CN112958055B - Adsorbing material for water pollutants, preparation method and mass spectrum detection application thereof - Google Patents
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Abstract
The invention relates to the technical field of analysis and detection, in particular to an adsorbing material for water pollutants, and a preparation method and application thereof. The adsorbing material for the water pollutants comprises a paper substrate and fluorine-doped boron nitride attached to the surface of the paper substrate, and the paper sheet is only required to be immersed in fluorine-doped boron nitride-absolute ethyl alcohol dispersion liquid, soaked, taken out and dried. The fluorine-doped boron nitride is attached to the surface of the paper base, and the interaction between hydroxyl on the surface of the paper base material and the target can be weakened due to the hydrophobicity of the fluorine-doped boron nitride, so that the target can be desorbed more easily under the elution effect of the eluent. In addition, the fluorine-doped boron nitride has certain conductivity, so that a target object can be better ionized, and the detection sensitivity is improved.
Description
Technical Field
The invention relates to the technical field of analysis and detection, in particular to an adsorbing material for water pollutants, a preparation method thereof and mass spectrometry detection application.
Background
The information disclosed 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.
Environmental pollution is one of the most significant concerns of the modern society public. Through the analysis to the pollutant in the environmental water, can carry out environmental monitoring better, have the significance to the protection people health. Bisphenol a has long been used in the manufacture of plastic (milk) bottles, drinking cups for infants, food and beverage (milk powder) can inside coatings, with its silhouettes ranging from mineral water bottles, medical devices to and within food packaging. Bisphenol A is also thought to be involved in endocrine disorders, cancer and obesity caused by metabolic disorders. The european union considered that the baby bottles containing bisphenol a induced precocious ripening, and therefore prohibited the production of baby bottles containing bisphenol a. Tetrabromobisphenol A is one of the most widely used bromine flame retardants worldwide at present, and is widely applied to textile, household electrical appliances and industrial products to reduce the combustion performance. Tetrabromobisphenol a is a potential organic contaminant with persistence, bioaccumulation, and toxicity. The research shows that it has obvious toxic side effect on algae, fish, mollusk, etc. However, due to the complex water matrix of the environment, the detection of water pollutants is seriously affected.
The paper spray ionization technology is a novel atmospheric pressure ionization technology, and the principle is that a triangular paper substrate is used as a carrier for sample separation and ionization, a sample or a spray solvent is dripped onto the paper substrate during analysis, and a target analyte is ionized under high pressure and then enters a detector for detection. The paper spraying technology can overcome the defects of the traditional ionization technology to a certain extent, and has the advantages of simple operation, low price and no need of carrying out a complex pretreatment process on the product. However, the inventors found after the study that due to the existence of hydroxyl groups on the surface of the paper substrate, when the target compound is analyzed by using paper spray, certain functional groups of the compound can form hydrogen bonds with the hydroxyl groups, so that the compound is difficult to elute in a short time, thereby reducing the sensitivity of the paper spray mass spectrum.
Disclosure of Invention
In order to solve the problem that when a target compound is analyzed by using paper spraying, certain functional groups of the compound can form hydrogen bonds with hydroxyl groups, so that the compound is difficult to elute in a short time, and the sensitivity of paper spraying mass spectrometry is reduced, the invention finds that fluorine-doped boron nitride has the characteristics of hydrophobicity, promotion of ionization and certain conductivity, and provides an adsorbing material for water pollutants, a preparation method and application thereof for the first time according to the characteristic of the fluorine-doped boron nitride. The fluorine-doped boron nitride is attached to the surface of the paper base, and the interaction between hydroxyl on the surface of the paper base and the target can be weakened due to the hydrophobicity of the fluorine-doped boron nitride, so that the target can be desorbed under the elution effect of the eluent more easily.
Specifically, the invention is realized by the following technical scheme:
the invention provides an adsorbing material for water pollutants, which comprises a paper substrate and fluorine-doped boron nitride attached to the surface of the paper substrate.
In a second aspect of the present invention, a preparation method of an adsorption material for water body pollutants is provided, which comprises: and (3) immersing the paper sheet into fluorine-doped boron nitride-absolute ethyl alcohol dispersion liquid, soaking, taking out and airing.
The third aspect of the invention provides application of an adsorbing material for water pollutants in a paper spray mass spectrometry detection device.
In a fourth aspect of the invention, the application of fluorine-doped boron nitride in an adsorption material for water pollutants and/or a paper spray mass spectrometry detection device is provided.
