CN108548788B - AcO detection in aqueous solution-Or F-And a method for detecting the same - Google Patents
AcO detection in aqueous solution-Or F-And a method for detecting the same Download PDFInfo
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- CN108548788B CN108548788B CN201810388033.6A CN201810388033A CN108548788B CN 108548788 B CN108548788 B CN 108548788B CN 201810388033 A CN201810388033 A CN 201810388033A CN 108548788 B CN108548788 B CN 108548788B
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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
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/314—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry with comparison of measurements at specific and non-specific wavelengths
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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
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/314—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry with comparison of measurements at specific and non-specific wavelengths
- G01N2021/3155—Measuring in two spectral ranges, e.g. UV and visible
Abstract
The invention discloses a method for detecting AcO in aqueous solution‑Or F‑The reagent and the detection method thereof. The reagent is a supermolecule system solution formed by dissolving p-diaminoazobenzene and spiral fourteen-element cucurbituril in water. The method comprises the following steps: firstly, toDissolving diaminoazobenzene and spiral fourteen-element melon in water according to a certain proportion to prepare supermolecule solution; transferring the prepared supramolecular solution into a cuvette, and adding an anion solution for ultraviolet absorption spectrum determination; analyzing the ultraviolet absorption spectrum measurement, if the absorption peak of the detection liquid at 491nm gradually blues to 389nm and an equal absorption point appears at 448nm, indicating that the sample solution to be detected contains AcO‑Or F‑(ii) a If the ultraviolet absorption spectrum of the detection liquid has no obvious influence, the detection indicates that the sample solution to be detected does not contain AcO‑Or F‑. The invention has the characteristics of high detection sensitivity, low detection cost, simple sample treatment, short detection time and no need of expensive equipment.
Description
Technical Field
The invention relates to a method for detecting AcO-Or F-The reagent and the detection method thereof, in particular to the detection of AcO in aqueous solution-Or F-The reagent and the detection method thereof.
Background
The spiral fourteen-element cucurbituril is a newer cucurbituril with larger polymerization degree so far in cucurbituril family members reported for the first time by the research group. The structure is twisted, flexible, with an internal and an external helical structure. The p-diaminoazobenzene compound is an aromatic azo compound, and because the azobenzene compound contains a nitrogen-nitrogen double bond (-N-), many purposes are related to the structure, and the compound generally exists in a trans-structure, and can be changed into a cis-structure only by external stimulation (light, heat, acid and the like).
In recent years, anion recognition and detection have attracted more and more attention in various fields such as environment, medicine, nuclear energy, biology and the like, wherein anions can be combined with receptors through electrostatic interaction, hydrogen bond interaction, hydrophobic interaction and the like to generate corresponding spectral changes, so that the anions can be recognized.
Wherein AcO-Plays a role in regulating and stabilizing the acidity of hemodialysis liquid in clinical dialysis, and when the content is too low, the acidity of the hemodialysis liquid can not meet the requirement, so that Ca in the hemodialysis liquid can not meet the requirement2+And HCO3 -Reaction takes place and CaCO is formed3Precipitation, which in turn damages the dialysis machine; when the content is too high, the metabolic capability of the body is exceeded, and adverse reactions such as nausea, tiredness, muscle spasm and the like are caused, so that AcO-The accurate detection of the method has very important significance.
Fluoride ion (F)-) Is very important in health, especially in dental care and treatment of osteoporosis. Therefore, people often add fluoride to toothpastes and people's drinking water. However, when the fluorine ion is excessive, bone diseases, macular tooth, and the like can be caused.
However, the AcO is currently available-And F-The detection difficulty of the method is high, and the defects of low detection sensitivity, high detection cost, complex sample treatment, long detection time consumption and expensive detection equipment mainly exist.
Disclosure of Invention
The invention aims to provide a method for detecting AcO in a solution-Or F-The reagent and the detection method thereof. The invention has the characteristics of high detection sensitivity, low detection cost, simple sample treatment, short detection time and no need of expensive equipment.
The technical scheme of the invention is as follows: AcO detection in aqueous solution-Or F-The reagent is a supermolecular system solution formed by dissolving p-diaminoazobenzene and spiral fourteen-element cucurbituril in water.
Detection of AcO in aqueous solution as described previously-Or F-The reagent contains 2.1-4.2mg of p-diaminoazobenzene and 25.1-75.1mg of spiral fourteen-element cucurbituril in every 80-120mL of water.
Detection of AcO in aqueous solution as described previously-Or F-The reagent contains 2.1-3.2mg of p-diaminoazobenzene and 25.1-45.1mg of spiral fourteen-element cucurbituril in every 90-110mL of water.
