CN101799389B - Method for determining correlationship of lignin content and fiber quality in cotton fiber - Google Patents
Method for determining correlationship of lignin content and fiber quality in cotton fiber Download PDFInfo
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- CN101799389B CN101799389B CN201010143263XA CN201010143263A CN101799389B CN 101799389 B CN101799389 B CN 101799389B CN 201010143263X A CN201010143263X A CN 201010143263XA CN 201010143263 A CN201010143263 A CN 201010143263A CN 101799389 B CN101799389 B CN 101799389B
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Abstract
The invention provides a method for determining correlationship of lignin content and fiber quality in cotton fiber. The traditional Klason method is improved to measure the lignin content in the cotton fiber so as to build the relevant relationship of lignin content with fiber length, specific strength as well as Micronaire value and a regression equation. The invention enriches fiber quality evaluation ways and has the positive meaning for guiding cotton breeding and production.
Description
One, technical field
The invention belongs to biochemical analysis field, relate to a kind of fiber quality check and analysis method, be specially a kind of method of establishing content of lignin and fiber quality correlationship in the cotton fiber.
Two, background technology
Cotton fiber by the ovule epidermal cell in prefecundation after differentiation projection, elongation, secondary wall thickens and dewater maturation and form.Chinese scholars is thought and is not contained the lignin that forms the cell membrane cross-linked structure in the ripe cotton fiber, but project team of the present invention contains the lignin that forms the cell membrane cross-linked structure through cotton fiber quality being formed the big quantity research of mechanism in the cotton fiber by molecular biology experiment, Fluirescence observation, multiple biochemical analysis method proof maturation.And propose lignin and be cotton fiber cell wall important composition composition and form cross-linked structure, influence the growth, intensity, morphogenesis of cell membrane and the resistance of biological and abiotic stress with the polysaccharide of cell membrane.Current research shows that the phenylpropyl alcohol alkane metabolic pathway that forms lignin is the second largest metabolic pathway that is only second to the cellulose metabolic pathway in the cotton fiber development simultaneously, the expression that raises up of related gene is grown synchronously with the cotton fiber secondary wall, so the content of lignin may have material impact to cotton fiber quality.Yet also be in blank both at home and abroad for the relation research between content of lignin in the cotton fiber and fiber quality.Aspect the cotton fiber quality Analysis and Identification, do not utilize the concrete practice of content of lignin as fiber quality Indirect evaluation index yet.
Modern textile industry is to stress to emphasize interior qualities such as fiber specific strength and mic value on the long basis of certain suede to the requirement of raw cotton quality.Wherein the cotton fiber specific strength is the most important index of quality of raw cotton, with spinning yarn quality confidential relation is arranged.Have and discover that the cotton fiber specific strength is relevant with cellulosic supramolecular structure with the thickness of secondary wall, simultaneously also with cotton fiber in non-fiber polysaccharide crosslinked relevant.Wherein lignin is the chief component of the cross-linked structure material of non-fiber polysaccharide, and therefore the relation of content of lignin and cotton fiber quality has crucial meaning for the biochemical basis that correct understanding cotton fiber quality forms in detection and the definite cotton fiber.
The Klason method also is direct method, sulfuric acid process, is the method for the analysis lignin of classics, compares with ultraviolet spectrophotometry, need not preparing standard solution, the mensuration program is simple, and not only quantification but also precision are higher, makes it obtain using widely in mensuration plant lignin.This method mainly is to be used to measure materials such as the higher relatively peanut shell of content of lignin, timber, rice husk, tobacco leaf, bast-fibre at present.But because the cotton fiber content of lignin is very low, this assay method can not directly be spreaded to the detection that is applied to content of lignin in the cotton fiber.
Three, summary of the invention
The purpose of this invention is to provide a kind of method that detects and establish content of lignin and fiber quality correlationship in the cotton fiber.
