CN116698776A - Color development-free spectrophotometry for quantitatively analyzing chitosan - Google Patents
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Abstract
The invention relates to the technical field of macromolecular detection, in particular to a color development-free spectrophotometry for quantitatively analyzing chitosan. According to the invention, the absorbance value is increased along with the increase of the chitosan content in a certain concentration range by utilizing the chitosan solution under the wavelength of 190-195 nm, and a certain linear relationship is presented, so that the quantitative basis of chitosan is used, and a color development-free spectrophotometry for analyzing chitosan is established. The method of the invention does not need to add a color developing agent, reduces various interference factors in the color developing link, has low requirements on instruments and equipment, is simple to operate, and ensures the quantitative stability and reproducibility. The method has excellent applicability to quantitative analysis of chitosan in a controllable system (or a pure system) without the interference of other organic molecules or inorganic ligands.
Description
Technical Field
The invention relates to the technical field of macromolecular detection, in particular to a color development-free spectrophotometry for quantitatively analyzing chitosan.
Background
Chitosan is a polyelectrolyte rich in amino and hydroxyl functional groups and has multifunctional natural activity. For the last twenty years, researchers have received extensive attention in the fields of medicine, food, chemical industry, environmental protection and the like. Chitosan has many natural excellent properties such as moisture absorption and air permeability, biocompatibility, biodegradability, no antigenicity, no inflammatory, no harmful degradation products, adhesiveness, antibacterial property, etc., and thus is widely used in textile industry, biomedical science, daily environmental protection, etc.
In the fields of interaction of chitosan and solid phase and modification of chitosan, quantitative research of chitosan is necessary for deep research on related research mechanisms, and an accurate quantitative method is worthy of exploration.
Currently, methods for quantifying chitosan mainly include colorimetric detection, size exclusion chromatography, high performance liquid chromatography, elemental analysis, ultraviolet spectroscopy, and the like (table 1). Size exclusion chromatography, high performance liquid chromatography, elemental analysis, ultraviolet spectroscopy are relatively high in instrument conditions or operational details, and ninhydrin colorimetry is relatively common due to the high popularity of spectrophotometers. However, the ninhydrin colorimetric method comprises a mixed heating color development link of the ninhydrin, and the color development result is easily influenced by pH, temperature and color development time, and the defects of condensation reaction, uneven heating and photolysis with time of chitosan and the ninhydrin are respectively generated. Based on the method, development of a chitosan color-development-free quantitative method with strong applicability, simple operation and high accuracy is necessary.
Table 1: advantages and disadvantages of the existing chitosan quantification method
Disclosure of Invention
In order to solve the technical problems, the invention provides a color development-free spectrophotometry for quantitatively analyzing chitosan. The invention uses chitosan solution to increase absorbance value along with the increase of chitosan content in a certain concentration range under 190-195 nm wavelength, and presents a certain linear relation. Based on the quantitative analysis of chitosan, a color development-free spectrophotometry for analyzing chitosan is established.
A color-less spectrophotometry for quantitative analysis of chitosan, comprising the steps of:
(1) Drawing a standard curve: precisely weighing chitosan reference substance, and adding HClO with concentration of more than 1M 4 The aqueous solution (preferably 1M, M is mol/L, the same applies below) is immersed and dissolved, and then ultrapure water is added to HClO 4 The concentration of (2) is 0.01M, and shaking up is carried out to obtain a linear stock solution; with 0.01M HClO 4 Diluting the linear stock solution to different chitosan concentrations (the chitosan concentration is in the range of 0.1-50 mg/L) by using the aqueous solution to obtain a linear solution; detecting the absorbance of each linear solution by taking ultrapure water as a reference solution under the wavelength of 190-195 nm, and adjusting the absorbance value measured by the reference solution to 0; the absorbance of the chitosan-containing solution is marked as A, the chitosan concentration is taken as an abscissa, and the A is taken as an ordinate, so that a standard curve is drawn.
