CN102419305B - Method for determining gelatinization temperature and gelatinization degree of starch - Google Patents
Method for determining gelatinization temperature and gelatinization degree of starch Download PDFInfo
- Publication number
- CN102419305B CN102419305B CN 201110254158 CN201110254158A CN102419305B CN 102419305 B CN102419305 B CN 102419305B CN 201110254158 CN201110254158 CN 201110254158 CN 201110254158 A CN201110254158 A CN 201110254158A CN 102419305 B CN102419305 B CN 102419305B
- Authority
- CN
- China
- Prior art keywords
- starch
- gelatinization
- value
- iod
- picture
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Images
Landscapes
- Investigating Or Analysing Materials By Optical Means (AREA)
Abstract
The invention discloses a method for determining the gelatinization temperature and gelatinization degree of starch. In the method, according to a principle that starch has a crystal structure which produces a birefringent light phenomenon under polarized light, an IOD (integral optical density) value and an OD (optical density) value of an acquired microscopic digital photo are analyzed by using professional image analysis software Image-proplus, and then the gelatinization degree of the starch is obtained through conversion. Compared with the traditional method, the method disclosed by the invention is scientific, simple, convenient and quick, and can characterize starch granules in a partially gelatinized state, therefore, the true situation in a sample gelatinization process can be reflected better, and obtained results are accurate and reliable; meanwhile, the higher-density observation of the starch under a microscope is realized, the experiment workload is reduced, and the results have high statistical significance.
Description
Technical field
The present invention relates to the assay method of starch gelatinization temperature and gelatinization degree, the starch granules that particularly relates to is (online) or the assay method of the gelatinization situation of gained sample (non-online) after treatment in gelatinization process.
Background technology
Traditional gelatinization theory thinks that the gelatinization of starch is a kind of by the phase transition process of tactical rule to irregular transformation.When ative starch heated in water, their polycrystallinity faded away, and caused structural destruction, and the starch polymer is dispersed in the solution subsequently.Begin just to have many researchers to propose starch gelatinization theory separately from 19th-century, but the structural transition process that this hydrothermal treatment consists causes is still understood thoroughly.Discover more and more that in recent years the gelatinization phase transformation of starch is a more complicated nonequilibrium process, changing mutually in a quite wide temperature range of starch takes place, and the phase transition process difference of the starch experience of separate sources is very big.The most important parameter of gelatinization phenomenon comprises gelatinization point (initial gelatinization point stops gelatinization point, gelatinization temperature range) and gelatinization degree.
Many amyloid food are experiencing different hot procedures and unit operations and can make its starch granules be in part to the different phase of whole gelatinizations, and these affect the physicochemical property of the middle product of processing and product jointly.From the angle of food science, as breakfast sowens oatmeal and bake based food, these contain the food of living starch or part gelatinized starch, its after meal the blood sugar response more and more be subjected to people's attention.The gelatinization degree that studies show that starch is the starch deciding factor of blood sugar response in vivo, and both have good correlativity.Therefore the gelatinization degree of monitoring and control starch product has great importance.
In the production run of converted starch, because various water, the effect of heat and chemical reagent, the starch product that obtains has in various degree gelatinization with respect to ative starch, and it is a typical phenomenon that its birefringent light weakens.But tradition is utilized the technology of microexamination, can only describe this phenomenon qualitatively, the degree that can't quantitative measurment weakens, and the degree of corresponding gelatinization.The gelatinization degree of converted starch product needs control, to guarantee product yield and quality.
The structure of ative starch is to carry out the layering combination with four kinds of different yardsticks, comprising: molecular scale, thin layer yardstick, growth circle yardstick and whole starch granules yardstick.These four kinds of yardstick levels all are associated with the gelatinization phenomenon.The gelatinization of starch and relevant character can obtain based on chemistry, zymetology and physical laboratory facilities and commercial measurement with many, comprise measuring diesis end point, viscosity variation, X-diffraction (comprising WAXD and SAXS), the variation of DSC ∕ TMA detection heat content, amylose-iodine compound (blue valve), enzyme digestability, NMR, expansion, dissolving or precipitation etc.These method principle differences, they characterize the gelatinization characteristic of starch from different perspectives, and the measured physico-chemical property that obtains is unique and connect each other separately.
Hot platform polarizing microscope is a kind of instrument of research starch gelatinization commonly used, utilizes the crystal property of starch, and the principle of the birefringent light that occurs under polarized light is paid close attention to the regular texture of starch granules under 500nm light wave length dimension.Classical way is that the temperature when 2% and 98% particle loses polarisation is defined as gelatinization initial temperature and gelatinization final temperature respectively, and the latter also often is called as birefringence end point temperature.Parada and Jos ' E M. Aguilera think that the polygon area in starch polarisation zone and gelatinization degree have good correlativity, but it has been ignored birefringent light and is experiencing from being attenuated to this fact of disappearance process.Starch is in gelatinization process, and the birefringent light of starch is not to disappear the starch granules that is in part gelatinization state in a large number that exists in gelatinization process in a flash.The method of traditional number particle disappearance quantity even be not a geometric parameter, so they can't characterize out the truth of certain time point starch gelatinization simultaneously.