In a fifth aspect of the present invention, a paper spray mass spectrometry detection apparatus for detecting water pollutants is provided, which is characterized by comprising:
an adsorbent material for organic contaminants;
a mass spectrometer;
and one end of the metal clamp is connected with an external high-voltage direct-current power supply, and the other end of the metal clamp clamps the paper substrate loaded with the fluorine-doped boron nitride, so that the tip of the adsorbing material is aligned to a sample inlet of the mass spectrometer.
The invention provides a paper spray mass spectrometry detection method of water pollutants, which is characterized by comprising the following steps:
preparing an adsorbing material of water pollutants;
water sample pretreatment and preparation of an adsorption material with a target object;
clamping the adsorbing material adsorbed with the target object by using a metal clamp, injecting an elution solvent onto the adsorbing material, and applying high-voltage electricity to the adsorbing material to realize desorption of the target object and simultaneously form electrospray of the target object at the tip of the paper substrate;
the electrospray is received by a mass spectrometer for detection.
One or more embodiments of the present invention have the following advantageous effects:
1) the fluorine-doped boron nitride is attached to the surface of the paper base, and the interaction between hydroxyl on the surface of the paper base material and the target can be weakened due to the hydrophobicity of the fluorine-doped boron nitride, so that the target can be desorbed more easily under the elution effect of the eluent.
2) The fluorine-doped boron nitride has certain conductivity, so that a target object can be better ionized, and the detection sensitivity is improved.
3) The fluorine-doped boron nitride is attached to the paper base, other adhesives are not needed, and the adsorbing material for water pollutants is efficiently and quickly prepared;
4) a new paper spray mass spectrometry detection method is established, the advantages of fluorine-doped boron nitride are combined with the characteristics of a paper spray mass spectrometry method, and efficient detection is realized.
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. Embodiments of the invention are described in detail below with reference to the attached drawing figures, wherein:
FIG. 1 is a transmission electron microscopy characterization of fluorine-doped boron nitride prepared in example 1 of the present invention;
FIG. 2 is a contact angle of fluorine-doped boron nitride prepared in example 1 of the present invention;
FIG. 3 is a scanning electron micrograph of an unmodified paper substrate according to example 2 of the present invention;
FIG. 4 is a scanning electron microscope image of the paper substrate modified with fluorine-doped boron nitride in example 2 of the present invention;
FIG. 5 is a schematic diagram of a detection process in embodiment 3 of the present invention, which sequentially includes a few layers of fluorine-doped boron nitride nanosheets, fluorine-doped boron nitride coated paper, sample addition, elution sample injection, and mass spectrum signals;
fig. 6 is a comparison of the water sample of the microcuvette for detecting water pollutants by using the hollow paper and the water pollutant adsorbing material in example 4 of the present invention.
FIG. 7 is a comparison of the adsorption materials of hollow white paper and water pollutants in the detection of a black tiger spring water sample for water pollutants in example 4 of the present invention;
wherein: 1. the adsorption material of organic pollutant, 2, mass spectrograph, 3, metal clamp, 4, external high voltage direct current power supply.
Detailed Description
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Experimental procedures without specific conditions noted in the following examples, generally according to conventional conditions or according to conditions recommended by the manufacturers.
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 example embodiments according to the present disclosure. 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 order to solve the problem that when a target compound is analyzed by using paper spraying, certain functional groups of the compound can form hydrogen bonds with hydroxyl groups, so that the compound is difficult to elute in a short time, and the sensitivity of paper spraying mass spectrometry is reduced, the invention finds that fluorine-doped boron nitride has the characteristics of hydrophobicity, promotion of ionization and certain conductivity, and provides an adsorbing material for water pollutants, a preparation method and application thereof for the first time according to the characteristic of the fluorine-doped boron nitride. The fluorine-doped boron nitride is attached to the surface of the paper base, and the interaction between hydroxyl on the surface of the paper base material and the target can be weakened due to the hydrophobicity of the fluorine-doped boron nitride, so that the target can be desorbed more easily under the elution effect of the eluent.
Specifically, the invention is realized by the following technical scheme:
the invention provides an adsorbing material for water pollutants, which comprises a paper substrate and fluorine-doped boron nitride attached to the surface of the paper substrate.
The inventors have studied and found that due to the presence of hydroxyl groups on the surface of a paper substrate, when a target compound is analyzed using paper spray, certain functional groups of the compound may form hydrogen bonds with the hydroxyl groups, resulting in a difficulty in eluting the compound in a short period of time, thereby reducing the sensitivity of paper spray mass spectrometry. The fluorine-doped boron nitride is loaded on the surface of the paper substrate to prepare the adsorption material of the water pollutants, the fluorine-doped boron nitride is attached to the surface of the paper substrate, and the hydrophobic property of the fluorine-doped boron nitride can weaken the interaction between hydroxyl on the surface of the paper substrate and a target object, so that the target object can be desorbed more easily under the elution effect of the eluent. And the fluorine-doped boron nitride has certain conductivity, so that a target object can be better ionized, and the detection sensitivity is improved.
