CN110220873A - A kind of preparation method of FITC label chitosan fluorescent slurry - Google Patents
A kind of preparation method of FITC label chitosan fluorescent slurry Download PDFInfo
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- CN110220873A CN110220873A CN201910227488.4A CN201910227488A CN110220873A CN 110220873 A CN110220873 A CN 110220873A CN 201910227488 A CN201910227488 A CN 201910227488A CN 110220873 A CN110220873 A CN 110220873A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0006—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid
- C08B37/0024—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid beta-D-Glucans; (beta-1,3)-D-Glucans, e.g. paramylon, coriolan, sclerotan, pachyman, callose, scleroglucan, schizophyllan, laminaran, lentinan or curdlan; (beta-1,6)-D-Glucans, e.g. pustulan; (beta-1,4)-D-Glucans; (beta-1,3)(beta-1,4)-D-Glucans, e.g. lichenan; Derivatives thereof
- C08B37/0027—2-Acetamido-2-deoxy-beta-glucans; Derivatives thereof
- C08B37/003—Chitin, i.e. 2-acetamido-2-deoxy-(beta-1,4)-D-glucan or N-acetyl-beta-1,4-D-glucosamine; Chitosan, i.e. deacetylated product of chitin or (beta-1,4)-D-glucosamine; Derivatives thereof
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
- G01N21/6428—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
- G01N21/643—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes" non-biological material
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Abstract
The invention discloses a kind of preparation methods of FITC label chitosan fluorescent slurry.Preparation step includes: to disperse Chitosan powder in acetic acid diluted aqueous solution, until completely dissolved, isometric methanol is added, add FITC methanol solution, it is sufficiently stirred at the place of being protected from light, pH to 7~8 is adjusted, FITC label chitosan product is precipitated, is washed repeatedly with methanol/water mixed solvent and is centrifuged removal impurity；Obtained FITC label chitosan acetic acid diluted aqueous dissolution, then dialyse in distilled water, FITC label chitosan slurry can be obtained after vacuum freeze drying.Preparation process of the present invention is simple, obtained FITC label chitosan slurry has good fluorescent effect, the general detection regulation of comparison, utilize the yarn after the slurry sizing, only need using fluorescence microscope substitution ordinary optical microscope can Accurate Determining chitosan slurries be impregnated with rate, covering rate and integrated rate of starch film, solve the problems, such as the measurement difficulty of spinning sizing agent field chitosan slurries impregnability and coating property.
Description
Technical field
The invention belongs to sizing fabric performance detection modification of chitosan Size Technology fields, and in particular to a kind of FITC mark
Remember the preparation method of chitosan fluorescent slurry.
Background technique
Warp yarn sizing is a vital process in weaving production, and China textile worker is often referred to as " tiger
Mouthful ", external weaving academia was also once commented on: " sizing one minute, one class of cloth machine ".Starching is the necessary process of Weaving prepartion
One of, purpose resists the ability that external complex Mechanics of Machinery acts on (such as stretching rubs) precisely in order to assigning warp thread, improves and passes through
The weavability of yarn ensures that manufacturing process is gone on smoothly, and almost all of spun yarn and long filament all need to process by starching.On warp thread
When slurry, the slurries being adsorbed on yarn can be divided into two parts, and the surface that a part is coated in yarn forms serous coat, another part
Then it is impregnated into the inside of yarn.Sizing technique requires slurries that can be adsorbed in around yarn body, has both and is impregnated with and is coated, this is to promote slurry
Yarn quality, save usage of sizing agent important guarantee, if slurries be impregnated with and be coated ratio control it is improper, will to rear road weave produce
Raw serious influence.