Summary of the invention
The object of the invention is to overcome the shortcoming of conventional art, provides a kind of and can accurately measure the starch gelatinization degree methods.
Purpose of the present invention realizes by following two kinds of technical schemes:
1, the on-line determination method of a kind of starch gelatinization temperature and gelatinization degree comprises step:
(1) simulation and shooting: the starch milk system of mass concentration 5-20% in simulation practical study and the production technology, the starch milk of configuration same concentrations, behind balance 1-2h under the room temperature, draw the uniform starch milk film-making of 50-80 μ l, place hot platform under polarizing microscope, heat up and heat, the control temperature is lower than 100 ℃; Take sampling continuously by the digital camera that links to each other with microscope;
(2) analysis of digital picture: analyze the original I OD value that obtains whole digital photo with professional image analysis software Image-pro plus 5.0;
(3) calculating of gelatinization degree and sign:
Background correction: D=A-B; DG%=1-D/C ╳ 100%
Wherein, DG%: starch is gelatinization degree under certain temperature; The physical significance of DG% can be interpreted as with respect to original state, under certain temperature starch with birefringent light intensity be sign crystalline texture intensity weaken degree.
A: preliminary survey IOD value refers to the IOD value that original polarisation picture records;
B: background IOD value refers to the IOD value of the picture that the birefringent light of all starch disappears;
C: the actual IOD value of original state, the actual IOD value when referring to the starting point of experiment measuring temperature;
D: actual IOD value refers to that starch sample in the picture has the integral optical density value of the starch crystals part of birefringent light character;
(4) determine gelatinization point:
Initial gelatinization point T
0, stop gelatinization point T
eDetermine by following relational expression with gelatinization temperature range T`: T
0=T
DG%=10%T
e=T
DG%=99%T`=T
e-T
0T wherein
DG%=10%Temperature during expression DG%=10%; T
e=T
DG%=99%Temperature during expression DG%=99%.
Preferably, the preferred cornstarch of starch, farina, tapioca or the pea starch in the described step (1).Their gelatinization final temperature is below 100 ℃.
When heating up in the described step (1), heating rate is less than 5 ℃/min.
The sampling spot frequency of described step (1) shooting sampling is less than 2 ℃ and gets a shooting once.
In the digital image acquisition process, photo requires pixel more than 2,000,000 in the step (1), and bit depth is more than 12, monochromatic mode.High-quality digital pictures has guaranteed graphical analysis result's accuracy.
Under the on-line measurement situation, the selection of the starch concentration in the described step (1) is that few mutual superposition of trying one's best is good according to requirement of experiment and with starch granules uniform spreading in the visual field.
In heating up in the described step (1) under the on-line measurement situation, maximum temperature all can not be higher than 100 ℃, breaks through the sealing slide to avoid producing a large amount of water vapor.
Take sampling process under the on-line measurement situation in the described step (1) continuously, should close the Automatic white balance in the photographing program, for photographic system configuration voltage stabilizer, guarantee fixing shooting condition simultaneously.
2, the non-on-line determination method of a kind of starch gelatinization temperature and gelatinization degree comprises step:
(1) take: configuration quality concentration is the starch milk of 1-5%, draws one with glue head dropper, drips on microslide, and covered is evenly disperseed drop; Place to take under the polarizing microscope and obtain digital pictures;
(2) analysis of digital picture: analyze the original I OD value that obtains whole digital photo with professional image analysis software Image-pro plus 5.0;
(3) calculating of gelatinization degree and sign:
C=A-B；D=C/E；DG%=1—G?/F╳100%
Wherein, DG%: starch is gelatinization degree under certain temperature;
A: preliminary survey IOD value refers to the IOD value that original polarisation picture records;
B: background IOD value refers to not have the IOD value of the blank picture of starch granules;
C: actual IOD value refers to that starch sample in the picture has the integral optical density value of the starch crystals part of birefringent light character;
The D:OD value refers to that starch sample in the picture has the optical density value of the starch crystals part of birefringent light character;
E: the area of starch granules in the visual field;
F: the OD value of undressed ative starch;
G: the OD value of starch sample after treatment.
For non-on-line determination method, preferably, described starch is cornstarch, farina, tapioca, pea starch or green starch; Or be esterification and crosslinking, the malleableize of feedstock production, the converted starch of amorphous particulate with cornstarch, farina, tapioca, pea starch or green starch.
In the digital image acquisition process, photo requires pixel more than 2,000,000 in the described step (1), and bit depth is more than 12, monochromatic mode.
The digital pictures of taking in the step (1) comprises the picture that has starch in the visual field under normal optical and the polarization light, comprises that also the picture of no starch granules in the polarization light downward view is to carry out the background correction.