Detection of AcO in aqueous solution as described previously-Or F-The reagent of (1), per 100mL of water, contains 2.1mg of p-diaminoazobenzene and 25.1mg of spiro-deca-quaternary cucurbituril.
Detection of AcO in aqueous solution as described previously-Or F-The structural formula of the p-diaminoazobenzene is as follows:
detection of AcO in aqueous solution as described previously-Or F-The structural formula of the spiral fourteen-element cucurbituril is as follows:
one of the aforementioned methods for detecting AcO in an aqueous solution-Or F-Detection of AcO-Or F-The method comprises the following steps:
1) preparing a detection solution: dissolving diaminoazobenzene and spiral fourteen-element melon in water according to a certain proportion to prepare supermolecule solution;
2) ultraviolet absorption spectrum determination: transferring the supramolecular solution prepared in the step 1) into a cuvette, and adding an anion solution for ultraviolet absorption spectrum determination;
3) analysis of measurement results: analyzing the ultraviolet absorption spectrum measurement in the step 2), wherein if the absorption peak of the detection solution at 491nm gradually blues to 389nm and an equal absorption point appears at 448nm, the detection indicates that the sample solution to be detected contains AcO-Or F-(ii) a If the ultraviolet absorption spectrum of the detection liquid has no obvious influence, the detection indicates that the sample solution to be detected does not contain AcO-Or F-。
Detection of AcO as described above-Or F-The method of (1), step 2), wherein the mass ratio of the supramolecular solution to the anionic solution is 1: 70-200.
Detection of AcO as described above-Or F-OfMethod, the mass ratio of the supramolecular solution to the anionic solution being 1: 100.
detection of AcO as described above-Or F-The method of (1), wherein in step 2), the ultraviolet absorption spectrum measurement is performed by an ultraviolet-visible spectrophotometer.
The invention has the advantages of
1. The invention forms a supermolecule system by utilizing p-diaminoazobenzene and a spiral fourteen-element cucurbituril, and the system is subjected to AcO-Or F-When the ultraviolet absorption spectrum is influenced, the ultraviolet absorption spectrum is strongly influenced, and the influence on AcO is reduced-Or F-Is very sensitive to the detection of AcO by test detection-Or F-Detection limit is respectively as low as 10-5mol·L-1And 10-4mol·L-1。
2. According to the invention, only two substances, namely diaminoazobenzene and spiral deca-quaternary cucurbituril, are required to form the detection reagent, and meanwhile, the detection reagent is analyzed by an ultraviolet-visible spectrophotometer, so that the reagent cost is low, and the equipment is common.
3. The reagent is slightly influenced by other anions, and the detection can be carried out by adding the reagent without carrying out excessive treatment on a sample during detection.
To further illustrate the beneficial effects of the present invention, the applicant made the following experiments:
anti-interference experiment
Taking the concentration of 2.00 × 10-5mol·L-1The reagent of the present invention, to which (100 times) of an anion of 2.00 × 10 was added-1mol·L-1(AcO-，F-，Cl-，ClO2 -，SO4 2-，NO3 -，Br-，I-，PF4 -，H2PO4 -， ClO4 -，HSO4 -) Then, ultraviolet-visible light absorption spectrometry was performed, respectively. The results are shown in FIG. 4, with addition of AcO-Or F-When the absorbance peak of the reagent at 491nm is blue-shifted to 389nm and the absorbance decreases, one at 448nm appearsThe absorption point is equal, and when other anions are added, the absorption spectrum of the reagent is hardly changed.
Drawings
FIG. 1 is a structural formula of a spiral ten-four melon ring (tQ 14);
FIG. 2 is a structural formula of p-Diaminoazobenzene (DAAB);
FIG. 3 is tQ [14]]And DAAB (2.00 × 10)-5mol·L-1) UV-visible absorption spectrum of action and A-NtQ [14]]the/NDAAB variation curves are shown by DAAB and tQ [14]]/DAAB(2.00×10-5mol·L-1) A graph under natural light;
as can be seen from FIG. 3, the fixed DAAB solution concentration was 2.00 × 10 as determined by the molar ratio method-5mol·L-1Changing tQ [14]](0, 0.2, 0.4, 0.6, 0.8, 1.0 … … 3.2.2, 3.4, 3.6, 3.8, 4.0) times before the UV-VIS absorption spectrum of the solution. DAAB solution absorbed at 389nm and tQ [14] was added]The DAAB absorption peak at 389nm is red-shifted to 491nm and the absorbance decreases, while an isoabsorbance point appears at 448 nm.
