CN106770798A - A kind of detection method of feed starch gelatinization degree - Google Patents
A kind of detection method of feed starch gelatinization degree Download PDFInfo
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- CN106770798A CN106770798A CN201710073838.7A CN201710073838A CN106770798A CN 106770798 A CN106770798 A CN 106770798A CN 201710073838 A CN201710073838 A CN 201710073838A CN 106770798 A CN106770798 A CN 106770798A
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Abstract
The invention discloses a kind of detection method of feed starch gelatinization degree, step（1）Sampling；Step（2）Weigh dextrose standard sample；Step（3）Sample treatment：To be gelatinized sample entirely, a in addition is not exclusively to be gelatinized sample to a sample；Respectively to 2mL Glucoamylase Solutions are added in two conical flasks, 40min or so is heated in 40 DEG C of water-baths, then treatment obtains two parts of solution to be measured respectively；Step（4）, standard liquid and two parts of solution to be measured are detected using liquid chromatogram, obtain the retention time and peak area of each component in dextrose standard sample and solution to be measured；The starch burn degree of Feed Sample is：(incomplete gelatinization sample glucose peaks area/be gelatinized sample glucose peaks area completely）×100%.The method can eliminate influence of other reduced sugars to measurement result, make result more accurate.
Description
Technical field
The present invention relates to a kind of detection method of feed starch gelatinization degree.
Background technology
Starch burn degree is also starch curing degree, and its gelatinization degree is higher, represents feed in process by high temperature
The degree ripe with the effect of high pressure is higher.Now, the production of many feeds uses expanding treatment, and feedstuff is through expanding treatment
Afterwards, gelatinization degree and fragrance increase, and palatability is improved, can stimulating animal appetite.Meanwhile, make the organic matters such as starch, protein, fat
Backbone be changed into the degree of short-chain structure and increase, therefore become more easy to digest.
At present, the measure of starch burn degree is mainly by American soybean Association doctor Xiong Yiqiang according to U.S. feed in feed
The assay method that industrial quarters is generally used simplifies（Method is originated：The measure of easily strong feed starch gelatinization degree (curing degree) of bear
[J] feed industries, 2000,21 (3):30-31）.Altogether after heat, enlarged volume, viscosity rises, as amorphism for starch and water
Starch, easily glucose is turned under the state by Glucoamylase hydrolysis, and it is exactly that make use of shallow lake that the above method determines feed starch gelatinization degree
This characteristic of powder.Wherein, the method for the glucose reduced sugar after hydrolysis is determined, but reduced sugar and non-glucose one kind,
So sometimes other reduced sugars can be impacted to result in feed.
The content of the invention
It is an object of the invention to provide a kind of detection method of feed starch gelatinization degree, to eliminate other reduced sugars to surveying
Determine the influence of result, make result more accurate.
In order to reach above-mentioned purpose, the technical scheme is that：
A kind of detection method of feed starch gelatinization degree, comprises the steps of：
Step（1）, sampling：The two parts of mesh sieve of mistake 40 Feed Samples identical in quality are weighed, 0.0001g is accurate to；
Step（2）, the dextrose standard sample of certain mass is weighed, added water constant volume with 100mL volumetric flasks, obtain standard liquid；
Step（3）, sample treatment：Respectively by two parts of steps（1）In sample be placed in addition 50mL anhydrous sodium acetates-acetate buffer
In the 150mL conical flasks of liquid, a copy of it sample boiling water bath heating 40min ± 4min in water-bath is taken, then use running water
Shower is cooled down, and sample is as gelatinized entirely, and a in addition is not exclusively to be gelatinized sample；Respectively to addition 2mL sugar in two conical flasks
Change enzyme solutions, 40min ± 4min is heated in 40 DEG C of water-baths, be then respectively adding 2mL sulfuric acid solutions, sequentially added after shaking up
2mL sodium tungstate solutions, shake up again；After liquid in two conical flasks is transferred in 100mL volumetric flasks into the constant volume that adds water respectively
Filtered with filter paper, collect filtrate, obtain two parts of solution to be measured；
Step（4）, standard liquid and two parts of solution to be measured are detected using liquid chromatogram, obtain dextrose standard sample and treat
Survey the retention time and peak area of each component in solution；The starch burn degree of Feed Sample is：(not exclusively it is gelatinized sample grape
Sugared peak area/be gelatinized sample glucose peaks area completely）×100%.