In the computing formula of gelatinization degree, the physical significance of DG% is with respect to ative starch in the described step (3), the gained starch product with birefringent light intensity be sign crystalline texture intensity weaken degree.
The principle of the invention: gray scale is to represent the degree of the pixel color depth in the digital picture in image analysis system.From the most black be 256 gray levels to the brightest being divided into, minimum value is 0, is stain in image; Maximal value is 255, is bright spot in image.The more little color of gray-scale value is more dark.
Optical density (OD) claim absorbance again, refers to that light passes through to get incident intensity I before solution or a certain material
0With this light by the projection light intensity I behind solution or the material
bThe logarithm of ratio, i.e. OD=lg (I
0/ I
b).The OD value is more big, and then to be absorbed degree more big for light, and the color relation of solution or material is more dark, and solutes content is just more high; Vice versa.In image analysis system, OD only refers to the OD value on a certain pixel in the image, so in order to obtain the summation of the OD value in a certain zone, we just accumulate the OD value in this zone, and the total amount of contained positive material is directly proportional in the integral optical density on the sample that obtains in a certain position (IOD) value (being defined as the summation of the OD value of all picture elements in this region, position) and this position.MOD(average optical in certain zone, mean optical density) multiply by on this region area S numerical value and equal the IOD value.What MOD reflected then is the concentration of positive material in the target area.
But the optical density value in the image analysis system is actually by gray-scale value and calculates, is the digital pictures gray values of pixel points because computing machine can Direct Recognition.For example use image analysis software Image-pro plus, adopt the free measurement pattern of light intensity, namely do not carry out standard absorbance and correct, the IOD value of target substance is actually the accumulation of each pixel gray-scale value in the gray scale picture that obtains.The OD value of digital pictures will be linear proportional relation with the brightness of measuring object.
Utilize the gelatinization of the photo densitometry function monitoring starch of image analysis system, the crystal structure of supposing starch granules is " positive material ", be directly proportional with its birefringent light intensity under polarized light because it is strong and weak, we just can measure the situation of change of the starch birefringence light intensity relevant with crystallization degree, thus the gelatinization degree of quantitatively characterizing starch.Under the on-line measurement situation, in the computing formula of gelatinization degree, the background correction refers to initial IOD value background correction IOD value to reflect the real IOD value of starch itself in the step (3).Because except under polarization light, showing the starch crystals structure division of birefringent light characteristic, still have other interference type light, as background printing opacity and other luminiferous non-positive material of glass sheet in the field of microscope.They also can measure optical density value, and this optical density value is also corresponding to illusory " a positive material content ", " positive material " that stricti jurise is illusory but be the non-positive material of any contribute light density.Therefore during the positive material content on considering sample, must deduct this illusory " positive material content ".
Utilize hot platform polarizing microscope to observe the starch gelatinization process with respect to existing, measure the technology of gelatinization degree, the present invention has following advantage:
(1) the IOD value is and area and OD value relevant integral function all, the area correspondence be what of quantity of starch crystals structure, OD then is directly proportional with the power of starch crystals structure.The gelatinization process that characterizes starch based on the IOD value can with traditional several particles, and consider that merely Method for Area relatively, more can accurately characterize the total amount of the crystalline texture of starch to " area " and " power " two parameter generating responses of birefringent light.
(2) the same digital pictures of duplicate measurements, the optical density resultant error is in 0.1%.Show that the systematic error of digital pictures in gatherer process can be controlled in more among a small circle, sampling process stability is high.
(3) this method repeatability better, parallel laboratory test shows, with a kind of measuring result error of sample in 5%.
(3) can observe 1000 above starch granules at most on this method one number sign indicating number picture, this concentration and starch granules size with starch milk is relevant.Realize the higher density observation of starch at microscopically, reduced the experimental work amount, the statistical significance height.
Description of drawings
Fig. 1 is the graph of a relation of cornstarch DG% and temperature among the embodiment 1.
Fig. 2 is the graph of a relation of pea starch DG% and temperature among the embodiment 2.
Fig. 3 is farina DG% and the graph of a relation of heat time heating time among the embodiment 3.
Embodiment
For better understanding the present invention, the present invention will be further described below in conjunction with embodiment, but the scope of protection of present invention is not limited to the scope that embodiment represents.
The professional image analysis software Image-Pro Plus 5.0 that the present invention uses is released by U.S. Media Cybernetics company, it provides the advanced person for image forming apparatus, graphical analysis control and robotization, solution easy and simple to handle, for researchist, scientist, laboratory technicians, slip-stick artist and experts such as quality assurance and research design, it provide easier, rapider and more accurately method with the details in reproduction, collection, the analysis image.Range of application comprises the pathology micro image analysis; Area form and densitometric analysis; SABC; Fluoroscopic image analysis etc.What this patent used is its densitometric analysis function.