(2) Sample detection: precisely weighing the sample, and adding HClO with concentration of more than 1M 4 The aqueous solution (preferably 1M) is immersed and dissolved, and ultrapure water is added to HClO 4 The concentration of (2) is 0.01M, and shaking uniformly; the absorbance value measured by the reference solution is adjusted to 0 by taking ultrapure water as the reference solution at the wavelength of 190-195 nm, the absorbance of the sample solution is detected and is marked as A, and if A exceeds the linear range, 0.01M HClO is used 4 Diluting the aqueous solution to obtain a sample solution with proper concentration;
substituting A into the standard curve equation in the step (1) to obtain chitosan concentration, multiplying the chitosan concentration by dilution times, and multiplying the obtained concentration (mass volume concentration) by the volume to obtain the mass of chitosan; and calculating the content of chitosan in the sample according to the mass of chitosan/the sample weighing amount of the sample.
The chitosan contained in the chitosan reference substance and the sample is low molecular weight chitosan, the viscosity is 20-300cP, and the deacetylation degree is more than 75%;
or the chitosan contained in the chitosan reference substance and the sample is medium molecular weight chitosan, the viscosity is 200-800cP, and the deacetylation degree is more than 75%;
or the chitosan contained in the chitosan reference substance and the sample is high molecular weight chitosan, the viscosity is more than 400cP, and the deacetylation degree is more than 75%;
in the method of the invention, no other organic substances or inorganic ligands exist in the test sample.
Preferably, the sample is an adsorption system of an inorganic mineral adsorption material-chitosan solution, wherein the inorganic mineral adsorption material comprises at least one of montmorillonite, kaolinite, illite, magnetite and the like.
Compared with the prior art, the invention has the beneficial effects that:
compared with the prior art, the method does not need to add a color developing agent, reduces various interference factors in a color developing link, has low requirements on instruments and equipment, is simple to operate, and ensures quantitative stability and reproducibility. The method has excellent applicability to quantitative analysis of chitosan in a controllable system (or a pure system) without the interference of other organic molecules or inorganic ligands.
Drawings
FIG. 1 is a scanning spectrum of low molecular weight chitosan with different concentrations in the range of 190-300 nm;
FIG. 2 is a scanning spectrum of the medium molecular weight chitosan with different concentrations in the range of 190-300 nm;
FIG. 3 is a scan pattern of high molecular weight chitosan at 190-300 nm at different concentrations;
FIG. 4 is a linear relationship diagram of low molecular weight chitosan;
FIG. 5 is a graph of the linear relationship of medium molecular weight chitosan;
FIG. 6 is a graph showing the linear relationship of high molecular weight chitosan.
Detailed Description
The present invention is further described below by the applicant in connection with examples and the accompanying drawings, but the scope of the present invention is not limited to these examples. It will be understood by those skilled in the art that equivalent substitutions and corresponding modifications to the technical features of the present invention are included within the scope of the present invention.
The experimental methods used in the following examples are all conventional methods unless otherwise specified; the water used is ultrapure water (resistivity > 18.25 M.OMEGA.cm); materials, reagents and the like used, unless otherwise indicated, are all commercially available.
In the following examples, low molecular weight (20-300 cP, degree of deacetylation > 75%), medium molecular weight (200-800 cP, degree of deacetylation > 75%) and high molecular weight (> 400cP, degree of deacetylation > 75%) chitosan were used as test subjects, and the low, medium and high molecular weight chitosan were purchased from Sigma-Aldrich, product codes 102428982, 102466447 and 102473231, respectively, and the production standards were: CAS No.9012-76-4.
The apparatus used in the examples below was a dual beam spectrophotometer (Beijing Pu Zhou TU-1901, wavelength range 190-700 nm).