FIG. 4 shows tQ [14]]/DAAB(2.00×10-5mol·L-1) Uv-vis absorption spectra with different anions (100 x);
FIG. 5 shows tQ [14]]/DAAB(2.00×10-5mol·L-1) Graph under natural light with different anions (100 times);
FIG. 6 shows tQ [14]]/DAAB(2.00×10-5mol·L-1) With different concentrations of AcO-Ultraviolet titration chart and calibration curve;
as can be seen from FIG. 6, at a concentration of 2.00 × 10-5mol·L-1tQ[14]Adding AcO with different concentrations into the solution of/DAAB-With AcO-Respectively, and the absorption spectrum curves are measured. tQ [14]]The absorption peak of/DAAB at 491nm gradually blued to 389nm, with an isoabsorption point at 448 nm. The specific absorption is formed at wavelengths of 491nm and 389 nm.
FIG. 7 shows tQ [14]]/DAAB(2.00×10-5mol·L-1) With different concentrations of F-Ultraviolet titration chart and working curve;
as can be seen from FIG. 7, at a concentration of 2.00 × 10-5mol·L-1tQ[14]Adding F with different concentrations into the solution of/DAAB-With F-Respectively, and the absorption spectrum curves are measured. tQ [14]]The absorption peak of/DAAB at 491nm gradually blued to 389nm, with an isoabsorption point at 448 nm. The specific absorption is formed at wavelengths of 491nm and 389 nm.
Detailed Description
The present invention is further illustrated by the following examples, which are not to be construed as limiting the invention.
Examples of the invention
Example 1: AcO detection in aqueous solution-Or F-The reagent of (1), per 100mL of water, contains 2.1mg of p-diaminoazobenzene and 25.1mg of spiro-deca-quaternary cucurbituril.
Example 2: AcO detection in aqueous solution-Or F-The reagent of (1) contains 2.8mg of p-diaminoazobenzene and 35.1mg of spiro-deca-quaternary cucurbituril per 80mL of water.
Example 3: AcO detection in aqueous solution-Or F-The reagent of (1) contains 3.2mg of p-diaminoazobenzene and 55.1mg of spiro-deca-quaternary cucurbituril per 90mL of water.
Example 4: AcO detection in aqueous solution-Or F-The reagent of (1) contains 3.7mg of p-diaminoazobenzene and 65.1mg of spiro-deca-quaternary cucurbituril per 110mL of water.
Example 5: AcO detection in aqueous solution-Or F-The reagent of (4.2 mg of p-diaminoazobenzene and 75.1mg of spiro-deca-quaternary cucurbituril per 120mL of water.
Example 6: AcO detection in aqueous solution-Or F-The method comprises the following steps:
1) preparing a detection solution: dissolving diaminoazobenzene and spiral fourteen-element cucurbituril in water according to a proportion to prepare a supermolecule solution;
2) ultraviolet absorption spectrum determination: transferring the supramolecular solution prepared in the step 1) into a cuvette, respectively adding an anion solution, and performing ultraviolet absorption spectrometry by using an ultraviolet-visible spectrophotometer, wherein the mass ratio of the supramolecular solution to the anion solution is 1: 100, respectively;
3) analysis of measurement results: analyzing the ultraviolet absorption spectrum measurement in the step 2), wherein if the absorption peak of the detection solution at 491nm gradually blues to 389nm and an equal absorption point appears at 448nm, the detection indicates that the sample solution to be detected contains AcO-Or F-(ii) a If the ultraviolet absorption spectrum of the detection liquid has no obvious influence, the detection indicates that the sample solution to be detected does not contain AcO-Or F-。
Example 7: AcO detection in aqueous solution-Or F-The procedure of (1) is the same as in example 6, except that the mass ratio of the supramolecular solution to the anionic solution in this example is 1: 70.
Example 8: AcO detection in aqueous solution-Or F-The procedure of (1) is the same as in example 6, except that the mass ratio of the supramolecular solution to the anionic solution in this example is 1: 200.