Embodiment 1: the gelatinization point and the crystal characteristic gelatinization curve thereof that are used for measuring cornstarch
The cornstarch emulsus liquid system of analog-quality concentration (butt) 5% detects its starch gelatinization degree change situation in continuous temperature-rise period.
1, the shooting of digital photo.Comprise the steps and process conditions:
(1) the cornstarch emulsus liquid of configuration quality concentration (butt) 5%, balance 2h under the room temperature, firmly stir the starch milk after the balance, its starch that avales is stirred, in system, be more evenly distributed, draw 60 μ l starch milks with glue head dropper, drip two to three rapidly and drip to the glass sheet central authorities that coat a circle fluid sealant at the edge, and with glue head dropper tip paddling, starch milk is evenly distributed, cover another sheet glass sheet then, compress sealing.Starch is sprawled evenly in the film-making requirement microscopic field, and stack is less between the starch granules.
(2) regulate polarizing microscope aperture and photographic exposure time, make the photo exposure amount suitable.Arranging and taking pixel is 2048 * 1536, preserves form TIFF, bit depth 16, monochromatic mode.Selecting enlargement factor for use is 200 times order, and Automatic white balance is closed in the object lens combination simultaneously.
(3) slide that makes is placed hot platform, under the good polarizing microscope of debugging, choose the visual field, heating schedule is set is, 40 ℃ of initial temperatures, 80 ℃ of final temperatures, programming rate are 2 ℃/min.
(3) in heating process, the digital camera that links to each other with microscope is taken continuously, makes 40-60 ℃ every 5 ℃, and 60-80 ℃ every 2 ℃ of once sampling.
2, the analysis of digital picture.
The digital picture of taking is imported Image-pro plus software, use AOI (Automated Optical Inspection, " automated optical detection ") the selected whole pictures of rectangle frame select tool, click " measure "-" count/size "-" measure "-select measure "; selected " IOD " item; click " OK "; in the Previous Menu hurdle, click then " edit "; select " convert AOI (s) To Object (s) "; double-click picture, can obtain the IOD value of a pictures.Obtain the IOD value of every number sign indicating number picture according to above step.
3, the calculating of gelatinization degree and sign.
Background correction: D=A-B;
DG%=1—D?/C╳100%。
Physics meaning:
DG: cornstarch is gelatinization degree under certain temperature;
A: preliminary survey IOD value refers to the IOD value that original polarisation picture records;
B: background IOD value refers to the IOD value of the picture that the birefringent light of all starch disappears;
C: the actual IOD value of original state, the actual IOD value when referring to the starting point of experiment measuring temperature;
D: actual IOD value refers to that starch in the picture has the integral optical density value of the starch crystals part of birefringent light character.
The graph of a relation of cornstarch DG% and temperature as shown in Figure 1, as can be seen from Figure 1, below 55 ℃, cornstarch has slight gelatinization, gelatinization speed begins to accelerate after 55 ℃, speed sharply increases after about 64 ℃, slows down until complete gelatinization after 68 ℃.This is the crystal characteristic gelatinization curve of cornstarch, experiment gained starch gelatinization temperature T
0=62 ℃; T
e=72 ℃; T`=10 ℃.Tradition number particle method gained starch gelatinization temperature T
0=62 ℃; T
e=72 ℃; T`=10 ℃.The gelatinization point that both record is identical.
The gelatinization degree that several particle methods in gelatinization mid-term record will be less than the measured gelatinization degree of IOD method, low about 10-15%.The gelatinization later stage then is lower than 5%, as what mention in the background technology, in gelatinization process, there is the starch granules that is in part gelatinization state in a large number, classic method has very big deficiency to be that it is parameter with " number ", the gelatinization process of sign starch that can only be roughly even is not a geometric parameter.
Embodiment 2: the gelatinization point and the crystal characteristic gelatinization curve thereof that are used for measuring pea starch.
The pea starch emulsion system of analog-quality concentration (butt) 10% detects its starch gelatinization degree change situation in continuous temperature-rise period.
Be used for to measure pea starch is about 90% emulsion fluid in water cut gelatinization process.
1, the shooting of digital photo.
Comprise the steps and process conditions:
(1) the pea starch emulsion fluid of configuration quality concentration (butt) 10%, balance 1h under the room temperature, firmly stir the starch milk after the balance, its starch that avales is stirred, in system, be more evenly distributed, draw 80 μ l starch milks with glue head dropper, drip two to three rapidly and drip to the glass sheet central authorities that coat a circle fluid sealant at the edge, and with glue head dropper tip paddling, starch milk is evenly distributed, cover another sheet glass sheet then, compress sealing.Starch is sprawled evenly in the film-making requirement microscopic field, and stack is less between the starch granules.
(2) regulate polarizing microscope aperture and photographic exposure time, make the photo exposure amount suitable.Arranging and taking pixel is 2048 * 1536, preserves form TIFF, bit depth 16, and, monochromatic mode. and selecting enlargement factor for use is 100 times order, and Automatic white balance is closed in the object lens combination simultaneously.