Example 1: analytical method establishment
1) Wavelength selection
Saturated hydrocarbon derivatives containing O, N, S, halogen and other heteroatoms can generate light absorption at 150-250 nm, which provides a basic basis for the color development-free quantification of chitosan. The ultra-pure water scanning spectrum is firstly used for detecting the stability of the short wave band of the machine, so that the ultra-pure water short wave is ensured to have no obvious light absorption. The ultra-pure water spectral line is taken as a baseline, and the low, medium and high molecular weight chitosan solutions with different concentrations are swept in the range of 190-300 nm, as shown in figures 1-3.
The preparation process of the chitosan solution comprises the following steps: with 10mL of 1M HClO 4 Soaking in water solution, dissolving 0.1g chitosan, and adding ultrapure water to HClO 4 The concentration of the chitosan is 0.01M, shaking is carried out uniformly, and the concentration of the chitosan is 100mg/L; then using 0.01M HClO 4 The chitosan solution is diluted into different concentrations (low, medium and high molecular weight chitosan is prepared by the same method) by aqueous solution.
From FIGS. 1-3, it can be seen that 190nm is the absorption peak in the range, but considering that 190nm is the critical detection wavelength of the instrument, there may be instability of the instrument at this wavelength, so the present invention selects 195nm as the wavelength for quantitative detection.
2) Solvent selection (influence of anions)
Under electromagnetic radiation, some inorganic substances can generate light absorption due to charge migration transition and coordination field transition, and before shortwave non-chromogenic quantification of chitosan is realized, the influence on accurate quantification of chitosan under the coexistence of various ligands and other anions and cations is required to be cleared.
Considering the size range of chitosan absorbance, we consider that absorbance error of 0.01 can be subtracted by correction, while absorbance of 0.1 can have an effect on chitosan quantification.
Aqueous sulfuric acid, nitric acid, hydrochloric acid, perchloric acid and acetic acid solutions of different concentrations were prepared, the absorbance of each solution was measured at a wavelength of 195nm using ultrapure water as a reference solution, and the effect of acid radical ions (inorganic ligands) was examined, and the results are shown in tables 2 and 3 below:
table 2: concentration range of anion absorbance greater than 0.01
Table 3: concentration range of anion absorbance greater than 0.1
As can be seen from tables 2 and 3, the light absorption coefficient of perchlorate is the smallest at 195nm wavelength; whereas chitosan is insoluble in water, alkali and general organic solvents, but can be dissolved in dilute acid. In summary, the present invention selects 0.01mol/L perchloric acid as the solvent.
3) Influence investigation of cations
Preparing KClO with different concentrations 4 、NaClO 4 、Ca(ClO 4 ) 2 、Mg(ClO 4 ) 2 The absorbance of each solution was measured at a wavelength of 195nm using an aqueous solution and ultrapure water as a reference solution, and the results are shown in table 4 below:
table 4: concentration range of cation absorbance greater than 0.01 (subtracting 0.01M perchlorate absorbance)
Conclusion: at 195nm wavelength, the usual K, na, ca, mg (perchlorate) cations have little interference with the process of the invention.
4) Investigation of the influence of pH
Hydroxyl ions were tested to give an absorbance of about 0.008 at 195nm at a concentration of 0.00001mol/L (0.00001 mol/L NaOH solution); and the higher the concentration of hydroxide ions, the higher the absorbance (because hydroxide is a stronger ligand, charge migration transition occurs under electromagnetic radiation, and light absorption occurs), and the absorbance of 0.01mol/L NaOH exceeds the detection limit of the method. While in an acidic or neutral environment, there is little light absorption due to hydrogen ions. Whereas chitosan itself is only protonated and soluble below ph6.3, so the effect of hydroxyl groups is negligible.
Example 2: analytical method validation
1) Linearity test
Linear stock solution: respectively precisely weighing 0.1g of chitosan with different molecular weights, and adding 10mL of 1M HClO 4 The aqueous solution was immersed and dissolved, and ultrapure water was added to 1L, and the mixture was shaken to prepare a linear stock solution.