Wherein, step（1）Middle Feed Sample sample weighting amount control is advisable between 0.4-1g, in addition, this method is equally applicable
In feedstuff（Such as popcorn）The measure of starch burn degree.
Wherein, step（2）Middle dextrose standard sample sample weighting amount is 0.0500-0.1000g, is accurate to 0.0001g, to judge
Treat in test sample used by glucose appearance time, glucose in Feed Sample is only judged by the chromatogram of dextrose standard sample
Go out peak position.
Wherein, present invention water used（The water that i.e. all preparation of reagents and mobile phase are used）It is deionized water.
Wherein, step（3）Middle anhydrous sodium acetate-acetate buffer liquid making method is as follows：4.1g anhydrous sodium acetates are taken to be dissolved in
In 200mL water, plus 3.7mL acetic acid, 1000mL is settled to water, pH value of solution is between 4.4-4.7.
Wherein, step（3）Middle sulfuric acid solution and sodium tungstate solution are protein precipitant, can remove the albumen in sample.Sulphur
Acid solution compound method：The 10mL concentrated sulfuric acids are diluted with water to 100mL；Sodium tungstate solution compound method：Take 12.0g sodium tungstates molten
In 100mL water.
Wherein, step（3）Used in carbohydrase enzyme activity be 12000U/g.Enzyme solutions compound method is as follows：1g is taken to answer
Close amylase and be dissolved in 10mL steps（3）Middle anhydrous sodium acetate-acetate buffer, after shaking repeatedly, filtering takes filtrate, now with now
Match somebody with somebody.Such as according to the present invention operation when, can according to calculated using the actual enzyme activity of carbohydrase, the enzyme solutions enzyme activity of preparation is not with
It is defined less than the present invention.
Wherein, step（4）With water as mobile phase, the liquid chromatogram uses isocratic elution mode to described liquid chromatogram.
After using the above method, compared with prior art, beneficial effects of the present invention are embodied in following several respects：
（1）Interference of other reduced sugars to measurement result can be eliminated；
（2）Surveying instrument measure using liquid chromatogram can process more samples, and operating efficiency is improve to a certain extent；
（3）Measurement result computing formula is simple, is obtained a result by only needing glucose peak area ratio.
In a word, after the present invention is by Feed Sample Glucoamylase hydrolysis to be measured, glucose is measured using liquid chromatogram
（The content of glucose in glucose peaks area reflection sample）, influence of other reduced sugars to measurement result can be effectively eliminated,
So that result is more accurate.
Brief description of the drawings
Fig. 1 is dextrose standard sample chromatogram；
Fig. 2 is incomplete gelatinization sample chromatogram figure；
Fig. 3 is to be gelatinized sample chromatogram figure completely.
Specific embodiment
Embodiments of the invention are elaborated below, the present embodiment is carried out under premised on technical solution of the present invention
Implement, give detailed implementation method and specific operating process, but protection scope of the present invention is not limited to following implementations
Example.
Embodiment 1
The instrument and chromatographic condition that the present embodiment is used are as follows：
1. instrument and equipment
Electronic balance（It is accurate to 0.0001g）, laboratory Conventional glass vessel, 0.22 μm of micropore filtering film, solvent filter, band
The high performance liquid chromatography of time difference shading detector.
2. chromatographic condition
Chromatographic column：agilent Hi-Plex H（8 μm, 7.7mm × 300mm）
Column temperature：70℃
Mobile phase：Water
Sample size：20μL
A kind of detection method of starch burn degree, comprises the following steps：
（1）Weigh the two parts of mesh sieve of mistake 40 mixed feed sample 0.8000g identical in quality.
（2）The dextrose standard sample of 0.1000g is weighed, is added water constant volume with 100mL volumetric flasks, obtained standard liquid and cross 0.22
After μm organic miillpore filter of syringe needle upper machine testing is carried out by chromatographic condition.The chromatogram for obtaining is as shown in Figure 1.Portugal as shown in Figure 1
The retention time of grape saccharide is 9.552min.