(3) slide that makes is placed hot platform, under the good polarizing microscope of debugging, choose the visual field, heating schedule is set is, 40 ℃ of initial temperatures, 80 ℃ of final temperatures, programming rate are 2 ℃/min.
(4) in heating process, the digital camera that links to each other with microscope is taken continuously, makes 40-60 ℃ every 5 ℃, and 60-80 ℃ every 2 ℃ of once sampling.
2, the analysis of digital picture.
The digital picture of taking is imported Image-pro plus software, use AOI (Automated Optical Inspection, " automated optical detection ") the selected whole pictures of rectangle frame select tool, click " measure "-" count/size "-" measure "-select measure "; selected " IOD " item in the drop-down option frame of left side; click " OK "; in the Previous Menu hurdle, click then " edit "; select " convert AOI (s) To Object (s) "; double-click picture, can obtain the IOD value of a pictures.Obtain the IOD value of every number sign indicating number picture according to above step.
3) calculating of gelatinization degree and sign.
Background correction: D=A-B; DG%=1-D/C ╳ 100%.
Physics meaning:
DG: pea starch is gelatinization degree under certain temperature;
A: preliminary survey IOD value refers to the IOD value that original polarisation picture records;
B: background IOD value refers to the IOD value of the picture that the birefringent light of all starch disappears;
C: the actual IOD value of original state, the actual IOD value when referring to the starting point of experiment measuring temperature;
D: actual IOD value refers to that starch in the picture has the integral optical density value of the starch crystals part of birefringent light character.
The pea starch DG% that records and the graph of a relation of temperature as shown in Figure 2, as can be seen from Figure 2, below 45 ℃, the pea starch gelatinization is not obvious, and gelatinization speed begins to accelerate after 45 ℃, and speed sharply increases after about 60 ℃, gelatinization speed is slowed down after 62 ℃, further slows down until complete gelatinization after 72 ℃.The feature course of pea starch gelatinization process, its crystal shows special multistage property, this is the polycrystalline distribution character by C type starch, and the core that near the gelatinization point of the starch part the pyrenoid is absorbed water in advance reduces, and causes mobile equilibrium between the expansion rejection characteristic of effect that gelatinization accelerates and bean starch itself to determine.
Experiment gained starch gelatinization temperature T
0=55.5 ℃; T
e=79.3 ℃; T`=23.8 ℃.Tradition number particle method gained starch gelatinization temperature T
0=59.7 ℃; T
e=75.8 ℃; T`=16.1 ℃.Both have larger difference by the gained gelatinization point, and this is because this method is more responsive to the variation of starch in gelatinization process.Pea starch imbibition at a lower temperature causes the loss of crystalline texture, and after the pea grain pattern disappeared, outer field crystalline texture still needed to continue the gelatinization fully several times that heats up.
The gelatinization degree that several particle methods in gelatinization mid-term record will be less than the measured gelatinization degree of IOD method, low about 10-15%.The gelatinization later stage then is lower than 5%, as what mention in the background technology, in gelatinization process, there is the starch granules that is in part gelatinization state in a large number, classic method has very big deficiency to be that it is parameter with " number ", the gelatinization process of sign starch that can only be roughly even is not a geometric parameter.
Embodiment 3
Be used for part pasting potato starch milk preparation technology's heating-up temperature and the control of heat time heating time, prepare the potato starch products of different gelatinization degrees.
The farina emulsion system of analog-quality concentration (butt) 20% detects its starch gelatinization degree change situation in insulating process.
1, the shooting of digital photo.
Comprise the steps and process conditions:
(1) the farina emulsion fluid of configuration quality concentration (butt) 20%, balance 1.5h under the room temperature, firmly stir the starch milk after the balance, its starch that avales is stirred, in system, be more evenly distributed, draw 50 μ l starch milks with glue head dropper, drip two to three rapidly and drip to the glass sheet central authorities that coat a circle fluid sealant at the edge, and with glue head dropper tip paddling, starch milk is evenly distributed, cover another sheet glass sheet then, compress sealing.Starch is sprawled evenly in the film-making requirement microscopic field, and stack is less between the starch granules.
(2) regulate polarizing microscope aperture and photographic exposure time, make the photo exposure amount suitable, arranging and taking pixel is 2048 * 1536, preserves form TIFF, bit depth 16, monochromatic mode.Selecting enlargement factor for use is 100 times order, and Automatic white balance is closed in the object lens combination simultaneously.
(3) slide that makes is placed hot platform, under the good polarizing microscope of debugging, choose the visual field, heating schedule is set is, 200 ℃/min of programming rate, rising to holding temperature is 62,64,66,68 ℃, insulation 30min.
(4) in heating process, the digital camera that links to each other with microscope is taken continuously, every the 1min once sampling.
2, the analysis of digital picture.
