CN104062309A - Method for measuring relative crystallinity of starch - Google Patents

Method for measuring relative crystallinity of starch Download PDF

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Publication number
CN104062309A
CN104062309A CN201410343075.XA CN201410343075A CN104062309A CN 104062309 A CN104062309 A CN 104062309A CN 201410343075 A CN201410343075 A CN 201410343075A CN 104062309 A CN104062309 A CN 104062309A
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peak
area
noncrystalline
region
peak crystallization
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CN104062309B (en
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熊飞
余徐润
周亮
张静
于恒
王�忠
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Yangzhou University
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Yangzhou University
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Abstract

The invention relates to a method for measuring the relative crystallinity of starch. The method comprises the steps of obtaining an XRD (X-ray diffraction) spectrum of a starch sample to be analyzed; processing an XRD spectral graph through Photoshop software, marking regions of crystallized peaks and non-crystallized peaks through the Photoshop software, respectively clicking the regions, filling the regions with colors with different grey scales, and storing an image; opening an image to be processed through Image-ProPlus software to calculate the area of the regions of crystallized peaks and non-crystallized peaks, and calculating the relative crystallinity according to the calculation result. The method is easy to operate, is accurate and is high in operability, and errors can be reduced to an extreme.

Description

A kind of method of measuring starch relative crystallinity
Technical field
The invention belongs to bio-science, technical field of food science, be specifically related to a kind of method of measuring starch relative crystallinity.
Background technology
Starch crystals degree is an important parameter that characterizes starch granules crystallographic property, is also the important parameter that characterizes starch material series products character, and its size directly affects the application performance of starch product, the physical and mechanical property of starch material.Researcher's the concern extremely both at home and abroad of the research of quick, easy, the reliable determination method of starch and starch derivative crystallinity in recent years.According to the literature, X-ray diffraction method (XRD) is to measure one of the most frequently used method of starch granules crystallinity, and the methods such as Herman method, Wakelin method and anticipatory remark mountain method all can be measured the crystallinity of starch granules, but they all have shortcoming separately.Crystalline region in Herman method and amorphous area are demarcated entirely by rule of thumb, experiential operating sheerly when measurement, and arbitrariness is very large.Two " standard specimens " in Wakelin method are all nonstandard, disadvantage is to cause the crystallinity of measuring to be always tending towards higher compared with real crystallinity, but this method is that diffracted intensity subtracts each other at Data processing, the dispersion factors of a lot of impact experiments are died away or without correction.Anticipatory remark mountain method has been ignored different and other dispersion factors impact on diffracting spectrum of X ray on crystalline region and amorphous region diffraction effect etc., makes result produce error.
Summary of the invention
In order to solve the deficiencies in the prior art, the invention provides a kind of method of measuring starch relative crystallinity, the method that combines to analyze starch XRD wave spectrum calculation of starch relative crystallinity by Photoshop and Image Pro-Plus software has science, rationality and accuracy, has substantially overcome above assay method existent defect and deficiency.
A kind of method of measuring starch relative crystallinity of the present invention, comprises the following steps:
(1) obtain the XRD wave spectrum of starch sample to be analyzed; Process XRD wave spectrogram with Photoshop software, fill with different greyscale color respectively in the region that marks peak crystallization and noncrystalline peak, preserves image;
(2) with the image of preserving in Image-Pro Plus software opening steps (1), calculate peak crystallization and noncrystalline peak region area, then calculate accordingly relative crystallinity; Relative crystallinity=[peak crystallization area/(peak crystallization area+noncrystalline peak area)] × 100%.
Wherein, Photoshop software is processed the concrete operations of XRD wave spectrogram and is in step (1): draw straight line 4 °-30 ° of wave spectrum near crest base portion, then add anchor point with pen tool in the main bottom of peak crystallization and the baseline at noncrystalline peak, the level and smooth curve of each anchor point is connected with convert point tool, then uses paintbrush tool stroke path; Finally with magic wand menu, the region at noncrystalline peak between the peak crystallization of smooth curve top and curve and straight line chosen respectively and with the color filling of different gray scales, preserved image.
Reference area method concrete in step (2) is: click count/size icon, in count/size window, click slect colors and choose peak crystallization region, software can be identified this field color automatically, after clicking close, return count/size window, in menu, select successively Measure-selectmeasurements to select area (Area), return to rear some count, now software has completed the calculating of peak crystallization region area, clicks view-statistics and can obtain area data.In like manner can calculate noncrystalline peak region area.
The present invention compared with prior art, has following beneficial effect:
(1) whole process operation is simple, and common researcher practises getting final product complete operation a little, compares and has saved a lot of time compared with forefathers' general curve graphing method.
(2) what the drafting of curve was used is the pen tool in Photoshop, and other instrument of comparing is more professional, more accurate, handling better.
(3) the selected color region of magic wand menu is very concrete, careful about pixel scale, there will not be the loss of certain region area.
(4) what the identification of color adopted is the Eyedropper tool of Image-Pro Plus software, can ensure that like this area in each in advance painted region can come out accurately, and error has been reduced to the limit.
Brief description of the drawings
Fig. 1 is wheaten starch XRD wave spectrum;
Fig. 2 is the wave spectrum that adds straight line with Photoshop software between 4 °-30 °;
Fig. 3 is the wave spectrum adding after anchor point;
Fig. 4 is the wave spectrum that connects each anchor point with smooth curve;
Fig. 5 is the wave spectrum with paintbrush tool stroke path;
Fig. 6 is the wave spectrum of filling peak crystallization region and region, noncrystalline peak with different greyscale color;
Fig. 7 has been that peak crystallization region area calculates;
Fig. 8 is peak crystallization region area statistics;
Fig. 9 has been that noncrystalline peak region area calculates;
Figure 10 is non-peak crystallization region area statistics;
Figure 11 is the operating process that starch relative crystallinity calculates.
Embodiment
Specific operation process taking wheaten starch XRD wave spectrum as materials show this method is as Figure 11 below:
1. the XRD wave spectrum of wheaten starch grain
Wheaten starch after separating is absorbed water one week in the closed container that fills saturated nacl aqueous solution, then use polycrystal X ray diffractometer (XRD) analysis, wave spectrum is as Fig. 1.
2. draw straight line (Fig. 2) 4 °-30 ° of wave spectrum near crest base portion with Photoshop CS4 software, then use the pen tool in Photoshop to add anchor point (Fig. 3) in the bottom of each main peak crystallization and the baseline at noncrystalline peak, then utilize convert point tool that the smooth curve of each anchor point is connected to (Fig. 4), utilize paintbrush tool that path is filled to black lines (Fig. 5).Use the magic wand menu in Photoshop menu to divide the color filling wearing with different gray scales (Fig. 6) by the region between smooth curve top and curve and straight line.
3. open wave spectrogram after treatment with Image-Pro Plus software, select successively Measure-count/size, in count/size window, click select colors and choose peak crystallization field color, software can be identified this color region automatically, after clicking close, return to count/size window, in menu, select successively Measure-select measurements to select area (Area), return to rear some count, now software has completed the calculating (Fig. 7) of peak crystallization region area, click view-statistics and can obtain area data (Fig. 8), in like manner can calculate blue region area (Fig. 9, Figure 10).
4. the calculating of starch relative crystallinity, relative crystallinity=[A1/ (A1+A2)] × 100%=[24482/ (24482+45366)] × 100%=35.05%.

