CN111721900A - Method for detecting alpha-conversion degree of starch and product thereof - Google Patents
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- 229920002472 Starch Polymers 0.000 title claims abstract description 158
- 239000008107 starch Substances 0.000 title claims abstract description 157
- 235000019698 starch Nutrition 0.000 title claims abstract description 156
- 238000006243 chemical reaction Methods 0.000 title claims abstract description 33
- 238000000034 method Methods 0.000 title claims abstract description 28
- 239000007788 liquid Substances 0.000 claims abstract description 47
- 239000006185 dispersion Substances 0.000 claims abstract description 46
- 238000001556 precipitation Methods 0.000 claims abstract description 35
- 238000000926 separation method Methods 0.000 claims abstract description 7
- 230000008021 deposition Effects 0.000 claims abstract description 3
- 238000007069 methylation reaction Methods 0.000 claims abstract description 3
- 238000012545 processing Methods 0.000 claims abstract description 3
- 239000013049 sediment Substances 0.000 claims description 17
- 239000000725 suspension Substances 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 5
- 238000002360 preparation method Methods 0.000 claims description 5
- 238000004062 sedimentation Methods 0.000 claims description 2
- 238000011911 α-alkylation Methods 0.000 claims description 2
- 239000000047 product Substances 0.000 abstract description 49
- 239000002244 precipitate Substances 0.000 abstract description 2
- 238000001514 detection method Methods 0.000 description 10
- 238000005119 centrifugation Methods 0.000 description 9
- 238000004321 preservation Methods 0.000 description 6
- 238000006911 enzymatic reaction Methods 0.000 description 5
- 238000001507 sample dispersion Methods 0.000 description 4
- 238000009835 boiling Methods 0.000 description 3
- 238000007796 conventional method Methods 0.000 description 3
- 238000011534 incubation Methods 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 239000000693 micelle Substances 0.000 description 2
- 230000008961 swelling Effects 0.000 description 2
- 102000004190 Enzymes Human genes 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/02—Food
- G01N33/10—Starch-containing substances, e.g. dough
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Abstract
The invention discloses a method for detecting alpha-conversion degree of starch and a product thereof, which comprises the following steps: (1) preparing at least two starch products with known alpha-degree into dispersion liquids with the same concentration respectively, wherein the mass fraction of the dispersion liquids is 0.4-4%; (2) taking a dispersion liquid sample with the same mass, carrying out solid-liquid separation under the same condition, and then determining the volume of the precipitate; (3) the degree of α -methylation and the precipitation volume satisfy the following linear equation: a is aV + b, a is the degree of α -formation, V is the precipitation volume, a, b are parameters; combining the measured at least two groups of precipitation volumes and the corresponding alpha-degree with the linear equation, and calculating parameters a and b to obtain a linear equation; (4) and (3) taking the starch product to be detected, processing according to the conditions in the steps (1) and (2), determining the deposition volume Vx, and substituting the Vx into the linear equation to obtain the alpha-degree of the starch product to be detected. The invention can rapidly measure the alpha-degree of the starch and the products thereof, and has the advantages of high accuracy, short time and low cost.
Description
Technical Field
The invention relates to a method for detecting alpha-conversion degree of starch and a product thereof.
Background
Raw starch molecules are closely arranged by intermolecular hydrogen bonding to form bundle-like micelles, the gaps between the raw starch molecules are small, water molecules are difficult to permeate into the raw starch molecules, and the raw starch with the micelle structure is called beta-starch. After the beta-starch is heated in water, the starch granules absorb water and expand, the volume is increased, the starch granules break, and the process of becoming a viscous colloid solution is called alpha-gelatinization.
When the starch is heated for alpha-melting, the physical change of the processes of water absorption swelling-re-swelling-infinite swelling-dissolving is presented. The alpha-swelling of the starch is a key typical characteristic of alpha-gelatinization of the starch, and the alpha-swelling rate of the starch refers to the percentage of the swelling volume of the alpha-gelatinized starch in the swelling volume of the full alpha-gelatinized starch, so that the alpha-gelatinization degree of the starch can be represented, and the alpha-gelatinization effect of the starch is reflected.