The digital picture of taking is imported Image-pro plus software, use AOI (Automated Optical Inspection, " automated optical detection ") the selected whole pictures of rectangle frame select tool, click " measure "-" count/size "-" measure "-select measure "; selected " IOD " item in the drop-down option frame of left side; click " OK "; in the Previous Menu hurdle, click then " edit "; select " convert AOI (s) To Object (s) "; double-click picture, can obtain the IOD value of a pictures.Obtain the IOD value of every number sign indicating number picture according to above step.
3, the calculating of gelatinization degree and sign.
Background correction: D=A-B;
DG%=1—D?/C╳100%。
Physics meaning:
DG: farina is gelatinization degree under certain temperature;
A: preliminary survey IOD value refers to the IOD value that original polarisation picture records;
B: background IOD value refers to the IOD value of the picture that the birefringent light of all starch disappears;
C: the actual IOD value of original state, the actual IOD value when referring to the starting point of experiment measuring temperature;
D: actual IOD value refers to that starch in the picture has the integration of the starch crystals part of birefringent light character
Optical density value.
The farina DG% that records and the graph of a relation of heat time heating time as shown in Figure 3, as can be seen from Figure 3, heating-up temperature is more high, final gelatinization degree is more big, it is more short to reach final gelatinization degree required time.When being incubated at a lower temperature, reach before the final gelatinization degree, it is few to the gelatinization degree increase of starch to prolong heat time heating time.
When holding temperature was 62,64,66,68 ℃, behind 2,4,9,12min, final gelatinization degree was stabilized in 26,53,70,87% respectively.
Embodiment 4: the gelatinization degree that is used for measuring the converted starch product
Select the acetate tapioca (degree of substitution 0.06) of prepared in laboratory for use, malleableize cornstarch (55 ℃ malleableize 7 hours) is measured it with respect to the gelatinization situation of ative starch.
1, the shooting of digital photo.
Comprise the steps and process conditions:
(1): the starch emulsion fluid of configuration finite concentration (corn 1%, cassava 5%, butt), draw one with glue head dropper, drip on microslide, covered is evenly disperseed drop.
(2): regulate polarizing microscope aperture and photographic exposure time, make the photo exposure amount suitable, arranging and taking pixel is 2048 * 1536, preserves form TIFF, bit depth 16, monochromatic mode.Select enlargement factor 200 times order respectively for use, Automatic white balance is closed in the object lens combination simultaneously.
(3): the slide that makes placed under the polarizing microscope to take obtain three photos: under the photo that starch is evenly distributed under normal optical, polarization light starch be evenly distributed and polarization light under do not have the blank digital pictures of starch granules.
2, the analysis of digital picture.
The digital picture of taking is imported Image-pro plus software, at first handle the photo that starch is evenly distributed under the normal optical: click " measure "-" count/size "-" Manual "-" Select Colors ", utilize Eyedropper Tool wherein, will be all selected with respect to the starch granules that the brilliant white background is grey black, because the option of software default area measurement, so the time directly click " count "-" view "-" statistics ", wherein the value of " Sum " is the area (elemental area) of institute's favored area.
Two remaining polarisation photos, use AOI (Automated Optical Inspection, " automated optical detection ") the selected whole pictures of rectangle frame select tool, click " measure "-" count/size "-" measure "-select measure "; selected " IOD " item in the drop-down option frame of left side; click " OK "; in the Previous Menu hurdle, click then " edit "; select " convert AOI (s) To Object (s) "; double-click picture, can obtain the IOD value of a pictures.
(3): the analysis of digital picture: analyze the original I OD value that obtains whole digital photo with professional image analysis software Image-pro plus 5.0;
The calculating of gelatinization degree and sign:
C=A-B；D=C/E；DG%=1—G?/F╳100%；
Physics meaning:
DG: starch is gelatinization degree under certain temperature;
A: preliminary survey IOD value refers to the IOD value that original polarisation picture records;
B: background IOD value refers to not have the IOD value of the blank picture of starch granules;
C: actual IOD value refers to that starch sample in the picture has the integral optical density value of the starch crystals part of birefringent light character;
The D:OD value refers to that starch sample in the picture has the optical density value of the starch crystals part of birefringent light character;
E: the area of starch granules in the visual field;
F: the OD value of undressed ative starch;
G: the OD value of starch sample after treatment.
(4): measurement result: malleableize cornstarch DG%=15.5%, acetate tapioca 18.5%.