The method of content of lignin and fiber quality correlationship comprises the steps: in the establishment cotton fiber provided by the invention
A, sample collecting and preparation: gather ripe cotton fiber sample 30-50 part, carry out cotton fiber quality and detect, record fibre length, specific strength, the mic value of each sample;
B, sample pre-treatments: remove non-cotton fiber impurity such as blade and kind shell fragment, take by weighing the 5-10g cotton sample, with twice of homogenization buffer solution for cleaning, clean twice with 80% acetone again, pure acetone cleans once, clean all vortex, extruding and cotton fiber is placed in the metal clip garlic device extrudes residual liquid repeatedly at every turn, clean the 45 ℃ of dry for standby of cotton sample after finishing;
C, filter paper are handled: fine and close quantitative filter paper is soaked the back fully with dilute sulfuric acid be washed till neutrality with distilled water, dry to constant weight in 60 ℃ of baking ovens;
D, content of lignin are measured: take by weighing the 2-3g sample and place in the 50ml tool plug glass bottle, add the 10-20ml concentrated sulphuric acid of precooling in 4 ℃ of refrigerators in advance, fully behind the mixing, place 1-3h under the room temperature, change in the 1L autoclaving bottle, sulfuric acid concentration when adding distil water is diluted to the filter paper processing, bottleneck sealing back high-pressure sterilizing pot pyroprocessing 1h naturally cools to room temperature; Fine and close quantitative filter paper with the oven dry constant weight filters, be washed with distilled water to filter paper neutrality, filter paper is placed in 60 ℃ of baking ovens together with residue dries to constant weight, 575 ℃ of following ashing in the muffle furnace, claim ash content weight, the difference of the weight of filter paper deducts the weight that ash content weight is lignin, and each cotton sample repeats 2-3 time and gets its mean value;
E, correlation analysis: with content of lignin in the cotton fiber is dependent variable y, and fibre length, specific strength, mic value are respectively independent variable X
1, X
2, X
3, statistical study obtains content of lignin and fiber quality correlationship regression equation, and carries out statistical test.
The present invention is improved the Klason method of traditional analysis content of lignin, example weight is increased to 2g, boiling reflux in the sample processing procedure commonly used changed in high-pressure sterilizing pot, keep 1h, can reduce the loss of acid in the heating process like this and the pollution of surrounding environment.And filter paper in the Klason method dried more than 100 ℃ with crucible change into 60 ℃ of oven dry of fine and close quantitative filter paper (φ 15cm), because filter paper is handled under the same conditions before and after filtering, can control test error preferably, break when also having avoided filter paper after 3% sulfuric acid treatment at high temperature to dry and situation about can't use takes place.
Adopt this method on based on traditional sulfuric acid process (Klason method) experimental facilities condition basis, to finish,, cancelled reflow process, and reduced the filter paper bake out temperature, thereby guaranteed the accuracy of testing result owing to strengthened example weight.Compare with ultraviolet spectrophotometry, need not preparing standard solution, the mensuration program is simple, and can accomplish the mathematical computations of weighing result, not only quantification but also precision are higher, the little higher detection precision that guaranteed of systematic error, thus content of lignin and fiber quality correlationship regression equation can on the basis of statistical study, be set up, and determined related coefficient has higher level of significance.This method is the correct biochemical basis that cotton fiber quality forms of understanding, and enriches the evaluation approach of fiber quality, instructs cotton production to have positive effect.Particularly in breeding, select the target gene of decision content of lignin, and on cultivation step, form influence factor, thereby the indirect adjustments and controls cotton fiber quality has reality and important meaning by the control lignin.
Four, embodiment
Embodiment 1
1, instrument and reagent
High-pressure sterilizing pot, constant temperature thermostatic drying chamber, HVI SPECTRUM-I type cotton fiber quality detector.