Linear solution: taking proper amount of linear stock solution, and using 0.01M HClO 4 The aqueous solutions were diluted to 0.1, 0.2, 0.5, 1, 2, 5, 10, 20, 50mg/L, respectively, as linear solutions.
The absorbance value was adjusted to 0 by using ultrapure water as a reference solution, and the absorbance of each linear solution was measured at a wavelength of 195nm and designated as A. Standard curves are plotted on the abscissa with concentration and on the ordinate with a, see fig. 4, 5 and 6, with the results given in tables 5 (corresponding to fig. 4), 6 (corresponding to fig. 5) and 7 (corresponding to fig. 6):
table 5: linear test results of Low molecular weight chitosans
Table 6: linear test results of medium molecular weight chitosan
Table 7: results of linear experiments on high molecular weight chitosan
2) Repeatability test
Repeatability test solution: low, medium and high molecular weight chitosan (10 mg/L, prepared as a solution according to the linear test item of the present example) was prepared separately. The absorbance A of the above concentration sample was measured at a wavelength of 195nm by adjusting the absorbance to 0 using ultrapure water as a reference solution. Substituting absorbance A into 1) a corresponding standard curve equation in the linear test to obtain the measured concentration. Recovery = (measured concentration × 100/formulated concentration)%.
Table 8: results of the chitosan repeatability test (%)
Conclusion: repeating for 5 times, the recovery rate is 103.5% -108.5%, the recovery rate RSD is 0.55-3.09, and the repeatability of the method is good.
Claims (6)
1. A color-less spectrophotometry for quantitative analysis of chitosan, comprising the steps of:
(1) Drawing a standard curve: precisely weighing chitosan reference substance, and usingHClO with concentration of more than 1M 4 Soaking in water solution, dissolving, and adding ultrapure water to HClO 4 The concentration of (2) is 0.01M, and shaking up is carried out to obtain a linear stock solution; with 0.01M HClO 4 Diluting the linear stock solution to different chitosan concentrations by using the aqueous solution to obtain a linear solution, wherein the chitosan concentration is in the range of 0.1-50 mg/L; detecting the absorbance of each linear solution by taking ultrapure water as a reference solution at the wavelength of 190-195 nm, and marking the absorbance as A; drawing a standard curve by taking the concentration as an abscissa and the A as an ordinate;
(2) Sample detection: precisely weighing the sample, and adding HClO with concentration of more than 1M 4 Soaking in water solution, dissolving, and adding ultrapure water to HClO 4 The concentration of (2) is 0.01M, and shaking uniformly; detecting absorbance of a sample solution by taking ultrapure water as a reference solution at a wavelength of 190-195 nm, and marking the absorbance as A; substituting A into the standard curve equation in the step (1) to obtain chitosan concentration, and then calculating the chitosan content in the sample;
the chitosan contained in the chitosan reference substance and the sample is low molecular weight chitosan, the viscosity is 20-300cP, and the deacetylation degree is more than 75%;
or the chitosan contained in the chitosan reference substance and the sample is medium molecular weight chitosan, the viscosity is 200-800cP, and the deacetylation degree is more than 75%;
or the chitosan contained in the chitosan reference substance and the sample is high molecular weight chitosan, the viscosity is more than 400 and cP, and the deacetylation degree is more than 75%.
2. The color-free spectrophotometry of claim 1, wherein the detection wavelength is 195 nm.
3. The color-less spectrophotometry according to claim 1, wherein HClO is used for dissolving chitosan control and test sample 4 Is 1M.
4. A color-free spectrophotometry according to any of claims 1-3, wherein no other organic substance, or inorganic ligand is present in the sample.
5. The method according to claim 4, wherein the sample is an adsorption system of chitosan solution, which is an inorganic mineral adsorption material.
6. The color-less spectrophotometry of claim 5, wherein the inorganic mineral adsorbing material is one or more of montmorillonite, kaolinite, illite, magnetite.
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