Claims (8)
1. the on-line determination method of a starch gelatinization temperature and gelatinization degree is characterized in that comprising step:
(1) simulation and shooting: the starch milk system of mass concentration 5-20% in simulation practical study and the production technology, the starch milk of configuration same concentrations, behind balance 1-2h under the room temperature, draw the uniform starch milk film-making of 50-80 μ l, place hot platform under polarizing microscope, heat up and heat, the control temperature is lower than 100 ℃; Take sampling continuously by the digital camera that links to each other with microscope;
(2) analysis of digital picture: analyze the original I OD value that obtains whole digital photo with professional image analysis software Image-pro plus 5.0;
(3) calculating of gelatinization degree and sign:
Background correction: D=A-B; DG%=1-D/C ╳ 100%
Wherein, DG%: starch is gelatinization degree under certain temperature;
A: preliminary survey IOD value refers to the IOD value that original polarisation picture records;
B: background IOD value refers to the IOD value of the picture that the birefringent light of all starch disappears;
C: the actual IOD value of original state, the actual IOD value when referring to the starting point of experiment measuring temperature;
D: actual IOD value refers to that starch sample in the picture has the integral optical density value of the starch crystals part of birefringent light character;
(4) determine gelatinization point:
Initial gelatinization point T
0, stop gelatinization point T
eDetermine by following relational expression with gelatinization temperature range T`: T
0=T
DG%=10%T
e=T
DG%=99%T`=T
e-T
0T wherein
DG%=10%Temperature during expression DG%=10%; T
e=T
DG%=99%Temperature during expression DG%=99%.
2. method according to claim 1, it is characterized in that: the starch in the described step (1) is cornstarch, farina, tapioca or pea starch.
3. method according to claim 1 is characterized in that: when heating up in the described step (1), heating rate is less than 5 ℃/min.
4. method according to claim 1 is characterized in that described step (1) takes the sampling spot frequency of sampling and be less than 2 ℃ and get a shooting once.
5. method according to claim 1 is characterized in that: in the digital image acquisition process, photo requires pixel more than 2,000,000 in the step (1), and bit depth is more than 12, monochromatic mode.
6. the non-on-line determination method of a starch burn degree is characterized in that comprising step:
(1) take: configuration quality concentration is the starch milk of 1-5%, draws one with glue head dropper, drips on microslide, and covered is evenly disperseed drop; Place to take under the polarizing microscope and obtain digital pictures;
(2) analysis of digital picture: analyze the original I OD value that obtains whole digital photo with professional image analysis software Image-pro plus 5.0;
(3) calculating of gelatinization degree and sign:
C=A-B；D=C/E；DG%=1—G?/F╳100%
Wherein, DG%: starch is gelatinization degree under certain temperature;
A: preliminary survey IOD value refers to the IOD value that original polarisation picture records;
B: background IOD value refers to not have the IOD value of the blank picture of starch granules;
C: actual IOD value refers to that starch sample in the picture has the integral optical density value of the starch crystals part of birefringent light character;
The D:OD value refers to that starch sample in the picture has the optical density value of the starch crystals part of birefringent light character;
E: the area of starch granules in the visual field;
F: the OD value of undressed ative starch;
G: the OD value of starch sample after treatment.
7. method according to claim 6, it is characterized in that: described starch is cornstarch, farina, tapioca, pea starch or green starch; Or be esterification and crosslinking, the malleableize of feedstock production, the converted starch of amorphous particulate with cornstarch, farina, tapioca, pea starch or green starch.
8. method according to claim 6 is characterized in that: in the digital image acquisition process, photo requires pixel more than 2,000,000 in the described step (1), and bit depth is more than 12, monochromatic mode.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110254158 CN102419305B (en) | 2011-08-31 | 2011-08-31 | Method for determining gelatinization temperature and gelatinization degree of starch |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110254158 CN102419305B (en) | 2011-08-31 | 2011-08-31 | Method for determining gelatinization temperature and gelatinization degree of starch |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102419305A CN102419305A (en) | 2012-04-18 |
| CN102419305B true CN102419305B (en) | 2013-07-03 |
Family
ID=45943819
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 201110254158 Expired - Fee Related CN102419305B (en) | 2011-08-31 | 2011-08-31 | Method for determining gelatinization temperature and gelatinization degree of starch |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102419305B (en) |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102680426A (en) * | 2012-04-28 | 2012-09-19 | 中国农业大学 | Method for rapidly determining starch gelatinization degree of steam-tabletting corn |