Tris-HCl (Beijing is glad through company of section); Qu Latong x-100 analyzes pure (Beijing is glad through company of section); NaCl analyzes pure (Xi'an chemical reagent factory); Acetone is analyzed pure (the many chemical reagent of Zhengzhou moral factory); The concentrated sulphuric acid is analyzed pure (vast Fine Chemical Co., Ltd is contained in Tianjin).
Even matter damping fluid (50mM Tris-HCl, 1% song draw logical x-100,1M NaCl, pH8.3).
72% sulfuric acid (w/w), 4 ℃ of refrigerators are preserved.
2, cotton sample collecting and fiber quality are measured
Gather 40 parts in land for growing field crops natural maturity cotton fiber sample, pick out the blade of sneaking in the cotton fiber and plant non-cotton fiber impurity such as shell, adopt HVI SPECTRUM-I type cotton fiber quality detector to measure cotton fiber quality weighing apparatus definiteness mark: fibre length, specific strength, mic value.
3, cotton sample pre-treatments
Every sample takes by weighing the 10g cotton sample, with homogenization buffer solution for cleaning cotton fiber twice, cleans once to avoid the interference of soluble substance to analyzing with twice of 80% acetone cleaning and pure acetone respectively again.Clean all vortex, extruding repeatedly at every turn, cotton fiber be placed in the metal clip garlic device and extrude residual liquid, 45 ℃ of dry for standby at last.
4, filter paper is handled
Fine and close quantitative filter paper (Φ 15cm) soaks the back fully with 3% dilute sulfuric acid and is washed till neutrality with distilled water, dries to constant weight in 60 ℃ of baking ovens.
5, the sample content of lignin is measured
Take by weighing dry sample 2.0g, place in the 50ml tool plug centrifugal bottle, add 15ml 72% sulfuric acid of precooling in 4 ℃ of refrigerators in advance, fully behind the mixing, place 2h under the room temperature and make fibre composition be hydrolyzed into polysaccharide or monose, change in the 1L autoclaving bottle, adding distil water is diluted to 560ml then.After the sealing reagent bottle is positioned in the high-pressure sterilizing pot, 121 ± 3 ℃ keep 1h down, and autoclave is lowered the temperature naturally, is cooled to room temperature.Filter with the quantitative filter paper of in 60 ℃ of baking ovens, drying in advance, and be washed with distilled water to neutrality (dropping 10%BaCl in the filtrate to constant weight
2Not having precipitation produces), filter paper is placed in 60 ℃ of baking ovens together with residue dries to constant weight, ash content weight is measured in 575 ℃ of following ashing in the muffle furnace.Each cotton sample repeats 3 times, and content of lignin is averaged.
The difference of the weight of filter paper deducts the weight that ash content weight is lignin.The computing formula of its lignin degree is:
Content of lignin %={ (G2-G1)-G3}/2 * 100
In the formula: the filter paper after the G2-oven dry is together with residue heavy (gram)
The weight of G1-filter paper (gram)
G3-ash content heavy (gram)
6, correlation analysis
Length, specific strength, mic value and the content of lignin of above-mentioned each sample that records are carried out statistical study, calculate related coefficient and regression equation.
