CN115290778B - Analysis and identification method for trace glucocorticoid in environmental water body - Google Patents
Analysis and identification method for trace glucocorticoid in environmental water body Download PDFInfo
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Abstract
The invention discloses an analysis and identification method of trace glucocorticoid in environmental water, which comprises the following steps: filling a covalent organic framework material based on three-dimensional hydroxylation into a solid-phase extraction tube to prepare a solid-phase extraction column; sequentially introducing methanol and water to activate the solid phase extraction column; introducing the water sample into the activated solid phase extraction column for adsorption; and introducing desorption liquid into the solid-phase extraction column for desorption, and then carrying out nitrogen blowing, re-dissolution and membrane passing on the desorption liquid, and detecting by liquid chromatography-tandem mass spectrometry. When the liquid chromatography detection method is adopted to detect the extracted substances, the detection method has wide linear range, low detection limit and high accuracy.
Description
Technical Field
The invention belongs to the technical field of environmental analysis, and particularly relates to an analysis and identification method of trace glucocorticoids in environmental water, wherein covalent organic framework materials prepared by the method can be used for simultaneously detecting six glucocorticoids of Prednisone (PNS), prednisolone (PNL), hydrocortisone (HC), betamethasone (BM), fluocinolone (FM) and triamcinolone acetonide (TCA) in environmental water.
Background
The statements herein merely provide background information related to the present disclosure and may not necessarily constitute prior art.
The glucocorticoid has anti-inflammatory and antiallergic pharmacological actions, and is widely used for treating inflammatory, allergic and autoimmune diseases of livestock, poultry and human. In addition to therapeutic effects, glucocorticoids can also increase feed conversion rates and are used as growth promoters in mariculture. The widespread use of glucocorticoids has led to the entry of glucocorticoids into environmental and agricultural water supply systems, and studies have shown that residual glucocorticoids in aqueous environments can have adverse effects on humans and aquatic organisms even at very low concentrations. In order to ensure the safety of water quality, it is important to establish a high-sensitivity analysis method of glucocorticoids in environmental water.
The solid phase extraction is widely applied due to the advantages of high recovery rate, high concentration multiple, low organic solvent consumption and the like, and the traditional solid phase extraction columns have the defects of low adsorption efficiency, low recycling rate, high cost and the like due to the complex matrix of an environmental water sample and low residual glucocorticoid concentration.
Disclosure of Invention
Aiming at the defects existing in the prior art, the invention aims to provide an analysis and identification method for trace glucocorticoid in environmental water.
In order to achieve the above object, the present invention is realized by the following technical scheme:
an analysis and identification method for trace glucocorticoids in environmental water body comprises the following steps:
Filling the three-dimensional hydroxylation covalent organic framework material into a solid phase extraction column tube to prepare a solid phase extraction column;
sequentially activating the self-made solid phase extraction column by using methanol and water;
under the drive of a water pump, a certain volume of water sample flows through a solid phase extraction column, proper desorption liquid is selected for desorption, and the water sample is detected by a liquid chromatography tandem mass spectrometry after nitrogen blowing, re-dissolution and film passing;
The preparation method of the three-dimensional hydroxylation covalent organic framework material comprises the following steps: the catalyst is prepared by solvothermal reaction by taking tetra (4-aminophenyl) methane (TAM) and 2, 5-Dihydroxyterephthalaldehyde (DHTA) as monomers, taking mixed liquid of 1, 2-dichlorobenzene and N, N-dimethylacetamide as a solvent and taking acetic acid as a catalyst.
The beneficial effects achieved by one or more embodiments of the present invention described above are as follows:
The solid phase extraction column is prepared by taking the three-dimensional hydroxylation covalent organic framework material as a filler, and the prepared solid phase extraction column has the advantages of high separation and enrichment efficiency and reusability. The liquid chromatography tandem mass spectrometry is adopted to detect the glucocorticoid in the environmental water body, and the detection method has the advantages of wide linear range, low detection limit and high accuracy.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the invention.
FIG. 1 is a scanning electron microscope image of a three-dimensional hydroxylated covalent organic framework material according to example 1 of the present invention;
FIG. 2 is an infrared spectrum of a three-dimensional hydroxylated covalent organic framework material according to example 1 of the present invention;
FIG. 3 is an N 2 adsorption-desorption curve for a three-dimensional hydroxylated covalent organic framework material according to example 1 of the present invention;
FIG. 4 is a graph showing the effect of pH, ionic strength, type of desorbent, volume of desorbent, flow rate and volume of sample on the extraction of a self-made solid phase extraction column according to example 2 of the present invention.
Detailed Description
It should be noted that the following detailed description is illustrative and is intended to provide further explanation of the invention. 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.