| CN106645125B (en) * | 2016-12-29 | 2019-09-03 | 南昌傲农生物科技有限公司 | A kind of measuring method of Gelatinization Degree of Maize Starch |
| CN107782672B (en) * | 2017-09-27 | 2020-03-27 | 珠海格力电器股份有限公司 | Method and device for determining porridge cooking degree |
| CN110064375B (en) * | 2019-04-11 | 2020-09-22 | 华南理工大学 | Preparation method of modified starch with efficient adsorption and controlled release of ethylene |
| CN111721900A (en) * | 2020-06-19 | 2020-09-29 | 佛山市海天（江苏）调味食品有限公司 | Method for detecting alpha-conversion degree of starch and product thereof |
| CN113887309B (en) * | 2021-09-02 | 2024-04-30 | 华南理工大学 | Mask R-CNN-based starch granule identification method |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2096764A (en) * | 1981-04-10 | 1982-10-20 | Ranks Hovis Mcdougall Ltd | Measuring optical rotation |
| CN1158994A (en) * | 1996-03-06 | 1997-09-10 | 王维麒 | Starch burn degree measuring system |
| CN101067623A (en) * | 2007-06-18 | 2007-11-07 | 中国农业大学 | Rice dextrinization temperature and amylose content cooperative determining method |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8039776B2 (en) * | 2008-05-05 | 2011-10-18 | California Institute Of Technology | Quantitative differential interference contrast (DIC) microscopy and photography based on wavefront sensors |
-
2011
- 2011-08-31 CN CN 201110254158 patent/CN102419305B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2096764A (en) * | 1981-04-10 | 1982-10-20 | Ranks Hovis Mcdougall Ltd | Measuring optical rotation |
| CN1158994A (en) * | 1996-03-06 | 1997-09-10 | 王维麒 | Starch burn degree measuring system |
| CN101067623A (en) * | 2007-06-18 | 2007-11-07 | 中国农业大学 | Rice dextrinization temperature and amylose content cooperative determining method |
Non-Patent Citations (8)
| Title |
|---|
| In situ Imaging of Pea Starch in Seeds;Mary L. Parker,Andrew R. Kirby,Victor J. Morris;《FOOD BIOPHYSICS》;20080331;第3卷;第66-76页 * |
| Mary L. Parker,Andrew R. Kirby,Victor J. Morris.In situ Imaging of Pea Starch in Seeds.《FOOD BIOPHYSICS》.2008,第3卷66－76. |
| 李芬芬,等.聚焦光束反射分析仪测定淀粉糊化过程中糊化度的变化.《食品与发酵工业》.2011,第37卷(第2期), |
| 淀粉糊化过程的数字图像分析技术动态监测;高群玉,谢钦;《华南理工大学学报(自然科学版)》;20111231;第39卷(第12期);第105-109页 * |
| 熊易强.饲料淀粉糊化度(熟化度)的测定.《饲料工业》.2000,第21卷(第3期), |
| 聚焦光束反射分析仪测定淀粉糊化过程中糊化度的变化;李芬芬,等;《食品与发酵工业》;20110228;第37卷(第2期);第151-154页 * |
| 饲料淀粉糊化度(熟化度)的测定;熊易强;《饲料工业》;20001231;第21卷(第3期);第30-31页 * |
| 高群玉,谢钦.淀粉糊化过程的数字图像分析技术动态监测.《华南理工大学学报(自然科学版)》.2011,第39卷(第12期), |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102419305A (en) | 2012-04-18 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102419305B (en) | Method for determining gelatinization temperature and gelatinization degree of starch | |
| Borsos et al. | Multi-impurity adsorption model for modeling crystal purity and shape evolution during crystallization processes in impure media | |
| CN104614321B (en) | A kind of crop growing state method of real-time based on spectrum picture | |
| CN102564598B (en) | Method for calibrating and correcting temperature measurement of infrared probe as well as corresponding temperature measuring method | |
| Beaufort | Weight estimates of coccoliths using the optical properties (birefringence) of calcite | |
| EP3270120B1 (en) | Measurement method, measurement device, and program | |
| WO2012142806A1 (en) | Method and device for gold immune quantitative detection on basis of inbuilt ccd image acquisition | |
| CN110243825B (en) | Method for measuring solubility, super-solubility and solution concentration in crystallization process based on online image method | |
| JP2021515203A (en) | Methods and systems for calibrating and using cameras to detect analytes in a sample | |
| Lamb et al. | Digitalization of colourimetric sensor arrays for volatile fatty acid detection in anaerobic digestion | |
| Schwartz et al. | In situ monitoring and control of lysozyme concentration during crystallization in a hanging drop | |
| Mortensen et al. | Real-time monitoring and chemical profiling of a cultivation process | |
| CN110044894B (en) | Colorimetric detection method of triadimenol | |
| CN103760124B (en) | The online concentration detection method of crystallisation by cooling Procedures Drug active component | |
| Soto et al. | Ketoprofen solubility in pure organic solvents using in situ FTIR and UV–Vis and analysis of solution thermodynamics | |
| CN107515198A (en) | A kind of online test method of starch burn degree and gelatinization point | |
| CN108827962B (en) | Egg maturity detection method based on light transmission method | |
| JP2009014355A (en) | Image processor and processing program | |
| Rajabi et al. | Instantaneous mapping of liquid crystal orientation using a polychromatic polarizing microscope | |
| CN104198397B (en) | The method that chamber crop nutrient content is detected under N P and K reciprocation | |
| CN117476124A (en) | Polyvinylidene fluoride auxiliary filling intelligent control management system | |
| CN113640237B (en) | Method for rapidly detecting sucrose and reducing sugar in sugar solution | |
| CN203870015U (en) | On-line concentration detection device for active pharmaceutical ingredient in cooling crystallization process | |
| CN208520494U (en) | A kind of solution saturation temperature self-operated measuring unit | |
| CN111398334A (en) | Novel melting point sliding point instrument and correction measurement method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20130703 Termination date: 20200831 |