Claims (3)

1. measure a method for starch relative crystallinity, it is characterized in that comprising the following steps:
(1) obtain the XRD wave spectrum of starch sample to be analyzed; Process XRD wave spectrogram with Photoshop software, fill with different greyscale color respectively in the region that marks peak crystallization and noncrystalline peak, preserves image;
(2) with the image of preserving in Image-Pro Plus software opening steps (1), calculate peak crystallization and noncrystalline peak region area, then calculate accordingly relative crystallinity; Relative crystallinity=[peak crystallization area/(peak crystallization area+noncrystalline peak area)] × 100%.
2. method according to claim 1, it is characterized in that Photoshop software in step (1) processes the concrete operations of XRD wave spectrogram and be: draw straight line 4 °-30 ° of wave spectrum near crest base portion, then add anchor point with pen tool in the main bottom of peak crystallization and the baseline at noncrystalline peak, the level and smooth curve of each anchor point is connected with convert point tool, then uses paintbrush tool stroke path; Finally with magic wand menu, the region at noncrystalline peak between the peak crystallization of smooth curve top and curve and straight line chosen respectively and with the color filling of different gray scales, preserved image.
3. method according to claim 1, it is characterized in that the concrete operations that calculate peak crystallization and noncrystalline peak region area described in step (2) are: click count/size icon, in count/size window, click slect colors and choose peak crystallization region, software can be identified this field color automatically, after clicking close, return count/size window, in menu, select successively Measure-select measurements to select area A rea, return to rear some count, now software has completed the calculating of peak crystallization region area, click view-statistics and can obtain area data, in like manner can calculate noncrystalline peak region area.
CN201410343075.XA 2014-07-17 2014-07-17 Method for measuring relative crystallinity of starch Expired - Fee Related CN104062309B (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106645239A (en) * 2017-01-08 2017-05-10 扬州大学 Graph analysis method for starchy small-angle X-ray scattering spectrum parameters
CN107607565A (en) * 2017-08-30 2018-01-19 华能国际电力股份有限公司 Method for measuring gamma' phase volume fraction in nickel-based single crystal superalloy
CN113670959A (en) * 2021-07-21 2021-11-19 扬州大学 Novel method for analyzing relative crystallinity of starch

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
徐斌 等: "粉末X射线衍射图谱计算植物淀粉结晶度方法的探讨", 《植物学报》 *
陈翠兰 等: "淀粉结晶度计算的新方法", 《食品科学》 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106645239A (en) * 2017-01-08 2017-05-10 扬州大学 Graph analysis method for starchy small-angle X-ray scattering spectrum parameters
CN107607565A (en) * 2017-08-30 2018-01-19 华能国际电力股份有限公司 Method for measuring gamma' phase volume fraction in nickel-based single crystal superalloy
CN113670959A (en) * 2021-07-21 2021-11-19 扬州大学 Novel method for analyzing relative crystallinity of starch

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