example 9: a method for detecting AcO-or F-in an aqueous solution, comprising the steps of:
1)tQ[14]preparation of DAAB solution: 2.1mg of DAAB, 25.1mg of tQ [14] were weighed out]Dissolving to obtain 100mL solution with concentration of 1.00 × 10-4mol·L-1；
2)AcO-Solution: 637.0mg of analytically pure tetrabutylammonium acetate were weighed out, dissolved in redistilled water and made into 10mL of solution, AcO-Has a concentration of 2.00 × 10-1mol·L-1Diluting the mixture to proper concentration step by using secondary distilled water according to needs;
3)F-solution: 522.9mg of tetrabutylammonium fluoride was weighed out and dissolved in redistilled water to prepare a 10mL solution, F-The concentration is 2.00 × 10-1mol·L-1The preparation of other coexisting anion solution is the same as that;
4) to a 10.0mL volumetric flask was added tQ [14]]Solution of/DAAB (1.00 × 10)-4mol·L-12000. mu.L), anionic AcO-Solutions ofOr F-Solution (2.00 × 10)-1mol·L -1100. mu.L). Diluting with secondary distilled water to scale, shaking, transferring into 1cm quartz cuvette, and measuring by ultraviolet absorption spectrum. Other anions (Cl)-，ClO2 -，SO4 2-，NO3 -，Br-，I-，PF4 -，H2PO4 -，ClO4 -，HSO4 -) Ultraviolet absorption spectroscopy was as above. AcO-Or F-Enable tQ [14]The absorption peak of/DAAB at 491nm gradually blued to 389nm, with an isoabsorption point at 448 nm. That is, with the exception of AcO-Or F-Is added to tQ [14]]In addition to the significant absorption signal of/DAAB, other anions (Cl)-，Br-， I-，HSO4 -，NO3 -，AcO-，ClO4 -，PF6 -，H2PO4 -) To tQ [14]No UV absorption response signal was evident for either/DAAB (FIG. 4).
The ultraviolet-visible spectrophotometer used in the present invention is UV-1800, manufactured by Shimadzu corporation of Japan.
tQ [14] in the method of the invention]/DAAB as trace AcO-Or F-A specific absorption reagent for detection of ions; the method has the advantages of excellent detection performance, good detection stability, small background interference, high selectivity, low detection limit, no need of separation, capability of testing under a water-soluble condition and the like. Simple operation and control method and unique performance.
At tQ [14]In DAAB solution, AcO was measured at different concentrations-Or F-To tQ [14]The absorbance change at 491nm for/DAAB was determined, and calibration curves were obtained (shown in FIG. 5 (b) and FIG. 6 (b)). tQ [14] is determined and calculated from the slope of the calibration curve and the standard deviation of the blank value determined 10 times, respectively]/DAAB detection of AcO-Or F-The calibration curve, linear coefficient and detection limit of the ions are shown in table 1.
TABLE 1 tQ [14]/DAAB detection of AcO-And F-Analysis parameter of
| Ion(s) | Calibration curve | R2 | Detection limit (mol/L) |
| AcO- | ΔA＝-0.0058c-0.60 | 0.990 | 5.17×10-4 |
| F- | ΔA＝-0.0013c-0.52 | 0.988 | 1.84×10-4 |
Claims (8)
1. AcO detection in aqueous solution-Or F-The reagent of (2), characterized in that: is a supermolecular system solution formed by dissolving p-diaminoazobenzene and spiral fourteen-element cucurbituril in water.
2. Detection of AcO in aqueous solution according to claim 1-Or F-The reagent of (2), characterized in that: every 80-120mL of water contains 2.1-4.2mg of p-diaminoazobenzene and 25.1-75.1mg of spiral fourteen-element cucurbituril.
3. A water soluble polymer according to claim 1Detection of AcO in liquid-Or F-The reagent of (2), characterized in that: every 90-110mL of water contains 2.1-3.2mg of p-diaminoazobenzene and 25.1-45.1mg of spiral fourteen-element cucurbituril.
4. Detection of AcO in aqueous solution according to claim 2-Or F-The reagent of (2), characterized in that: every 100mL of water contains 2.1mg of p-diaminoazobenzene and 25.1mg of spiral fourteen-element cucurbituril.
5. Detection of AcO in aqueous solution using any of claims 1-4-Or F-Detection of AcO-Or F-The method is characterized by comprising the following steps:
1) preparing a detection solution: dissolving diaminoazobenzene and spiral fourteen-element melon in water according to a certain proportion to prepare supermolecule solution;
2) ultraviolet absorption spectrum determination: transferring the supramolecular solution prepared in the step 1) into a cuvette, and adding an anion solution for ultraviolet absorption spectrum determination;
3) analysis of measurement results: analyzing the ultraviolet absorption spectrum measurement in the step 2), wherein if the absorption peak of the detection solution at 491nm gradually blues to 389nm and an equal absorption point appears at 448nm, the detection indicates that the sample solution to be detected contains AcO-Or F-(ii) a If the ultraviolet absorption spectrum of the detection liquid has no obvious influence, the detection indicates that the sample solution to be detected does not contain AcO-Or F-。
6. The method of detecting an AcO of claim 5-Or F-The method of (2), characterized by: in step 2), the mass ratio of the supramolecular solution to the anionic solution is 1: 70-200.
7. The method of detecting an AcO of claim 6-Or F-The method of (2), characterized by: the mass ratio of the supramolecular solution to the anionic solution is 1: 100.
8. the method of detecting an AcO of claim 5-Or F-The method of (2), characterized by: in the step 2), the ultraviolet absorption spectrum measurement is performed by an ultraviolet-visible spectrophotometer.
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