In one or more embodiments of the invention, the paper substrate is a paper substrate in paper spray ionization, which is shaped as an isosceles triangle.
In a second aspect of the present invention, a preparation method of an adsorption material for water body pollutants is provided, which comprises: and (3) immersing the paper sheet into fluorine-doped boron nitride-absolute ethyl alcohol dispersion liquid, soaking, taking out and airing.
The preparation method of the fluorine-doped boron nitride comprises the following steps:
mixing boron nitride powder with isopropanol solution, stirring, cooling, performing ultrasonic treatment, standing, performing centrifugal washing, drying to obtain single-layer or few-layer boron nitride, stirring the single-layer or few-layer boron nitride and fluoboric acid, cooling, performing centrifugal washing, and drying to obtain the boron nitride.
In one or more embodiments of the invention, the ratio of boron nitride powder to isopropyl alcohol is 0.2-2 g: 30-80mL, preferably 0.5 g: 50 mL;
preferably, the boron nitride powder is mixed with an isopropanol solution, stirred for 18-30h at 40-60 ℃, cooled to room temperature, ultrasonically treated for 15-25h, kept stand for 0.5-2 days, and washed with acetone;
preferably, the boron nitride powder is mixed with an isopropanol solution, stirred for 24 hours at 50 ℃, subjected to ultrasonic treatment for 20 hours, and kept stand for 1 day;
preferably, the ratio of the single layer or few layers of boron nitride to the fluoroboric acid is 0.2-2 g: 30-80mL, preferably 0.5 g: 50 mL;
preferably, the single-layer or few-layer boron nitride and the fluoroboric acid are mixed and stirred for 5-10h at the temperature of 40-60 ℃, cooled to room temperature and washed by deionized water;
preferably, the single-layer or few-layer boron nitride and the fluoroboric acid are mixed and stirred for 8 hours at 50 ℃;
in one or more embodiments of the present invention, in the fluorine-doped boron nitride-absolute ethanol dispersion, the concentration of fluorine-doped boron nitride is 0.5-3mg/mL, preferably 1 mg/mL;
preferably, the soaking time is 0.2-3h, preferably 1.5 h.
In a third aspect of the invention, an application of an adsorption material for water pollutants in a paper spray mass spectrometry detection device is provided.
In a fourth aspect of the invention, there is provided the use of fluorine-doped boron nitride in an adsorbent material for water pollutants and/or a paper spray mass spectrometry detection apparatus.
In a fifth aspect of the present invention, a paper spray mass spectrometry detection apparatus for detecting water pollutants is provided, which is characterized by comprising:
an adsorbent material for organic contaminants;
a mass spectrometer;
and one end of the metal clamp is connected with an external high-voltage direct-current power supply, and the other end of the metal clamp clamps the paper substrate loaded with the fluorine-doped boron nitride, so that the tip of the adsorbing material is aligned to a sample inlet of the mass spectrometer.
Preferably, the voltage of the external high-voltage direct-current power supply is-3 KV to-4 KV, and is preferably-3.5 KV.
The invention provides a paper spray mass spectrometry detection method of water pollutants, which is characterized by comprising the following steps:
preparing an adsorbing material of water pollutants;
water sample pretreatment and preparation of an adsorption material with a target object;
clamping the adsorbing material adsorbed with the target object by using a metal clamp, injecting an elution solvent onto the adsorbing material, and applying high-voltage electricity to the adsorbing material to realize desorption of the target object and simultaneously form electrospray of the target object at the tip of the paper substrate;
the electrospray is received by a mass spectrometer for detection.
In one or more embodiments of the invention, the water sample pretreatment refers to filtering the water samples through a 0.22 μm water system filter membrane, diluting the water samples by 10 times with purified water, and adding bisphenol a and tetrabromobisphenol a;
preferably, the preparation of the adsorption material with the target object is specifically that 20 μ L of water sample is dripped on the adsorption material of the water body pollutants and dried at 37 ℃;
preferably, the elution solvent is methanol: water 9:1 by volume, and 1% by volume of aqueous ammonia was added to the elution solvent. The ionization efficiency of the analyte can be improved by using ammonia or triethylamine in a negative ion mode.