Most of methods for detecting the alpha-degree of starch in the prior art are based on enzyme hydrolysis, and then the alpha-degree of starch is detected by methods such as absorbance, peak area, titration and the like, so that the steps are complicated, the detection time is long, and some expensive devices such as an ultraviolet-visible spectrophotometer, a liquid chromatograph and the like are required. In addition, the quadratic linear equation method needs to collect multiple sets of data to obtain an equation, and a traditional enzymolysis method is also adopted in the process of acquiring data.
Disclosure of Invention
In order to solve the defects and shortcomings in the prior art, the invention aims to provide a method for detecting the alpha-conversion degree of starch and products thereof, which is simple to operate, low in cost and short in time consumption.
In order to realize the purpose, the technical scheme adopted by the invention is as follows:
a method for detecting the alpha-conversion degree of starch and products thereof comprises the following steps:
(1) preparing at least two kinds of starch or starch products with known alpha-degree into dispersion liquid with the same concentration respectively, wherein the mass fraction of the dispersion liquid is 0.4-4%;
(2) taking dispersion liquid samples with the same mass, carrying out solid-liquid separation under the same conditions, and then respectively measuring the precipitation volume in each sample;
(3) determining a linear relationship between the degree of alpha-gelatinization and the sedimentation volume of the starch or starch preparation: the degree of α -methylation and the precipitation volume satisfy the following linear equation: a ═ aV + b, where a is the degree of α -alkylation, V is the precipitation volume, and a, b are parameters; combining at least two groups of precipitation volume data and corresponding alpha-degree determined in the step (2) with the linear equation, and calculating parameters a and b to obtain the linear equation;
(4) determining the alpha-conversion degree of the starch or starch product to be detected: and (3) taking the starch or starch product to be detected, processing according to the conditions in the steps (1) and (2), determining the deposition volume Vx, and substituting the Vx into the linear equation obtained in the step (3) to obtain the alpha-degree of the starch or starch product to be detected.
The inventor finds that under certain concentration conditions, the alpha-conversion degree of the starch and the products thereof has a linear relation with the precipitation volume. Therefore, the linear equation A is fitted to aV + b according to more than two types of starch with known alpha-conversion degrees, so that the alpha-conversion degrees of the starch to be measured and the products thereof can be calculated according to the precipitation volume.
Controlling the mass fraction of the dispersion to be 0.4-4% is the applicable concentration of the detection method of the present invention, and the alpha-conversion degree and the precipitation volume of the starch and the products thereof are in a linear relationship in the range, and beyond the range, the detection method of the present invention cannot be applied.
Preferably, in the step (2), the solid-liquid separation method is as follows: centrifuging for 3-10 min under 3000-6000 r/min. In the invention, the solid-liquid separation condition has larger influence on the accuracy of the measurement of the precipitation volume, and the purpose of accurate measurement can be achieved by carrying out solid-liquid separation under the condition provided by the invention.
Preferably, in step (1), two starches or starch preparations of known degree of α -gelatinization are used. More preferably, in the step (1), raw starch (or raw starch product) having an α -gelatinization degree of 0 and fully cooked starch (or fully cooked starch product) having an α -gelatinization degree of 100% are used. In this case, the calculation formula of the degree of α -formation of the starch or starch product to be measured is as follows:
Ax＝(Vx-V0)/(V100-V0)×100％
ax: determining the degree of alpha-formation of the starch or starch product
Vx: the corresponding precipitation volume of the starch or starch product to be detected;
v0: a sediment volume corresponding to raw starch (or raw starch product) with an alpha-degree of 0;
v100: the degree of alphatization is the sediment volume corresponding to 100% of fully cooked starch (or fully cooked starch preparation).
In the step (1), the dispersion is prepared by a conventional method, and can be prepared in one step or step by step.
Preferably, the dispersion of the fully cooked starch (or fully cooked starch product) having the degree of α -gelatinization of 100% is prepared by: preparing starch suspension with the mass fraction of 2-8% by using raw starch, heating the starch suspension in a water bath until the starch suspension is completely alpha-shaped to obtain starch paste, and preparing the starch paste into solution with the mass fraction of 20-50%, wherein the solution is the dispersion liquid of the fully cooked starch (or fully cooked starch products).