An analysis and identification method for trace glucocorticoids in environmental water body comprises the following steps:
Filling the three-dimensional hydroxylation covalent organic framework material into a solid phase extraction column tube to prepare a solid phase extraction column;
sequentially activating the self-made solid phase extraction column by using methanol and water;
under the drive of a water pump, a certain volume of water sample flows through a solid phase extraction column, proper desorption liquid is selected for desorption, and the water sample is detected by a liquid chromatography tandem mass spectrometry after nitrogen blowing, re-dissolution and film passing;
The preparation method of the three-dimensional hydroxylation covalent organic framework material comprises the following steps: the catalyst is prepared by solvothermal reaction by taking tetra (4-aminophenyl) methane (TAM) and 2, 5-Dihydroxyterephthalaldehyde (DHTA) as monomers, taking mixed liquid of 1, 2-dichlorobenzene and N, N-dimethylacetamide as a solvent and taking acetic acid as a catalyst.
In some embodiments, the water sample is filtered through an aqueous filter to remove impurities therefrom.
In some embodiments, the desorbing liquid is methanol.
In some embodiments, the multiple solution is 0.5mL of aqueous methanol at a volume ratio of 1:1.
In some embodiments, the chromatographic column used for liquid chromatography is a Thermo Fisher C18 column (100 mm. Times.2.1 mm,2.6 μm).
Preferably, the mobile phase is methanol and 0.1% formic acid in water.
Preferably, the flow rate is 0.3mL/min.
Preferably, the gradient elution procedure is 0-4.0min,50-80% methanol, 4.0-4.1min,80-50% methanol, 4.1-7.0min,50% methanol.
In some embodiments, mass spectrometry conditions: electrospray ion source, positive ionization, multiple reaction monitoring mode.
The invention will now be described in further detail with reference to the following specific examples, which should be construed as illustrative rather than limiting.
Example 1
Preparation and characterization of three-dimensional hydroxylated covalent organic framework materials:
TAM (0.315 mmol) and DHTA (0.555 mmol) are weighed into a 38mL pressure-resistant bottle, 0.87mL of 1, 2-dichlorobenzene and 5.13mL of N, N-dimethylacetamide are added as reaction solvents, ultrasound is carried out for 5 minutes, 1.2mL of 6mol/L acetic acid is added, the reaction bottle is placed into a liquid nitrogen bath for freezing, and after three freezing-degassing-thawing cycles, the reaction is carried out for 72 hours in an oil bath at 120 ℃. Centrifuging, washing with methanol, and drying at 60deg.C to obtain yellow brown powder.
And carrying out morphology analysis on the three-dimensional hydroxylation covalent organic framework material by a scanning electron microscope, wherein the three-dimensional hydroxylation covalent organic framework material has a rhombic cubic structure as shown in figure 1. The infrared spectrum of fig. 2 shows that the N-H stretching vibration peak (3386 and 3317cm -1) in TAM and the c=o stretching vibration peak (1666 cm -1) in DHTA are substantially disappeared, and a stretching vibration characteristic peak attributed to c=n appears at the wave number 1607cm -1, indicating that the schiff base reaction occurs between TAM and DHTA, and an imine bond is formed. The N 2 adsorption-desorption curve shown in FIG. 3 shows that the specific surface area of the three-dimensional hydroxylated covalent organic framework material is 358.9m 2/g.
Example 2
Solid phase extraction flow and single factor method optimize solid phase extraction parameters:
50.0mg of three-dimensional hydroxylation covalent organic framework material is weighed and filled into an empty 3mL solid phase extraction column tube, and a solid phase extraction column is prepared. Activating a self-made solid-phase extraction column by using 6mL of methanol and 6mL of ultrapure water in sequence, adding a glucocorticoid standard solution with a certain concentration into a water sample, and desorbing the methanol after the sample solution flows through the self-made solid-phase extraction column. The desorbed solution was nitrogen-purged to dryness in a water bath with 0.5mL volume ratio of 1:1, and passing through a 0.22 μm organic filter membrane. And (4) examining the influence of the pH, the ionic strength, the desorption liquid type, the desorption liquid volume, the loading flow rate and the loading volume of the sample on the separation and enrichment effect of the self-made solid phase extraction column, wherein the related results are shown in figure 4.
Example 3
And (3) verifying methodology parameters:
Preparing a series of glucocorticoid standard solutions with concentration gradients, adding standard solutions with different concentrations into a water sample, preprocessing the sample according to the optimal solid phase extraction parameters obtained in the example 2, and detecting the complex solution by a liquid chromatograph tandem mass spectrometer. And drawing a standard curve, and calculating a detection Limit (LOD) and a quantification Limit (LOQ) of the method according to the concentration when the signal to noise ratio (S/N) is 3 and 10, wherein the related parameters are shown in table 1.