The cross section of sizing slice is made of 3 parts from outside to inside: serous coat, sizing have been impregnated with part and are not impregnated with part
(see sizing serial section schematic diagram, i.e. Fig. 1).Currently, being usually to the impregnability of slurries and the test of coating property in textile industry
Color developing agent coloring is immersed by making sizing slice (thickness≤20 μm) in advance, then by slice, is observed with ordinary optical microscope
Then the surface topography being sliced after coloring is weighed with microscope projector, area integral instrument or paper-cut (to draw the weight of paper
Substitution area) calculate slurries be impregnated with three rate, covering rate and integrated rate of starch film indexs, calculation method is respectively by formula
(1), shown in (2), (3) and schematic diagram:
A=(S-S2)/S × 100%=(G-G2)/G × 100% (1)
In formula (1), A: it is impregnated with rate, S: the sectional area of raw yarn, S2: sizing is not saturated the sectional area of part, G: drawing former
The paper weight in yarn section, G2: draw the paper weight that sizing is not saturated partial cross section.
B=(S1- S)/S × 100%=(G1- G)/G × 100% (2)
In formula (2), B: covering rate, S: the sectional area of raw yarn, S1: G: the sectional area of sizing draws the paper in raw yarn section
Weight, G1: draw the paper weight in sizing section.
F=Σ αi/ 360 ° × 100% (3)
In formula (3), F: integrated rate of starch film, αi: the angle of the surrounded raw yarn of serous coat everywhere.
Be sliced at present to sizing there are two types of the color developing agent coloured main: iodine-potassium iodide and iodo- acid reagent are used respectively
In two kinds of main spinning sizing agents --- the coloring of starch and PVA sizing.The chitosan biological based textile size important as one kind,
Existing sizing quality assessment method does not provide corresponding color developing agent but, thus leads to not measure being impregnated with for chitosan slurries
Property and coating property.FITC (fluorescein isothiocynate) is a kind of common fluorescent labeling reagent, and quantum yield is high, is had preferable
Photostability and low-temperature coefficient are widely used in protein detection, immunofluorescence technique and DNA sequence analysis etc..However, mesh
It is preceding there is not yet FITC mark fluorescent chitosan product applied in sizing quality detection field research report.Therefore, for
Chitosan-based product develops the detection with good fluorescence characteristic of FITC label a kind of with modification of chitosan slurry to chitosan
The solution that slurries impregnability, coating property measure difficult problem has great importance.
Summary of the invention
The object of the present invention is to provide a kind of preparation methods of FITC label chitosan fluorescent slurry, poly- for shell to obtain
The modification of chitosan material with good fluorescence effect of glycosyl slurry slurries impregnability and the measurement of coating property.
The preparation method of FITC label chitosan fluorescent slurry of the invention, steps are as follows:
1) it disperses Chitosan powder in 0.10mol/L acetic acid aqueous solution, is configured to the shell of 1.0~3.0% (wt%)
Glycan solution, adds isometric methanol, is thoroughly mixed at room temperature uniformly；
2) the FITC methanol that the 2.0mg/mL of 0.050~0.20mL is added in the chitosan solution that step 1) obtains is molten
PH value of reaction system is adjusted to 7~8 with the NaOH solution of 0.20mol/L, made by liquid at room temperature after 2~4h is reacted at the place of being protected from light
FITC marks chitosan product to be precipitated；
3) the precipitation product of step 2) is placed in 10000rpm in centrifuge tube and is centrifuged 15min, be repeatedly 7:3's with volume ratio
The washing of methanol/water mixed solvent, centrifugation repeatedly, then with 0.1mol/L acetic acid aqueous solution dissolve FITC label chitosan product；
4) the FITC label chitosan solution that step 3) obtains is placed in bag filter, is dialysed using distilled water in the place of being protected from light
FITC label chitosan fluorescent slurry will can be obtained in 72h after product freeze-drying after dialysis.
The beneficial effects of the present invention are:
The present invention prepares chitosan solution using diluted acid solvent, by the way that different material is added under conditions of being sufficiently stirred
The fluorescent molecule FITC of amount adjusts the degree of substitution of chitosan, makes FITC label shell poly- after NaOH solution is added in the reaction system
Sugar is precipitated, then washed, centrifugation, dialysis removal impurity and residual solvent, and FITC mark is made by way of vacuum freeze drying
Remember chitosan fluorescent slurry.The degree of substitution of chitosan can be regulated and controled by adjusting the amount of addition FITC, FITC is marked to realize
The controllable adjustment for remembering chitosan slurry fluorescence intensity is allowed to be adapted to the impregnability of chitosan slurries and the measurement of coating property.