Compared with the prior art, the invention has the beneficial effects that: the detection method can rapidly detect the alpha-degree of the starch and the products thereof, has high accuracy, simple operation flow, low requirement on the operation skill of personnel, convenient practical production and application, low requirement on equipment, short detection time, no need of using chemical reagents in the whole detection process, environmental protection and low detection cost, and can be used for on-line detection and judgment.
Detailed Description
To better illustrate the objects, aspects and advantages of the present invention, the present invention is further illustrated by the following examples. It is apparent that the following examples are only a part of the embodiments of the present invention, and not all of them. It should be understood that the embodiments of the present invention are only for illustrating the technical effects of the present invention, and are not intended to limit the scope of the present invention.
The invention provides a method for detecting alpha-conversion degree of starch and a product thereof, which comprises the following steps:
(1) determination of the sediment volume in dispersions of fully cooked starch samples
Preparing starch suspension with the mass fraction of X1(X1 is 2-8%), putting the starch suspension into a container with a proper size, heating the starch suspension to 90-100 ℃ in a boiling water bath while stirring, and then preserving the heat for 0min, 10min, 30min, 50min, 70min, 90min, 110min and the like. And preparing the starch paste with the corresponding heat preservation time into a dispersion liquid with the mass fraction of X2 (20-50% of X2) to ensure the consistency of the concentration. And (3) taking the dispersion liquid with the same mass in a graduated centrifuge tube with a proper size, centrifuging the dispersion liquid for the same time T (3-10 min) under the condition of the same centrifugal rotating speed R (3000-6000R/min), reading the sediment volume in the centrifuge tube, measuring each sample in parallel twice, and taking the average value as the centrifugal sediment volume of a single sample. The sample with the largest centrifugal sediment volume and tending to be stable is taken as the all alpha-gelatinized starch dispersion, and the sediment volume is recorded as V100.
(2) Determination of the sediment volume in a raw starch dispersion
Preparing raw starch dispersion liquid with the mass fraction of X1 multiplied by X2, putting the raw starch dispersion liquid with the same mass as that in the step (1) into a graduated centrifuge tube with a proper size, centrifuging under the same centrifugation condition as that in the step (1), reading the precipitation volume in the centrifuge tube, performing parallel measurement twice, and taking the average value as the precipitation volume of the raw starch dispersion liquid and marking as V0.
(3) Determination of degree of alpha-formation of sample to be tested
Preparing a sample dispersion liquid according to the method in the step (1), determining the centrifugal precipitation volume in the sample dispersion liquid, recording the centrifugal precipitation volume as Vx, and calculating the alpha-conversion degree Ax of the sample to be detected:
Ax＝(Vx-V0)/(V100-V0)×100％。
example 1
A method for detecting the alpha-conversion degree of starch paste comprises the following steps:
(1) determination of the volume of precipitate in the Dispersion of the fully matured sample
Preparing starch suspension with mass fraction of 5%, placing in a container with proper size, heating to 100 deg.C in boiling water bath under stirring, and keeping the temperature for 0min, 10min, 30min, 50min, 70min and 90 min. And preparing the starch paste with the corresponding heat preservation time into a dispersion liquid with the mass fraction of 30% to ensure the consistency of the concentration. And (3) putting the dispersion liquid with the same mass into a graduated centrifuge tube with a proper size, centrifuging for the same time for 5min under the condition of 4000r/min, reading the sediment volume in the centrifuge tube, measuring each sample in parallel twice, and taking the average value as the centrifugal sediment volume of a single sample. Taking a sample which has the largest centrifugal precipitation volume and tends to be stable as a fully-ripened sample dispersion liquid, namely taking a sample which is subjected to heat preservation for 50min as the fully-ripened sample dispersion liquid, wherein the precipitation volume is 3.538 mL.
(2) Determination of the sediment volume in a raw starch dispersion
Preparing starch suspension with the mass fraction of 5% multiplied by 30% (namely 1.5%) to obtain raw starch dispersion liquid, putting the raw starch dispersion liquid with the same mass as that in the step (1) into a graduated centrifuge tube with a proper size, centrifuging under the same centrifugation condition as that in the step (1), reading the precipitation volume in the centrifuge tube, measuring in parallel twice, taking the average value as the precipitation volume of the raw starch dispersion liquid, and measuring to obtain the precipitation volume of the raw starch dispersion liquid to be 0.345 mL.