The present invention is described in further detail below with reference to specific examples, which should be construed as illustrative rather than restrictive.
Example 1
Preparation of fluorine-doped boron nitride
(1) Preparation of single-layer or few-layer boron nitride: 0.5g of boron nitride powder was placed in a 100mL round bottom flask, and 50mL of isopropanol was added. The mixture was magnetically stirred at 50 ℃ for 24 h. After cooling to room temperature, the mixture was sonicated in a low power sonicator for 20 h. After the ultrasonic treatment is finished, standing the obtained mixed solution at room temperature for 1 day, then extracting the supernatant for centrifugation, and washing the centrifuged milky white precipitate with acetone for several times so as to clean the isopropanol. The resulting product was dried at 60 ℃ and collected for future use.
(2) Single or few layer hexagonal boron nitride doped with fluorine: 0.5g of hexagonal boron nitride in a small amount was put into a 100mL round-bottomed flask, 50mL of fluoroboric acid was added, and the mixture was magnetically stirred at 50 ℃ for 8 hours and cooled to room temperature. The resulting product was centrifuged, washed several times with deionized water, dried at 60 ℃ and after collection the powder was dispersed to 1mg/mL with ethanol for further use.
Fig. 1 and fig. 2 are transmission electron microscope and contact angle characterization diagrams of fluorine-doped boron nitride prepared in the embodiment of the present invention, respectively. As can be seen from the characterization chart, the fluorine-doped boron nitride prepared in this example is a two-dimensional nanostructure material with few layers, and has a contact angle of 110.41 °, and good hydrophobicity.
Example 2
Preparation of adsorbing material for water pollutants
An isosceles triangle paper piece with the bottom of 5mm and the height of 7mm is immersed in 1mg/mL fluorine-doped boron nitride-absolute ethyl alcohol dispersion liquid, is taken out after being immersed for 1.5 hours, and is naturally dried at room temperature.
Fig. 3 and 4 are scanning electron microscope images of the unmodified paper base and the fluorine-doped boron nitride modified paper base in the embodiment, and it is obvious from the images that the fluorine-doped boron nitride material can be uniformly adsorbed on the paper base.
Example 3
As shown in fig. 5, the paper spray mass spectrometry detection device for detecting water body pollutants comprises: the adsorption material of organic pollutant, mass spectrograph, metal clamp, its one end of metal clamp is connected with external high voltage direct current power supply, and the other end is pressed from both sides the adsorption material of the water pollutant of embodiment 2 preparation makes the pointed end of adsorption material aim at the introduction port of mass spectrograph.
Example 4
A paper spray mass spectrometry detection method of water body pollutants comprises the following steps:
(1) preparing an adsorbing material adsorbing water pollutants: diluting a water sample by 10 times with purified water, and adding a certain amount of bisphenol A and tetrabromobisphenol A. Then, 20. mu.L of the mixed solution (500 pmol each of bisphenol A and tetrabromobisphenol A) was dropped on the fluorine-doped boron nitride-loaded paper base, and dried at 37 ℃.
(2) Mass spectrum detection: clamping a paper substrate adsorbing fluorine-doped boron nitride of water pollutants on a copper metal clamp, and continuously dripping methanol: bisphenol a and tetrabromobisphenol a were eluted from the paper base material with an eluting solvent of 9:1 (containing 1% by volume of aqueous ammonia), and finally the target was ionized by applying a voltage of-3.5 KV by an external power source and subjected to mass spectrometry for detection.
The actual samples are spring water from black tiger spring in the lower area of the city of Jinan and river water from the Xiaoqing river of Jinan, and all the water samples are filtered by a water system filter membrane of 0.22 mu m in order to remove floating impurities.
Fig. 6 and 7 are a comparison of an unmodified paper base (i.e., blank paper) and a paper base modified by fluorine-doped boron nitride (i.e., an adsorbing material of a water pollutant) in a water pollutant detection of a microcleant water sample and a tiger spring water sample, respectively. The specific detection results are shown in Table 1, and the superiority of the method can be obviously seen.
TABLE 1 comparison of blank paper and fluorine-doped boron nitride-modified paper base in detection of different water samples
Although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. 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 (14)
1. The application of the adsorbing material for the water pollutants in the paper spray mass spectrometry detection device is characterized in that the adsorbing material for the water pollutants comprises a paper substrate and fluorine-doped boron nitride attached to the surface of the paper substrate.
2. Use according to claim 1, characterized in that the paper substrate is a paper substrate in paper spray ionization, which is triangular in shape.
