CN111077123A - Method for rapidly determining average polymerization degree of cellulose based on fluorescence technology - Google Patents
Method for rapidly determining average polymerization degree of cellulose based on fluorescence technology Download PDFInfo
- Publication number
- CN111077123A CN111077123A CN201911317990.0A CN201911317990A CN111077123A CN 111077123 A CN111077123 A CN 111077123A CN 201911317990 A CN201911317990 A CN 201911317990A CN 111077123 A CN111077123 A CN 111077123A
- Authority
- CN
- China
- Prior art keywords
- cellulose
- fluorescence
- polymerization
- degree
- average
- 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.)
- Pending
Links
Images
Classifications
-
- 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
Landscapes
- Health & Medical Sciences (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Physics & Mathematics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
Abstract
The invention discloses a method for rapidly determining the average polymerization degree of cellulose based on a fluorescence technology, which comprises the steps of detecting the fluorescence intensity of standard glucan samples with different polymerization degrees, establishing a standard curve of the polymerization degree and the fluorescence intensity, detecting the fluorescence intensity of a cellulose sample to be detected, and obtaining the average polymerization degree of the cellulose sample to be detected according to the standard curve and the fluorescence intensity of the cellulose sample to be detected; in the fluorescence detection process, the excitation wavelength is 521-523 nm, and the fluorescence intensity at the position of the emission wavelength of 570-575 nm is detected. The method does not need to prepare other solutions, and can realize the rapid determination of the average polymerization degree of the cellulose.
Description
Technical Field
The invention belongs to the technical field of cellulose material detection, and relates to a method for rapidly determining the average polymerization degree of cellulose based on a fluorescence technology.
Background
The information in this background section is only for enhancement of understanding of the general background of the invention and is not necessarily to be construed as an admission or any form of suggestion that this information forms the prior art that is already known to a person of ordinary skill in the art.
Cellulose is a macromolecular polysaccharide composed of glucose which is widely distributed and contained in the nature, and is insoluble in water and common organic solvents. The glucose-based ring number of the cellulose macromolecules is targeted to be polymerization degree, and the size of the glucose-based ring number is used for representing the length of a cellulose molecular chain. Generally, the degree of polymerization of cellulose has heterogeneity, i.e., polydispersity, and is therefore usually expressed in terms of average degree of polymerization. The degree of polymerization of the cellulose can objectively and quantitatively reflect the damage degree to the fiber in the actual processing processes of spinning, weaving, dyeing and the like, and is an important index for measuring the quality of the fiber.
Currently, there are many methods for measuring the degree of polymerization of cellulose, such as a viscosity method, an osmotic pressure method, a terminal chemical titration method, a light scattering method, a boiling point increasing method, an ultracentrifugal sedimentation method, a diffusion method, and the like, and among them, the viscosity method is the most widely used method. When the degree of polymerization of cellulose is measured by adopting a viscosity method, the cellulose is dissolved in a solvent to prepare a cellulose solution with a certain concentration, and the solvent for dissolving the cellulose is a cuprammonium solution or a cuprammonium solution. However, the cuprammonium solution and the cuprammonium solution are unstable, difficult to store, complex in preparation process and long in cycle, so that the detection cycle of the polymerization degree of cellulose is long; meanwhile, both the cuprammonium solution and the cuprammonium solution are easy to cause serious oxidative degradation of cellulose, thereby damaging the cellulose.
Disclosure of Invention
In order to solve the defects of the prior art, the invention aims to provide a method for rapidly determining the average polymerization degree of cellulose based on a fluorescence technology, which can realize rapid determination of the average polymerization degree of cellulose without preparing other solutions.
In order to achieve the purpose, the technical scheme of the invention is as follows:
in one aspect, a fluorescence detection method is used for determining the average degree of polymerization of cellulose.
The inventor of the invention finds out that the average polymerization degree of the cellulose can be detected by adopting a fluorescence detection method for the first time.