(3) Determination of the degree of alpha-formation of a starch paste to be tested
And (2) carrying out alpha-conversion treatment according to the method in the step (1), preparing the starch paste to be detected subjected to alpha-conversion for 0min, 10min and 30min into the dispersion liquid with the same concentration as that in the step (1), putting the dispersion liquid with the same mass as that in the step (1) into a graduated centrifuge tube with a proper size, centrifuging under the same centrifugation condition as that in the step (1), reading the precipitation volume in the centrifuge tube, and respectively measuring the centrifugation precipitation volume to be 3.210mL, 3.416mL and 3.503 mL. The degree of alpha-formation of the starch pastes with alpha-formation incubation for 0min, 10min and 30min was calculated as follows:
the sample was incubated for 0min for α -conversion with the degree of α -conversion of (3.210-0.345)/(3.538-0.345). times.100% to 89.7%
The sample was incubated for 10min for alpha-conversion with the degree of alpha-conversion (3.416-0.345)/(3.538-0.345). times.100%. 96.2%
The samples were incubated for 30min for alpha-conversion with the degree of alpha-conversion (3.503-0.345)/(3.538-0.345). times.100%. 98.9%
Meanwhile, the degree of α -formation of the same sample was measured by the conventional method (enzymatic method), and the results are summarized in the following table.
| Incubation time (min) | 0 | 10 | 30 |
| Volume of centrifugation (mL) | 3.210 | 3.416 | 3.503 |
| α -degree of formation (calculated as in example 1) | 89.7％ | 96.2％ | 98.9％ |
| α degree of conversion (enzymatic method) | 88.3％ | 97.1％ | 99.1％ |
Example 2
A method for detecting the alpha-conversion degree of a starch product comprises the following steps:
(1) determination of the sediment volume in dispersions of fully cooked starch products
Preparing raw starch product according to product formula, heating to 100 deg.C under stirring in boiling water bath, and keeping the temperature for 0min, 20min, 40min, 60min, 80min, 100min and 120 min. And preparing the starch product finished product with the corresponding heat preservation time into dispersion liquid with the mass fraction of 30% to ensure the consistency of the concentration. And (3) putting the dispersion liquid with the same mass into a graduated centrifuge tube with a proper size, centrifuging for the same time for 5min under the condition of 4000r/min, reading the sediment volume in the centrifuge tube, measuring each sample in parallel twice, and taking the average value as the centrifugal sediment volume of a single sample. Taking a sample which has the largest centrifugal precipitation volume and tends to be stable as a fully cooked starch product dispersion liquid, namely the sample which is kept for 40min is the fully cooked starch product dispersion liquid, wherein the precipitation volume is 3.150 mL.
(2) Determination of the sediment volume in dispersions of raw starch products
Preparing a raw starch product according to a product formula, then preparing a suspension with the mass fraction of 30% to obtain a raw starch product dispersion liquid, putting the raw starch product dispersion liquid with the same mass as that in the step (1) into a graduated centrifuge tube with a proper size, centrifuging under the same centrifugation condition as that in the step (1), reading the precipitation volume in the centrifuge tube, measuring twice in parallel, taking the average value as the precipitation volume of the raw starch product dispersion liquid, and measuring to obtain the precipitation volume of the raw starch product dispersion liquid to be 0.285 mL.
(3) Determination of degree of alpha-formation of starch product to be tested
And (2) carrying out alpha-conversion treatment according to the method in the step (1), preparing the starch product to be detected subjected to alpha-conversion for 0min, 20min and 40min into the dispersion liquid with the same concentration as that in the step (1), putting the dispersion liquid with the same mass as that in the step (1) into a graduated centrifuge tube with a proper size, centrifuging under the same centrifugation condition as that in the step (1), reading the precipitation volume in the centrifuge tube, and respectively measuring the centrifugation precipitation volume to be 2.750mL, 2.875mL and 3.150 mL. The alpha-conversion degree of the starch product with the alpha-conversion heat preservation time of 0min, 20min and 40min is calculated as follows:
the degree of alpha-transformation of the starch product is (2.750-0.285)/(3.150-0.285). times.100%: 86.04%)
The degree of alpha-formation of the starch product is (2.875-0.285)/(3.150-0.285). times.100%: 90.40%)
The degree of alpha-formation of the starch product is (3.150-0.285)/(3.150-0.285). times.100%. alpha-formation is 100.00% after the starch product is subjected to alpha-formation and heat preservation for 40min
Meanwhile, the degree of α -formation of the same sample was measured by the conventional method (enzymatic method), and the results are summarized in the following table.