Detailed description of the invention
Fig. 1 is sizing serial section schematic diagram；
Fig. 2 is FITC mark fluorescent chitosan slurry sizing slice under photo (a) the blue light excitation under fluorescence microscope
(b) under light field (it is impregnated with rate: 35.52%, covering rate: 36.02%, integrated rate of starch film: 74.44%).
Specific embodiment
The present invention is further illustrated below in conjunction with example.The deacetylation of the chitosan used in following examples for 60%~
100%, molecular weight is 50000~800000.
Embodiment 1:
1) it disperses Chitosan powder in 0.10mol/L acetic acid aqueous solution, the chitosan for being configured to 1.0% (wt%) is molten
Liquid, adds the methanol isometric with acetic acid aqueous solution, is thoroughly mixed at room temperature uniformly；
2) the FITC methanol solution of the 2.0mg/mL of 0.050mL, room temperature are added in the chitosan solution that step 1) obtains
Under in the place of being protected from light react 2h after, pH value of reaction system is adjusted to 7~8 with the NaOH solution of 0.20mol/L, make FITC mark shell
Glycan product is precipitated；
3) the precipitation product of step 2) is placed in 10000rpm in centrifuge tube and is centrifuged 15min, be repeatedly 7:3's with volume ratio
The washing of methanol/water mixed solvent, centrifugation 5 times, then dissolved FITC label chitosan product with 0.10mol/L acetic acid aqueous solution；
4) the FITC label chitosan solution that step 3) obtains is placed in bag filter, is dialysed using distilled water in the place of being protected from light
FITC label chitosan fluorescent slurry will can be obtained in 72h after product freeze-drying after dialysis.
Embodiment 2:
1) it disperses Chitosan powder in 0.10mol/L acetic acid aqueous solution, the chitosan for being configured to 3.0% (wt%) is molten
Liquid, adds isometric methanol, is thoroughly mixed at room temperature uniformly；
2) the FITC methanol solution of the 2.0mg/mL of 0.20mL is added in the chitosan solution that step 1) obtains, at room temperature
After 4h is reacted at the place of being protected from light, pH value of reaction system is adjusted to 7~8 with the NaOH solution of 0.20mol/L, keeps FITC label shell poly-
Sugared product is precipitated；
3) the precipitation product of step 2) is placed in 10000rpm in centrifuge tube and is centrifuged 15min, be repeatedly 7:3's with volume ratio
The washing of methanol/water mixed solvent, centrifugation 5 times, then dissolved FITC label chitosan product with 0.10mol/L acetic acid aqueous solution；
4) the FITC label chitosan solution that step 3) obtains is placed in bag filter, is dialysed using distilled water in the place of being protected from light
FITC label chitosan fluorescent slurry will can be obtained in 72h after product freeze-drying after dialysis.
Embodiment 3:
1) it disperses Chitosan powder in 0.10mol/L acetic acid aqueous solution, the chitosan for being configured to 1.0% (wt%) is molten
Liquid, adds isometric methanol, is thoroughly mixed at room temperature uniformly；
2) the FITC methanol solution of the 2.0mg/mL of 0.10mL is added in the chitosan solution that step 1) obtains, at room temperature
After 3h is reacted at the place of being protected from light, pH value of reaction system is adjusted to 7~8 with the NaOH solution of 0.20mol/L, keeps FITC label shell poly-
Sugared product is precipitated；
3) the precipitation product of step 2) is placed in 10000rpm in centrifuge tube and is centrifuged 15min, be repeatedly 7:3's with volume ratio
The washing of methanol/water mixed solvent, centrifugation 5 times, then dissolved FITC label chitosan product with 0.10mol/L acetic acid aqueous solution；
4) the FITC label chitosan solution that step 3) obtains is placed in bag filter, is dialysed using distilled water in the place of being protected from light
FITC label chitosan fluorescent slurry will can be obtained in 72h after product freeze-drying after dialysis.