（3）Respectively by two parts of steps（1）In sample be placed in the 150mL for adding 50mL anhydrous sodium acetates-acetate buffer
In conical flask, a copy of it sample boiling water bath heating 40min or so in water-bath is taken, then cooled down with running water shower, i.e.,
It is full gelatinization sample；A in addition is incomplete gelatinization sample；Respectively to addition 2mL Glucoamylase Solutions in two conical flasks, in
40min or so is heated in 40 DEG C of water-baths, 2mL sulfuric acid solutions are then respectively adding, 2mL sodium tungstates is sequentially added after shaking up molten
Liquid, shakes up again；Filtered with filter paper after liquid in two conical flasks is transferred in 100mL volumetric flasks into the constant volume that adds water respectively,
Filtrate is collected, two parts of solution to be measured are obtained.Two parts of solution to be measured press chromatostrip after crossing 0.22 μm of organic miillpore filter of syringe needle respectively
Part carries out machine testing.The chromatogram for obtaining is as shown in Figures 2 and 3.Glucose in solutions retention time to be measured and peak area are such as
Shown in table 1.
The mixed feed of table 1 glucose in solutions retention time to be measured and peak area
| Project | Retention time（min） | Peak area |
| Not exclusively it is gelatinized sample | 9.553 | 562013.7 |
| Sample is gelatinized completely | 9.552 | 1030528.1 |
The starch burn degree of the mixed feed sample=（562013.7/1030528.1）×100%=54.53%
Embodiment 2
Using popcorn as sample, using with the identical operating procedure of embodiment 1, the final result such as table 2 of gained
It is shown.
The popcorn of table 2 glucose in solutions retention time to be measured and peak area
| Project | Retention time（min） | Peak area |
| Not exclusively it is gelatinized sample | 9.556 | 1315061.5 |
| Sample is gelatinized completely | 9.559 | 1542413.2 |
The starch burn degree of the popcorn sample=（1315061.5/1542413.2）×100%=85.26%
Test example 1
Above-mentioned mixed feed sample and popcorn sample are surveyed by control group of existing spectrophotometric determination method
Fixed, two methods of the measurement result of same sample is as shown in table 3：
The measurement result of the starch burn degree of table 3
| Sample | Control group | Experimental group |
| Mixed feed | 60.52% | 54.51% |
| Popcorn | 86.14% | 85.26% |
A small amount of whey powder is added in the mixed feed production process that the present invention is used, and the lactose in whey powder is reduced sugar
One kind, the spectrophotometer method that control group is used is a kind of method for determining reduced sugar, and its result is determined comprising glucose, breast
The reduced sugar of sugar and other species, exactly because this reason, as shown in Table 3, its result is more of the invention higher.Popcorn is
A kind of feedstuff, does not contain the reduced sugar of other species such as lactose, so, the knot of popcorn sample controls group and experimental group
Fruit closer to.
The starch burn degree that the present invention passes through liquid chromatogram measuring feed, reduced sugar is to result beyond eliminating glucose
Interference, so, it is as a result more accurate.The use of liquid chromatograph simultaneously can determine more samples, so be conducive to improving
Operating efficiency.
Claims (7)
1. a kind of detection method of feed starch gelatinization degree, it is characterised in that comprise the steps of：
Step（1）, sampling：The two parts of mesh sieve of mistake 40 Feed Samples identical in quality are weighed, 0.0001g is accurate to；
Step（2）, dextrose standard sample is weighed, added water constant volume with 100mL volumetric flasks, obtain standard liquid；
Step（3）, sample treatment：Respectively by two parts of steps（1）In sample be placed in addition 50mL anhydrous sodium acetates-acetate buffer
In the 150mL conical flasks of liquid, a copy of it sample boiling water bath heating 40min ± 4min in water-bath is taken, then use running water
Shower is cooled down, and sample is as gelatinized entirely, and a in addition is not exclusively to be gelatinized sample；Respectively to addition 2mL sugar in two conical flasks
Change enzyme solutions, 40min ± 4min is heated in 40 DEG C of water-baths, be then respectively adding 2mL sulfuric acid solutions, sequentially added after shaking up
2mL sodium tungstate solutions, shake up again；After liquid in two conical flasks is transferred in 100mL volumetric flasks into the constant volume that adds water respectively
Filtered with filter paper, collect filtrate, obtain two parts of solution to be measured；
Step（4）, standard liquid and two parts of solution to be measured are detected using liquid chromatogram, obtain dextrose standard sample and treat
Survey the retention time and peak area of each component in solution；The starch burn degree of Feed Sample is：(not exclusively it is gelatinized sample grape
Sugared peak area/be gelatinized sample glucose peaks area completely）×100%.