On the other hand, the method for rapidly determining the average polymerization degree of the cellulose based on the fluorescence technology detects the fluorescence intensity of standard glucan samples with different polymerization degrees, establishes a standard curve of the polymerization degree and the fluorescence intensity, detects the fluorescence intensity of the cellulose sample to be determined, and obtains the average polymerization degree of the cellulose sample to be determined according to the standard curve and the fluorescence intensity of the cellulose sample to be determined; in the fluorescence detection process, the excitation wavelength is 521-523 nm, and the fluorescence intensity at the position of the emission wavelength of 570-575 nm is detected.
Experiments show that the average polymerization degree of the cellulose can be detected by adopting a fluorescence method, and the average polymerization degree of the cellulose is detected by adopting the fluorescence method without preparing other solutions, so that the average polymerization degree of the cellulose can be rapidly measured, and the cellulose can be prevented from being damaged by other solutions.
The invention has the beneficial effects that:
the method can be used for rapidly and accurately measuring the average polymerization degrees of different types of cellulose, and has the advantages of no damage to samples, less time consumption, simple operation and the like compared with the conventional research method.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, are included to provide a further understanding of the invention, and are incorporated in and constitute a part of this specification, illustrate exemplary embodiments of the invention and together with the description serve to explain the invention and not to limit the invention.
FIG. 1 is a fluorescence spectrum of a cellulose sample to be tested in example 1 of the present invention.
Detailed Description
It is to be understood that the following detailed description is exemplary and is intended to provide further explanation of the invention as claimed. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of exemplary embodiments according to the invention. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, and it should be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof, unless the context clearly indicates otherwise.
In view of the defects that a cuprammonium solution and a cuprammonium solution are unstable, are not easy to store, have complex and long preparation process and cause severe oxidative degradation of cellulose in the conventional viscosity method for detecting the polymerization degree of cellulose, the invention provides a method for rapidly determining the average polymerization degree of cellulose based on a fluorescence technology.
In one exemplary embodiment of the present invention, a fluorescence detection method is provided for use in determining the average degree of polymerization of cellulose.
The inventor of the invention finds out that the average polymerization degree of the cellulose can be detected by adopting a fluorescence detection method for the first time.
The invention also provides a method for rapidly determining the average polymerization degree of cellulose based on a fluorescence technology, which comprises the steps of detecting the fluorescence intensity of standard glucan samples with different polymerization degrees, establishing a standard curve of the polymerization degree and the fluorescence intensity, detecting the fluorescence intensity of the cellulose sample to be detected, and obtaining the average polymerization degree of the cellulose sample to be detected according to the standard curve and the fluorescence intensity of the cellulose sample to be detected; in the fluorescence detection process, the excitation wavelength is 521-523 nm, and the fluorescence intensity at the position of the emission wavelength of 570-575 nm is detected.
Experiments show that the average polymerization degree of the cellulose can be detected by adopting a fluorescence method, and the average polymerization degree of the cellulose is detected by adopting the fluorescence method without preparing other solutions, so that the average polymerization degree of the cellulose can be rapidly measured, and the cellulose can be prevented from being damaged by other solutions.
In one or more embodiments of this embodiment, standard dextran samples of different degrees of polymerization are configured to the same concentration and then the fluorescence intensity is measured.
In this series of examples, the concentration is 0.1 wt% to 1 wt%.
In one or more embodiments of this embodiment, the cellulose is commercial pulp fiber, modified cellulose, or pure cellulose.
In this series of examples, the commercial pulp fibers were bleached softwood chemical pulp, dissolving pulp, or chemi-mechanical pulp.
In this series of examples, the modified cellulose was TEMPO oxidation treated cellulose.
In this series of examples, the pure cellulose is bacterial cellulose free of lignin and impurities.
In one or more embodiments of this embodiment, the excitation wavelength is 522 nm.
In one or more embodiments of this embodiment, the cuvette used in the fluorescence detection is a quartz cuvette that is transparent on all sides.
In one or more embodiments of this embodiment, the fluorescence detector is a HORIBASIC FluoroMax-4 fluorescence spectrometer.