The index of quality and the content of lignin of 40 duplicate samples that present embodiment records see Table 1
Table 1 cotton fiber quality index and content of lignin
| Sample number into spectrum | Length (mm) | Intensity (CN/tex) | Mic value | Lignin mean value (%) (± SE) |
| 1 | 31.50 | 34.9 | 4.21 | 0.617±0.026 |
| 2 | 34.09 | 33.1 | 4.29 | 0.438±0.029 |
| 3 | 32.31 | 37.4 | 4.25 | 0.550±0.025 |
| 4 | 26.49 | 24.8 | 4.78 | 1.892±0.040 |
| 5 | 30.40 | 23.9 | 4.52 | 0.750±0.003 |
| 6 | 33.99 | 37.2 | 3.86 | 0.658±0.011 |
| 7 | 25.81 | 31.5 | 5.53 | 0.573±0.016 |
| 8 | 28.58 | 26.8 | 3.86 | 1.090±0.042 |
| 9 | 28.73 | 28.8 | 4.43 | 0.633±0.019 |
| 10 | 29.69 | 29.1 | 4.30 | 0.632±0.017 |
| 11 | 28.75 | 30.5 | 4.82 | 0.637±0.022 |
| 12 | 30.35 | 34.0 | 3.93 | 1.040±0.080 |
| 13 | 35.69 | 33.8 | 4.34 | 0.442±0.007 |
| 14 | 29.31 | 36.1 | 4.32 | 0.655±0.020 |
| 15 | 28.59 | 28.4 | 5.65 | 0.502±0.012 |
| 16 | 32.11 | 34.5 | 4.57 | 0.685±0.003 |
| 17 | 31.47 | 34.0 | 3.77 | 0.752±0.024 |
| 18 | 30.45 | 34.3 | 4.49 | 0.633±0.006 |
| 19 | 25.98 | 30.2 | 4.24 | 0.822±0.013 |
| 20 | 30.20 | 28.5 | 4.22 | 0.575±0.006 |
| 21 | 28.36 | 30.2 | 5.06 | 0.468±0.025 |
| 22 | 33 | 39.2 | 3.8 | 0.683±0.068 |
| 23 | 30.35 | 29.5 | 3.89 | 0.675±0.005 |
| 24 | 30.73 | 31 | 3.85 | 0.703±0.015 |
| 25 | 24.72 | 27.8 | 4.48 | 1.837±0.091 |
| 26 | 32.6 | 35.45 | 4.12 | 0.713±0.013 |
| 27 | 32.13 | 31.9 | 4.06 | 0.660±0.010 |
| 28 | 27.44 | 30.02 | 5.18 | 0.783±0.045 |
| 29 | 27.83 | 27 | 5.37 | 0.738±0.013 |
| 30 | 30.61 | 29.4 | 3.54 | 0.578±0.018 |
| 31 | 27.38 | 26 | 4.08 | 1.078±0.033 |
| 32 | 27.98 | 28.3 | 4.29 | 0.663±0.003 |
| 33 | 30.56 | 28.8 | 4.67 | 0.502±0.019 |
| 34 | 29.86 | 28.6 | 3.83 | 0.860±0.030 |
| 35 | 27.95 | 26.6 | 4.81 | 0.370±0.008 |
| 36 | 29.49 | 26 | 3.66 | 0.723±0.038 |
| 37 | 26.81 | 27.3 | 4.25 | 0.498±0.027 |
| 38 | 28.59 | 28.9 | 4.72 | 1.405±0.037 |
| 39 | 27.11 | 28.9 | 4.7 | 1.090±0.015 |
| 40 | 30.91 | 32.1 | 3.77 | 1.103±0.019 |
Content of lignin and three index of quality of cotton fiber are carried out correlation analysis, its coefficient of multiple correlation R=0.52394**, simple correlation coefficient sees Table 2, and partial correlation coefficient sees Table 3.
Simple correlation coefficient between table 2 content of lignin and the index of quality
| Lignin | Length | Intensity | Mic value | |
| Lignin | 1 | |||
| Length | -0.44616** | 1 | ||
| Intensity | -0.30534 | 0.64909** | 1 | |
| Mic value | -0.04097 | -0.45605** | -0.25330 | 1 |
Annotate: * * is illustrated in the utmost point significant correlation of P＜0.01 level, down together.
Partial correlation coefficient between table 3 content of lignin and the index of quality
| Lignin | |
| Lignin | 1 |
| Length | -0.43186** |
| Intensity | -0.00396 |
| Mic value | -0.30614 |
Analyze by statistics, the simple correlation of content of lignin and cotton fiber length and partial correlation coefficient all reach the utmost point level of signifiance (P＜0.01).
