant k and nucleation index n, judge starch retrogradation speed with
Retrogradation nucleation type, wherein n is a nucleation less than 1, and n is multiple nucleation more than 1.
2. according to claim 1 utilization selects peak area to study starch retrogradation dynamic method,
It is characterized in that：The amylose drying that the step (1) and (2) obtain dries temperature to constant weight
It is 60-80 DEG C to spend, and smashing fineness crosses 80 mesh and shines net.
3. according to claim 1 utilization selects peak area to study starch retrogradation dynamic method,
It is characterized in that：When determining X-ray diffraction data in step (3), the scanning angle of diffraction (2 θ) from
0 ° to 60 °, step-length is 0.05, and interval time is 2s, obtains the total diffraction of amylose crystal
Peak area.
4. according to claim 1 utilization selects peak area to study starch retrogradation dynamic method,
Characterized in that, the raw material that the step (1) prepares amylose is sweet potato starch, potato shallow lake
Any one in powder, cornstarch, wheaten starch, barley starch, bean starch.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113670959A (en) * | 2021-07-21 | 2021-11-19 | 扬州大学 | Novel method for analyzing relative crystallinity of starch |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102226212A (en) * | 2011-05-11 | 2011-10-26 | 天津商业大学 | Method for preparing amylose having narrow molecular weight distribution range |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102226212A (en) * | 2011-05-11 | 2011-10-26 | 天津商业大学 | Method for preparing amylose having narrow molecular weight distribution range |
Non-Patent Citations (3)
| Title |
|---|
| A.ABD KARIM: "Methods for the study of starch retrogradation", 《FOOD CHEMISTRY》 * |
| 王婷婷: "淀粉回生动力学研究进展", 《粮食加工》 * |
| 郭俊杰: "马铃薯淀粉的分离、特性及回生研究进展", 《粮食加工》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113670959A (en) * | 2021-07-21 | 2021-11-19 | 扬州大学 | Novel method for analyzing relative crystallinity of starch |
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