In order to make the technical solutions of the present invention more clearly understood by those skilled in the art, the technical solutions of the present invention will be described in detail below with reference to specific embodiments.
Example 1
Adjusting standard glucan samples (D140060, D140063 and D140057) with different polymerization degrees to the concentration of 0.1 wt%, respectively placing 2mL of the standard glucan samples with different polymerization degrees and different polymerization degrees in different quartz cuvettes with light transmission on four sides, placing the quartz cuvettes with the samples into a HORIBA Scientific fluorescence Max-4 fluorescence spectrometer, setting the excitation wavelength to be 522nm and the emission wavelength range to be 550-600 nm, and performing fluorescence detection. Fluorescence intensities of emission peaks at 574nm were obtained for standard dextran samples of different degrees of polymerization, and a standard curve of the degree of polymerization versus fluorescence intensity of emission peak at 574nm was obtained (y ═ 525.6ln (x) +3674.5, R ═ 525.6 ln: (x)) +3674.52＝0.9865)。
Taking a cellulose sample of the bleached chemical pulp to be detected, and detecting by adopting a viscosity method, wherein the polymerization degree of the cellulose sample is 875. Preparing a suspension with the concentration of 0.1 wt% from the cellulose sample, placing 2mL of the suspension in different quartz cuvettes with light transmission on four sides, placing the quartz cuvettes with the suspension in a HORIBA Scientific FluoroMax-4 fluorescence spectrometer, setting the excitation wavelength to be 522nm and the emission wavelength to be 550-600 nm, and performing fluorescence detection, as shown in FIG. 1. And obtaining the fluorescence intensity of the emission peak of the cellulose sample to be detected at 574nm, carrying out three times of detection, carrying out average calculation on the fluorescence intensity of the three times of detection to obtain the average fluorescence intensity, and carrying out fitting calculation according to the average fluorescence intensity and the standard curve to obtain the polymerization degree of the cellulose sample to be detected, wherein the polymerization degree of the cellulose sample to be detected is 871.
Example 2
Adjusting standard glucan samples (D140060, D140063 and D140057) with different polymerization degrees to the concentration of 0.5 wt%, respectively placing 2mL of the standard glucan samples with different polymerization degrees and different polymerization degrees in different quartz cuvettes with light transmission on four sides, placing the quartz cuvettes with the samples into a HORIBA Scientific fluorescence Max-4 fluorescence spectrometer, setting the excitation wavelength to be 522nm and the emission wavelength range to be 550-600 nm, and performing fluorescence detection. Fluorescence intensities of emission peaks at 574nm were obtained for standard dextran samples of different degrees of polymerization, and a standard curve of the degree of polymerization versus fluorescence intensity of emission peak at 574nm was obtained (y ═ 543.2ln (x) +4237.5, R ═2＝0.9673)。
Taking a TEMPO oxidized cellulose sample to be detected, and detecting by adopting a viscosity method, wherein the polymerization degree of the cellulose sample is 325. Preparing the cellulose sample into a suspension with the concentration of 0.5 wt%, placing 2mL of the suspension into different quartz cuvettes with light transmission on four sides, placing the quartz cuvettes with the suspension into a HORIBA Scientific FluoroMax-4 fluorescence spectrometer, setting the excitation wavelength to be 522nm and the emission wavelength to be 550-600 nm, and carrying out fluorescence detection. And obtaining the fluorescence intensity of the emission peak of the cellulose sample to be detected at 574nm, carrying out three times of detection, carrying out average calculation on the fluorescence intensity of the three times of detection to obtain the average fluorescence intensity, and carrying out fitting calculation according to the average fluorescence intensity and the standard curve to obtain the polymerization degree of the cellulose sample to be detected as 319.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. An application of a fluorescence detection method in determining the average polymerization degree of cellulose.