3. The preparation method of the adsorbing material for water pollutants as claimed in claim 1, wherein the preparation method of the fluorine-doped boron nitride comprises the following steps:
mixing boron nitride powder with an isopropanol solution, stirring, cooling, performing ultrasonic treatment, standing, performing centrifugal washing, drying to obtain single-layer or few-layer boron nitride, stirring the single-layer or few-layer boron nitride and fluoboric acid, cooling, performing centrifugal washing, and drying to obtain the boron nitride powder;
the ratio of boron nitride powder to isopropyl alcohol is 0.2-2 g: 30-80 mL;
mixing the boron nitride powder with an isopropanol solution, stirring for 18-30h at 40-60 ℃, cooling to room temperature, performing ultrasonic treatment for 15-25h, standing for 0.5-2 days, and washing with acetone;
the ratio of the single-layer or few-layer boron nitride to the fluoroboric acid is 0.2-2 g: 30-80 mL;
mixing the single-layer or few-layer boron nitride and the fluoroboric acid, stirring for 5-10h at 40-60 ℃, cooling to room temperature, and washing with deionized water;
the method for loading the fluorine-doped boron nitride paper substrate comprises the following steps:
soaking the paper sheet in fluorine-doped boron nitride-absolute ethyl alcohol dispersion liquid, taking out and airing;
in the fluorine-doped boron nitride-absolute ethyl alcohol dispersion liquid, the concentration of the fluorine-doped boron nitride is 0.5-3 mg/mL; the soaking time is 0.2-3 h.
4. The method for preparing the adsorbing material for the water pollutants according to claim 3, wherein the adsorbing material for the water pollutants comprises a paper substrate and fluorine-doped boron nitride attached to the surface of the paper substrate.
5. The preparation method of the adsorbing material for water pollutants according to claim 3, wherein the ratio of the boron nitride powder to the isopropanol is 0.5 g: 50 mL.
6. The preparation method of the water body pollutant adsorption material according to claim 3, wherein the boron nitride powder is mixed with an isopropanol solution, stirred at 50 ℃ for 24h, subjected to ultrasonic treatment for 20h, and kept still for 1 day.
7. The preparation method of the adsorbing material for water body pollutants according to claim 3, wherein the ratio of the single-layer or few-layer boron nitride to the fluoroboric acid is 0.5 g: 50 mL.
8. The preparation method of the water body pollutant adsorption material according to claim 3, wherein the single layer or few layers of boron nitride and fluoroboric acid are mixed and stirred for 8 hours at 50 ℃.
9. The preparation method of the water body pollutant adsorption material according to claim 3, wherein the fluorine-doped boron nitride concentration is 1 mg/mL.
10. The preparation method of the water body pollutant adsorption material according to claim 3, wherein the soaking time is 1.5 h.
11. A paper spraying mass spectrum detection device for water body pollutant detection, its characterized in that includes:
an adsorbing material for water body pollutants prepared according to the preparation method of claim 3;
a mass spectrometer;
one end of the metal clamp is connected with an external high-voltage direct-current power supply, and the other end of the metal clamp clamps the paper substrate loaded with the fluorine-doped boron nitride, so that the tip of the adsorbing material is aligned to a sample inlet of a mass spectrometer;
the voltage of the external high-voltage direct-current power supply is minus 3 to minus 4 KV.
12. The paper spray mass spectrometry detection device for water body pollutant detection according to claim 11, wherein the voltage of the external high voltage direct current power supply is-3.5 KV.
13. The paper spray mass spectrometry detection device for water body pollutant detection according to claim 11, wherein the detection is carried out by the device, and the method comprises the following steps:
preparing an adsorbing material of water pollutants;
water sample pretreatment and preparation of an adsorption material with a target object;
clamping the adsorbing material adsorbed with the target object by using a metal clamp, injecting an elution solvent onto the adsorbing material, and applying high-voltage electricity to the adsorbing material to realize desorption of the target object and simultaneously form electrospray of the target object at the tip of the paper substrate;
receiving the electrospray by a mass spectrometer and detecting;
the elution solvent is methanol: water =9:1, volume ratio, and 1% by volume of ammonia water was added to the elution solvent.
14. The paper spray mass spectrometry detection device for detecting water body pollutants according to claim 11, wherein the water sample pretreatment is to filter the water sample through a 0.22 μm water system filter membrane, dilute the water sample by 10 times with purified water, and add bisphenol A and tetrabromobisphenol A;
the preparation of the adsorption material with the target object is specifically that 20 mu L of water sample is dripped on the adsorption material of water pollutants and dried at 37 ℃.
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