Embodiment 4:
1) it disperses Chitosan powder in 0.10mol/L acetic acid aqueous solution, the chitosan for being configured to 1.0% (wt%) is molten
Liquid, adds isometric methanol, is thoroughly mixed at room temperature uniformly；
2) the FITC methanol solution of the 2.0mg/mL of 0.15mL is added in the chitosan solution that step 1) obtains, at room temperature
After 3.5h is reacted at the place of being protected from light, pH value of reaction system is adjusted to 7~8 with the NaOH solution of 0.20mol/L, FITC is made to mark shell
Glycan product is precipitated；
3) the precipitation product of step 2) is placed in 10000rpm in centrifuge tube and is centrifuged 15min, be repeatedly 7:3's with volume ratio
The washing of methanol/water mixed solvent, centrifugation 5 times, then dissolved FITC label chitosan product with 0.10mol/L acetic acid aqueous solution；
4) the FITC label chitosan solution that step 3) obtains is placed in bag filter, is dialysed using distilled water in the place of being protected from light
FITC label chitosan fluorescent slurry will can be obtained in 72h after product freeze-drying after dialysis.
FITC marks the mark rate of chitosan fluorescent slurry under 1 difference FITC feed concentrations of table
Remarks: mark rate refers to the mass ratio of the FITC and glycan substrate that are grafted on chitosan fluorescent slurry strand.
Claims (2)
1. a kind of preparation method of FITC label chitosan fluorescent slurry, comprising the following steps:
1) it disperses Chitosan powder in 0.10mol/L acetic acid aqueous solution, is configured to the chitosan of 1.0~3.0% (wt%)
Solution, adds isometric methanol, is thoroughly mixed at room temperature uniformly；
2) the FITC methanol solution of the 2.0mg/mL of 0.050~0.20mL, room are added in the chitosan solution that step 1) obtains
Under temperature after 2~4h is reacted at the place of being protected from light, pH value of reaction system is adjusted to 7~8 with the NaOH solution of 0.20mol/L, makes FITC
Chitosan product is marked to be precipitated；
3) the precipitation product of step 2) is placed in 10000rpm in centrifuge tube and is centrifuged 15min, the first for being repeatedly 7:3 with volume ratio
Alcohol/water mixed solvent washing, centrifugation repeatedly, then with 0.10mol/L acetic acid aqueous solution dissolve FITC label chitosan product；
4) FITC that step 3) obtains label chitosan solution is placed in bag filter, using distilled water in the place of being protected from light dialysis 72h,
FITC label chitosan fluorescent slurry will can be obtained after product freeze-drying after dialysis.
2. a kind of preparation method of FITC label chitosan fluorescent slurry according to claim 1, it is characterised in that: described
Chitosan deacetylation be 60%~100%, molecular weight be 50000~800000.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910227488.4A CN110220873B (en) | 2019-03-25 | 2019-03-25 | Preparation method of FITC (fluorescein isothiocyanate) labeled chitosan fluorescent slurry |
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| CN201910227488.4A CN110220873B (en) | 2019-03-25 | 2019-03-25 | Preparation method of FITC (fluorescein isothiocyanate) labeled chitosan fluorescent slurry |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113235188A (en) * | 2021-05-10 | 2021-08-10 | 中国科学技术大学 | Fluorescent chitosan fiber for detecting miRNA-198 and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113235188A (en) * | 2021-05-10 | 2021-08-10 | 中国科学技术大学 | Fluorescent chitosan fiber for detecting miRNA-198 and preparation method thereof |
| CN113235188B (en) * | 2021-05-10 | 2022-09-06 | 中国科学技术大学 | Fluorescent chitosan fiber for detecting miRNA-198 and preparation method thereof |
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