2. A method for rapidly determining the average polymerization degree of cellulose based on a fluorescence technology is characterized by detecting the fluorescence intensity of standard glucan samples with different polymerization degrees, establishing a standard curve of the polymerization degree and the fluorescence intensity, detecting the fluorescence intensity of a cellulose sample to be detected, and obtaining the average polymerization degree of the cellulose sample to be detected according to the standard curve and the fluorescence intensity of the cellulose sample to be detected; in the fluorescence detection process, the excitation wavelength is 521-523 nm, and the fluorescence intensity at the position of the emission wavelength of 570-575 nm is detected.
3. The method for rapid determination of average degree of polymerization of cellulose based on fluorescence technique according to claim 2, wherein the standard glucan samples of different degree of polymerization are prepared to the same concentration, and then the fluorescence intensity is measured.
4. The method for rapidly measuring the average degree of polymerization of cellulose based on fluorescence technique according to claim 3, wherein the concentration is 0.1 to 1% by weight.
5. The method for rapidly measuring the average degree of polymerization of cellulose based on the fluorescence technique according to claim 2, wherein the cellulose is commercial pulp fiber, modified cellulose or pure cellulose.
6. The method for rapid determination of average degree of polymerization of cellulose based on fluorescence technology as claimed in claim 5, wherein the commercial pulp fiber is bleached softwood chemical pulp, dissolving pulp or chemi-mechanical pulp.
7. The method for rapid determination of average degree of polymerization of cellulose based on fluorescence technique as claimed in claim 5, wherein the modified cellulose is TEMPO oxidation treated cellulose.
8. The method for rapid determination of average degree of polymerization of cellulose based on fluorescence technique as claimed in claim 5, wherein said pure cellulose is bacterial cellulose without lignin and impurities.
9. The method for rapid determination of average degree of polymerization of cellulose based on fluorescence technique as claimed in claim 2, wherein the excitation wavelength is 522 nm.
10. The method for rapid determination of average degree of polymerization of cellulose based on fluorescence technique as claimed in claim 2, wherein the cuvette used in the fluorescence detection is a quartz cuvette with four sides transparent to light.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911317990.0A CN111077123A (en) | 2019-12-19 | 2019-12-19 | Method for rapidly determining average polymerization degree of cellulose based on fluorescence technology |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911317990.0A CN111077123A (en) | 2019-12-19 | 2019-12-19 | Method for rapidly determining average polymerization degree of cellulose based on fluorescence technology |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN111077123A true CN111077123A (en) | 2020-04-28 |
Family
ID=70315726
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201911317990.0A Pending CN111077123A (en) | 2019-12-19 | 2019-12-19 | Method for rapidly determining average polymerization degree of cellulose based on fluorescence technology |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111077123A (en) |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2012073089A (en) * | 2010-09-28 | 2012-04-12 | Gunze Ltd | Method for measuring degree of polymerization of cellulose |
| US20130171651A1 (en) * | 2010-11-22 | 2013-07-04 | Henkel Corporation | Methods for measuring degree of cure or soldification of a composition |
| CN104132868A (en) * | 2014-07-16 | 2014-11-05 | 河南科技大学 | Cellulose polymerization degree determination method |
| US20170370920A1 (en) * | 2015-03-13 | 2017-12-28 | Sysmex Corporation | Method for detecting analyte |
| CN109187276A (en) * | 2018-09-25 | 2019-01-11 | 中国科学院过程工程研究所 | A kind of cellulose relative polymerization degree measuring method based on ion liquid solvent |
| US20190265246A1 (en) * | 2018-02-28 | 2019-08-29 | Shimadzu Corporation | Glycan analysis method, glycan analysis system, program for glycan analysis, and kit for glycan analysis |