2. a kind of detection method of feed starch gelatinization degree as claimed in claim 1, it is characterised in that step（1）Middle feed sample
Product sample weighting amount is controlled between 0.4000-1.000g.
3. a kind of detection method of feed starch gelatinization degree as claimed in claim 1, it is characterised in that step（2）Middle glucose
Standard items sample weighting amount is 0.05-0.1g, is accurate to 0.0001g.
4. a kind of detection method of feed starch gelatinization degree as claimed in claim 1, it is characterised in that step（3）In anhydrous second
Sour sodium-acetate buffer liquid making method is as follows：4.1g anhydrous sodium acetates are taken to be dissolved in 200mL water, plus 3.7mL acetic acid, it is fixed with water
Hold to 1000mL, pH value of solution is between 4.4-4.7.
5. a kind of detection method of feed starch gelatinization degree as claimed in claim 1, it is characterised in that step（3）Middle sulfuric acid is molten
Liquid and sodium tungstate solution are protein precipitant, sulfuric acid solution compound method：The 10mL concentrated sulfuric acids are diluted with water to 100mL；Wolframic acid
Sodium solution compound method：12.0g sodium tungstates are taken to be dissolved in 100mL water.
6. a kind of detection method of feed starch gelatinization degree as claimed in claim 1, it is characterised in that step（3）Used in
Carbohydrase enzyme activity be 12000U/g；Enzyme solutions compound method is as follows：Take 1g composite alpha-amylases and be dissolved in 10mL steps（3）In it is anhydrous
Sodium acetate-acetic acid buffer solution, after shaking repeatedly, filtering takes filtrate, matching while using.
7. a kind of detection method of feed starch gelatinization degree as claimed in claim 1, it is characterised in that step（4）Described liquid
With water as mobile phase, the liquid chromatogram uses isocratic elution mode to phase chromatogram.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107478644A (en) * | 2017-07-13 | 2017-12-15 | 漳州傲农牧业科技有限公司 | A kind of method of starch burn degree in measure feed |
| CN108663478A (en) * | 2018-08-24 | 2018-10-16 | 天邦食品股份有限公司 | A kind of method of starch burn degree in Accurate Determining pannage |
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| CN1960643A (en) * | 2004-05-14 | 2007-05-09 | 株式会社芳珂 | Germinating brown rice |
| CN102613659A (en) * | 2012-04-11 | 2012-08-01 | 苏州先阔生物科技有限公司 | Composition capable of resisting starch retrogradation and application therof |
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2017
- 2017-02-10 CN CN201710073838.7A patent/CN106770798A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1960643A (en) * | 2004-05-14 | 2007-05-09 | 株式会社芳珂 | Germinating brown rice |
| CN102613659A (en) * | 2012-04-11 | 2012-08-01 | 苏州先阔生物科技有限公司 | Composition capable of resisting starch retrogradation and application therof |
Non-Patent Citations (3)
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| 中山医学院第二附属医院检验科: "《临床生化检验学基础》", 31 January 1977, 广州新华印刷厂 * |
| 梁龙等: "高效液相色谱法测定混菌发酵乳中乳糖、葡萄糖及半乳糖含量的变化", 《食品工业科技》 * |
| 熊易强: "饲料淀粉糊化度（熟化度）的测定", 《饲料工业》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107478644A (en) * | 2017-07-13 | 2017-12-15 | 漳州傲农牧业科技有限公司 | A kind of method of starch burn degree in measure feed |
| CN108663478A (en) * | 2018-08-24 | 2018-10-16 | 天邦食品股份有限公司 | A kind of method of starch burn degree in Accurate Determining pannage |
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Application publication date: 20170531 |