With the content of lignin is dependent variable Y, and length, specific strength, mic value are respectively independent variable X
1, X
2, X
3, obtain following multiple regression equation through regretional analysis:
Y＝-0.07998X
1-0.00041X
2-0.20084X
3+4.033655
This multiple regression equation is checked by statistics and is reached the utmost point level of signifiance (P＜0.01).
Claims (2)
1. method of establishing content of lignin and fiber quality correlationship in the cotton fiber, this method comprises the steps:
A, sample collecting and preparation: gather ripe cotton fiber sample 30-50 part, carry out cotton fiber quality and detect, record fibre length, specific strength, the mic value of each sample;
B, sample pre-treatments: remove non-cotton fiber impurity, take by weighing cotton sample 5-10g, with twice of homogenization buffer solution for cleaning, clean twice with 80% acetone again, pure acetone cleans once, clean all vortex, extruding and cotton fiber is placed in the metal clip garlic device extrudes residual liquid repeatedly at every turn, clean the 45 ℃ of dry for standby of cotton sample after finishing;
C, filter paper are handled: fine and close quantitative filter paper is soaked the back fully with dilute sulfuric acid be washed till neutrality with distilled water, dry to constant weight in 60 ℃ of baking ovens;
D, content of lignin are measured: take by weighing the 2-3g sample and place in the 50ml tool plug glass bottle, add the 10-20ml concentrated sulphuric acid of precooling in 4 ℃ of refrigerators in advance, fully behind the mixing, place 1-3h under the room temperature, change in the 1L autoclaving bottle, sulfuric acid concentration when adding distil water is diluted to the filter paper processing, bottleneck sealing back high-pressure sterilizing pot pyroprocessing 1h naturally cools to room temperature; Fine and close quantitative filter paper with the oven dry constant weight filters, be washed with distilled water to filter paper neutrality, filter paper is placed in 60 ℃ of baking ovens together with residue dries to constant weight, 575 ℃ of following ashing in the muffle furnace, claim ash content weight, the difference of the weight of filter paper deducts the weight that ash content weight is lignin, and each cotton sample repeats 2-3 time and gets its mean value;
E, correlation analysis: with content of lignin in the cotton fiber is dependent variable y, and fibre length, specific strength, mic value are respectively independent variable X
1, X
2, X
3, statistical study obtains content of lignin and fiber quality correlationship regression equation.
2. the method for claim 1 is characterized in that described cotton fiber sample is 40 parts, and the sample of sample pre-treatments is 10g, and 50mMTris-HCl that described homogenization damping fluid is pH8.3 and 1% song draw the mixed liquor of logical x-100 and 1M NaCl; The heavy 2g of sample when content of lignin is measured, 72% sulfuric acid of adding 15ml precooling is placed 2h under the room temperature, and distilled water diluting is to 560ml, and multiplicity is 3; The regression equation that statistical study obtains is
Y＝-0.07998X
1-0.00041X
2-0.20084X
3+4.033655
This multiple regression equation is checked by statistics and is reached the utmost point level of signifiance, i.e. P＜0.01.
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| CN103335974B (en) * | 2013-06-08 | 2015-06-03 | 广东中烟工业有限责任公司 | Measuring method of content of lignin in tobacco |
| CN104777275B (en) * | 2015-04-27 | 2017-02-01 | 南京农业大学 | Method for analyzing seed indexes of key cotton seed forming periods |
| CN109115644B (en) * | 2018-08-29 | 2020-12-22 | 重庆三磊玻纤股份有限公司 | Method for detecting acetone dissolution rate of glass fiber |
| CN114560290B (en) * | 2022-03-11 | 2024-11-15 | 山东亚历山大智能科技有限公司 | A fiber quality detection system and method based on crucible stand collaborative control |
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| CN101105444B (en) * | 2007-04-10 | 2010-05-26 | 新疆农业科学院核技术生物技术研究所 | Detection and analysis method for cotton fiber lignin content |
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