The detection conditions of the liquid chromatography tandem mass spectrometry are as follows: liquid chromatography conditions: the column was a Thermo Fisher C18 column (100 mm. Times.2.1 mm,2.6 μm); the mobile phase is methanol and 0.1% formic acid water solution; the flow rate is 0.3mL/min; gradient elution procedure was 0-4.0min,50-80% methanol, 4.0-4.1min,80-50% methanol, 4.1-7.0min,50% methanol; the sample volume was 10. Mu.L. Mass spectrometry conditions: the ionization mode is electrospray ionization (ESI) with positive ion mode, the scanning mode is multi-reaction monitoring mode, and the ion source temperature is 500 ℃. Other parameters are shown in table 2.
TABLE 1 established parameters of glucocorticoid detection method
TABLE 2 Mass Spectrometry detection conditions for glucocorticoids
Example 4
Glucocorticoid detection assay in actual samples:
in order to verify the applicability of the glucocorticoid detection method provided by the invention, the glucocorticoid in three environmental water samples (tap water, snow water and spring water) is detected. The water sample was first filtered through a 0.22 μm filter to remove impurities therein, and no glucocorticoid was detected in all three water samples. The labeling recovery experiments (labeling concentration is 5ng/L,25ng/L and 75 ng/L) are carried out on three actual water samples, the labeling recovery rate in tap water is 78.1-91.8%, the labeling recovery rate in snow water is 80.2-104.0%, and the labeling recovery rate in spring water is 79.0-95.5%, so that the detection method of the glucocorticoid provided by the invention has good accuracy and environmental water sample analysis applicability.
The above description is only of the preferred embodiments of the present invention and is not intended to limit the present invention, but various modifications and variations can be made to the present invention by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A method for analyzing and identifying trace glucocorticoids in environmental water is characterized by comprising the following steps: the method comprises the following steps:
Preparing a three-dimensional hydroxylation covalent organic framework material: weighing 0.315 mmol of tetra (4-aminophenyl) methane and 0.555 mmol of 2, 5-dihydroxyterephthalaldehyde in a pressure-resistant bottle of 38 mL, adding 0.87 mL of 1, 2-dichlorobenzene and 5.13 mL of N, N-dimethylacetamide as reaction solvents, carrying out ultrasonic treatment for 5 minutes, adding 1.2 mL of 6 mol/L of acetic acid, putting the reaction bottle into a liquid nitrogen bath for freezing, carrying out three freezing-degassing-thawing cycles, carrying out oil bath reaction at 120 ℃ for 72 h, centrifuging, washing with methanol, and drying at 60 ℃ to obtain yellowish brown powder;
Filling the three-dimensional hydroxylation covalent organic framework material into a solid phase extraction column tube to prepare a solid phase extraction column;
sequentially activating the self-made solid phase extraction column by using methanol and water;
And (3) enabling a water sample with a certain volume to flow through the solid phase extraction column under the driving of the water pump, selecting proper desorption liquid for desorption, blowing nitrogen, re-dissolving, passing through a membrane, and detecting by a liquid chromatography tandem mass spectrometry.
2. The method for analyzing and identifying trace glucocorticoids in an environmental water body according to claim 1, wherein the method comprises the following steps: the water sample is filtered by a water system filter membrane to remove impurities in the water sample.
3. The method for analyzing and identifying trace glucocorticoids in an environmental water body according to claim 1, wherein the method comprises the following steps: the desorption liquid is methanol.
4. The method for analyzing and identifying trace glucocorticoids in an environmental water body according to claim 1, wherein the method comprises the following steps: the redissolution adopted by the redissolution is methanol aqueous solution.
5. The method for analyzing and identifying trace amounts of glucocorticoids in an environmental body of water according to claim 4, wherein: in the complex solution, the volume ratio of methanol to water is 0.8-1.2:1.
6. The method for analyzing and identifying trace glucocorticoids in an environmental water body according to claim 1, wherein the method comprises the following steps: the chromatographic column used in the liquid chromatography is a Thermo Fisher C18 column, 100 mm ×2.1 mm, 2.6 μm.
7. The method for analyzing and identifying trace glucocorticoids in an environmental water body according to claim 1, wherein the method comprises the following steps: the mobile phase was methanol and 0.1% formic acid in water.
8. The method for analyzing and identifying trace glucocorticoids in an environmental water body according to claim 1, wherein the method comprises the following steps: the flow rate was 0.3 mL/min.
9. The method for analyzing and identifying trace glucocorticoids in an environmental water body according to claim 1, wherein the method comprises the following steps: gradient elution procedure was 0-4.0 min,50-80% methanol, 4.0-4.1 min,80-50% methanol, 4.1-7.0 min,50% methanol.
10. The method for analyzing and identifying trace glucocorticoids in an environmental water body according to claim 1, wherein the method comprises the following steps: mass spectrometry conditions: electrospray ion source, positive ionization, multiple reaction monitoring mode.
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