| Incubation time (min) | 0 | 20 | 40 |
| Volume of centrifugation (mL) | 2.750 | 2.875 | 3.150 |
| α -degree of formation (calculated as in example 2) | 86.0％ | 90.4％ | 100.0％ |
| α degree of conversion (enzymatic method) | 84.3％ | 92.6％ | 100.0％ |
As can be seen from the results of the above tests in examples 1 and 2, the degree of α -formation of the starch and its products measured by the methods of examples 1 and 2 of the present invention was very close to that of the same samples measured by the enzymatic method. The detection method has the advantages of high accuracy, simple method, short time consumption and low cost, and can be used for online detection and judgment.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (6)
1. A method for detecting the alpha-conversion degree of starch and products thereof is characterized by comprising the following steps:
(1) preparing at least two kinds of starch or starch products with known alpha-degree into dispersion liquid with the same concentration respectively, wherein the mass fraction of the dispersion liquid is 0.4-4%;
(2) taking dispersion liquid samples with the same mass, carrying out solid-liquid separation under the same conditions, and then respectively measuring the precipitation volume in each sample;
(3) determining a linear relationship between the degree of alpha-gelatinization and the sedimentation volume of the starch or starch preparation: the degree of α -methylation and the precipitation volume satisfy the following linear equation: a ═ aV + b, where a is the degree of α -alkylation, V is the precipitation volume, and a, b are parameters; combining at least two groups of precipitation volume data and corresponding alpha-degree determined in the step (2) with the linear equation, and calculating parameters a and b to obtain the linear equation;
(4) determining the alpha-conversion degree of the starch or starch product to be detected: and (3) taking the starch or starch product to be detected, processing according to the conditions in the steps (1) and (2), determining the deposition volume Vx, and substituting the Vx into the linear equation obtained in the step (3) to obtain the alpha-degree of the starch or starch product to be detected.
2. The method for detecting the degree of α -gelatinization of starch or starch products according to claim 1, wherein in step (2), the solid-liquid separation method comprises: centrifuging for 3-10 min under 3000-6000 r/min.
3. The method for detecting the degree of α -gelatinization of starch or starch products according to claim 1, wherein in step (1), two kinds of starch or starch products with known degrees of α -gelatinization are used.
4. The method for detecting the degree of α -gelatinization of starch or a product thereof according to claim 1, wherein in step (1), a raw starch or a raw starch product having a degree of α -gelatinization of 0 and a fully cooked starch or a fully cooked starch product having a degree of α -gelatinization of 100% are used.
5. The method for detecting the alpha-conversion degree of the starch or the starch product as claimed in claim 4, wherein the calculation formula of the alpha-conversion degree of the starch or the starch product to be detected is as follows:
Ax＝(Vx-V0)/(V100-V0)×100％
ax: determining the degree of alpha-formation of the starch or starch product
Vx: the corresponding precipitation volume of the starch or starch product to be detected;
v0: a sediment volume corresponding to raw starch or raw starch product with an alpha-degree of 0;
v100: the degree of alphatization is 100% of the sediment volume corresponding to a fully cooked starch or a fully cooked starch preparation.
6. The method for detecting the degree of α -gelatinization of starch or starch products according to claim 4, wherein said fully cooked starch or fully cooked starch product dispersion having a degree of α -gelatinization of 100% is prepared by: preparing starch suspension with the mass fraction of 2-8% by using raw starch, heating the starch suspension in a water bath until the starch suspension is completely alpha-shaped to obtain starch paste, and preparing the starch paste into solution with the mass fraction of 20-50%, wherein the solution is the fully cooked starch or the dispersion liquid of the fully cooked starch product.
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