-
2019
- 2019-12-19 CN CN201911317990.0A patent/CN111077123A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2012073089A (en) * | 2010-09-28 | 2012-04-12 | Gunze Ltd | Method for measuring degree of polymerization of cellulose |
| US20130171651A1 (en) * | 2010-11-22 | 2013-07-04 | Henkel Corporation | Methods for measuring degree of cure or soldification of a composition |
| CN104132868A (en) * | 2014-07-16 | 2014-11-05 | 河南科技大学 | Cellulose polymerization degree determination method |
| US20170370920A1 (en) * | 2015-03-13 | 2017-12-28 | Sysmex Corporation | Method for detecting analyte |
| US20190265246A1 (en) * | 2018-02-28 | 2019-08-29 | Shimadzu Corporation | Glycan analysis method, glycan analysis system, program for glycan analysis, and kit for glycan analysis |
| CN109187276A (en) * | 2018-09-25 | 2019-01-11 | 中国科学院过程工程研究所 | A kind of cellulose relative polymerization degree measuring method based on ion liquid solvent |
Non-Patent Citations (1)
| Title |
|---|
| GARIFULLIN, M. SH.: "MONITOR THE STATUS OF INSULATING PAPER IN OIL-FILLED ELECTRICAL EQUIPMENT BY OPTICAL METHODS", 《KONTROL DIAGNOSTIKA》 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Donaldson et al. | Quantification of compression wood severity in tracheids of Pinus radiata D. Don using confocal fluorescence imaging and spectral deconvolution | |
| Fras et al. | Analysis of the oxidation of cellulose fibres by titration and XPS | |
| Hubbe et al. | Analytical Staining of Cellulosic Materials: A Review. | |
| Siller et al. | Dissolution of rayon fibers for size exclusion chromatography: a challenge | |
| Vidal et al. | Polarization microscopy and microspectrophotometry of Sirius Red, Picrosirius and Chlorantine Fast Red aggregates and of their complexes with collagen | |
| White et al. | In situ surface enhanced resonance Raman scattering analysis of a reactive dye covalently bound to cotton | |
| Abu‐Rous et al. | A new method to visualize and characterize the pore structure of TENCEL®(Lyocell) and other man‐made cellulosic fibres using a fluorescent dye molecular probe | |
| Mazzuca et al. | Evaluating the influence of paper characteristics on the efficacy of new poly (vinyl alcohol) based hydrogels for cleaning modern and ancient paper | |
| Peretz et al. | Rapid quantification of cellulose nanocrystals by Calcofluor White fluorescence staining | |
| CN111077123A (en) | Method for rapidly determining average polymerization degree of cellulose based on fluorescence technology | |
| Wiener et al. | Differences between flax and hemp | |
| El Ouahabi et al. | A simple method for the analysis of extracellular vesicles enriched for exosomes from human serum by capillary electrophoresis with ultraviolet diode array detection | |
| LU500386B1 (en) | Method for rapidly measuring average polymerization degree of cellulose based on fluorescence technology | |
| Manson et al. | A study of graft copolymers. II. Viscosity and light‐scattering measurements | |
| CN112457502B (en) | Preparation method of composite fluorescent hydrogel and application of composite fluorescent hydrogel in detection of iron ions in water | |
| FR2643089A1 (en) | POLYAMIDE-IMIDE-BASED YARNS AND THE PROCESS FOR OBTAINING THEIR | |
| CN109632751B (en) | Method for detecting pH value based on triplet state-triplet state annihilation up-conversion fluorescence and pH detector | |
| Jiang et al. | Enhancing dye adsorption of wool by controlled and facile surface modification using sodium bisulphite | |
| CN107957403B (en) | Method for measuring chitosan content by using carmine as probe through ultraviolet spectrophotometry | |
| FR3053055A1 (en) | PROCESS FOR MARKING NANO-CELLULOSE AND / OR MICRO-FIBRILLEE SEMI-CRYSTALLINE | |
| Kimura et al. | Effect of lipid molecules on twisting motions of DNA helix studied by fluorescence polarization anisotropy | |
| CN110426323B (en) | Method for measuring permeability and coverage of chitosan slurry | |
| Kamath et al. | Microspectrophotometric study of ozone fading of disperse dyes in nylon | |
| Earland et al. | Formation of new crosslinkages in proteins by oxidation of the tyrosine residues with potassium nitrosyldisulphonate | |
| CN108458985A (en) | A method of differentiating bamboo fibre |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |