CN110511339B - Solid-phase microextraction adsorbent for pyrethroid pesticide detection and preparation method and application thereof - Google Patents
Solid-phase microextraction adsorbent for pyrethroid pesticide detection and preparation method and application thereof Download PDFInfo
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Abstract
The invention relates to a solid phase microextraction adsorbent for pyrethroid pesticide detection and a preparation method and application thereof. A covalent organic polymer has a repeating unit shown in formula I,
the covalent organic polymer shown in the formula I is used for preparing the solid phase microextraction probe, so that the sensitivity for detecting the pyrethroid pesticides in fruits, vegetables, tea and Chinese medicinal materials is high, and the limit of quantitation can reach 2 ng/g.
Description
Technical Field
The invention belongs to the technical field of pesticide detection, and particularly relates to a solid-phase microextraction adsorbent for pyrethroid pesticide detection, and a preparation method and application thereof.
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.
Pyrethroid is a broad-spectrum pesticide capable of preventing and controlling various pests, and because pyrethroid insecticides have the characteristics of wide insecticidal spectrum, good quick action, low toxicity and the like, the pyrethroid insecticides play an important role in the prevention and control of pests in the early stage. Since the use of high-toxicity organophosphorus pesticides is prohibited, pyrethroid insecticides have wider use space, but also bring problems of environmental pollution, food and drug safety and the like, and are listed as important detection objects of agricultural products and pesticide residues of traditional Chinese medicines. Therefore, in order to meet the requirements of food and drug safety detection, a detection method which has high sensitivity and low quantitative limit and can simultaneously detect the residual quantity of various pyrethroids is urgently needed to be established.
The countries set limit standards for pyrethroid pesticides, and have specific limitations for pyrethroid pesticides. The inventor finds that the existing detection method cannot realize the detection of pyrethroid pesticide with high sensitivity and low limit of quantification.
At present, C18 material is mostly adopted as the selection of the pyrethroid microextraction adsorbent. The inventors have found that the C18 solid phase extraction adsorbent has the problem of low quantitation limit.
Disclosure of Invention
In view of the problems in the prior art, an object of the present invention is to provide a solid phase microextraction adsorbent for pyrethroid pesticide detection, and a preparation method and applications thereof.
In order to solve the technical problems, the technical scheme of the invention is as follows:
in a first aspect, a covalent organic polymer having a repeat unit according to formula I,
the invention provides a method for adsorbing pyrethroid pesticide by using alkali as a catalyst, 1, 3, 5-mesitylene-trimethyl aldehyde and p-1, 3, 5-triacetylbenzene as reaction functional monomers, and researches show that the covalent organic polymer microspheres have good adsorption effect on the pyrethroid pesticide. The covalent organic polymer microspheres can specifically adsorb pyrethroid pesticides, and the characteristic can be applied to detection of residual pesticides in fruits, vegetables, tea and traditional Chinese medicinal materials.
The adsorption principle of the covalent organic polymer on the pyrethroid pesticide is intermolecular hydrogen bond, pi-pi acting force and the like.
In a second aspect, a method for preparing a covalent organic polymer comprises performing a condensation reaction between 1, 3, 5-mesitylene-triformal and p-1, 3, 5-triacetylbenzene as reaction functional monomers in a solvent with a base as a catalyst to obtain the covalent organic polymer.
The covalent organic polymer prepared by the method is in a cluster state.
The structural formula of the 1, 3, 5-mesitylene is shown in the specification
The structural formula of the 1, 3, 5-triacetylbenzene is shown in the specification
In some embodiments, the catalyst is one of sodium oxide, potassium hydroxide, sodium bicarbonate. In some embodiments, the molar ratio of 1, 3, 5-mesitylene-trioxaldehyde, 1, 3, 5-triacetylbenzene, catalyst is 1: 1: (0.1-0.3); preferably 1: 1: (0.1-0.2). In some embodiments, the solvent is one of toluene, o-xylene, mesitylene. In some embodiments, the mass ratio of the reaction solvent to the functional monomer 1, 3, 5-mesitylene-triformal is (10-15): 1; preferably (10-13): 1. in some embodiments, the reaction temperature is 100 ℃ to 120 ℃ and the reaction time is 16 to 24 hours.
In a third aspect, the use of the covalent organic polymer as a solid phase microextraction adsorbent.
In a fourth aspect, the solid phase microextraction adsorbent is used for preparing a solid phase microextraction probe.
In a fifth aspect, a solid phase microextraction probe comprises a carrier, the solid phase microextraction adsorbent and a sealant, wherein the amount of the solid phase microextraction adsorbent loaded on each square centimeter of the carrier is 1-5 mg.
In some embodiments, the sealant is an epoxy resin sealant or a polyurethane sealant, and the mass ratio of the sealant to the solid phase microextraction adsorbent is (0.5-1): 9. In some embodiments, the carrier is a stainless steel wire.
A preparation method of a solid phase micro-extraction probe comprises the steps of uniformly coating a sealant on the surface of a stainless steel needle wire, and adhering covalent organic polymer microspheres to the stainless steel needle wire through the sealant to obtain the solid phase micro-extraction probe.
In some embodiments, the reaction process is ambient.
In a sixth aspect, the solid phase microextraction probe is used for detecting pyrethroid pesticides in products.
In some embodiments, the product comprises fruits and vegetables, tea leaves and traditional Chinese medicines. Preferably, the fruits and vegetables include spinach, Chinese cabbage, rape, leek, tomato, apple, grape, orange, cabbage, eggplant and hawthorn; the Chinese medicinal materials include Mel, flos Lonicerae, flos Rosae Rugosae, fructus Lycii, flos Chrysanthemi, and herba Taraxaci; the tea leaf comprises green tea. In some embodiments, the pyrethroid pesticide includes tetramethrin, bifenthrin, fenpropathrin, phenothrin, cyhalothrin, cyfluthrin, permethrin, cyfluthrin, cypermethrin, cyfluthrin, tralomethrin, deltamethrin.
The method for detecting the pyrethroid pesticide in the product by using the solid phase microextraction probe comprises the specific steps of extracting the product to be detected by using an organic solvent, adsorbing an extracting solution by using the solid phase microextraction probe, taking out the solid phase microextraction probe, carrying out gas chromatography-tandem mass spectrometry detection, and carrying out thermal desorption on the solid phase microextraction probe in the gas chromatography detection process.
In some embodiments, the organic solvent is one of acetonitrile, methanol, ethanol. In some embodiments, the method of extracting the product to be detected is: mixing the product to be detected with the organic solvent, and then swirling for 0.4-0.6h, wherein the amount of the organic solvent in 1g of the product to be detected is 9-11 mL. In some embodiments, the temperature of thermal desorption is 280-300 ℃.
The pyrethroid pesticide of the product to be detected is fully dissolved in the extracting solution by the organic solvent, and the organic solvent with larger polarity is selected for extraction.
The invention has the beneficial effects that:
the solid-phase microextraction adsorbent disclosed by the invention can be suitable for a detection standard (GB2763-2014), can be used for detecting residual pyrethroid pesticides in various foods or Chinese medicinal materials, and can be used for identifying the foods or Chinese medicinal materials with residual quantities not meeting the standard.
In the prior art, a detection technology for detecting pyrethroid pesticides in fruits, vegetables, tea and traditional Chinese medicinal materials by utilizing solid-phase microextraction is blank, a pre-treated solid-phase microextraction agent is generally C18, and the limit of quantitation can reach 50 ng/g. The invention provides a covalent organic polymer as a solid phase microextraction adsorbent, provides a new idea for the development of solid phase microextraction materials, and the material provided by the invention is used as a solid (phase microextraction agent, the limit of quantitation can reach 2ng/g, and the technical effect is far better than that of the prior art.
The solid phase microextraction probe is combined with gas chromatography-tandem mass spectrometry, the detection method is simple and convenient, the detection method is GB/T5009.146-2008, and the detection result has accuracy.
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 embodiments of the invention and together with the description, serve to explain the invention and not to limit the invention.
FIG. 1 is an electron micrograph of a covalent organic polymer prepared according to example 1;
FIG. 2 is an electron microscope scan of the solid phase microextraction probe prepared in example 4;
FIG. 3 is an infrared spectrum of the covalent organic polymer prepared in example 1.
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 example embodiments according to the present application. 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.
As introduced in the background art, the solid phase microextraction of pyrethroid pesticides has been studied less in the prior art, and in order to solve the above technical problems, the application proposes a covalent organic polymer which can be used as a solid phase microextraction adsorbent for pyrethroid pesticides.
The invention will be further illustrated by the following examples
Example 1
162mg of 1, 3, 5-mesitylene-triformal, 204mg of 1, 3, 5-triacetylbenzene and 4mg of sodium hydroxide were weighed and added to 1.62g of a reaction solvent, which was toluene.
Adding the prepared reactants into a test tube, uniformly mixing, sealing, and carrying out oil bath reaction at a constant temperature of 100 ℃ for 14 hours to obtain a polymer;
the polymer prepared above was washed with an ethanol solution having an acetic acid volume fraction of 10%, and dried under vacuum at 60 ℃ to obtain 302mg of a covalent organic polymer.
FIG. 1 is an electron microscope scanning image of the covalent organic polymer prepared, and it can be seen from FIG. 1 that the morphology is cluster flower-like. FIG. 3 is an infrared characterization spectrum of a covalent organic polymer.
Example 2
162mg of 1, 3, 5-mesitylene-trioxaldehyde, 204mg of 1, 3, 5-triacetylbenzene and 10mg of potassium hydroxide were weighed and put into 2.00g of a reaction solvent, which was mesitylene.
Adding the prepared reactants into a test tube, uniformly mixing, sealing, and carrying out oil bath reaction at a constant temperature of 110 ℃ for 20 hours to obtain a polymer;
the polymer prepared above was washed with an ethanol solution having an acetic acid volume fraction of 10%, and vacuum dried at 60 ℃ to obtain 290mg of a covalent organic polymer.
Example 3
162mg of 1, 3, 5-mesitylene-trioxaldehyde, 204mg of 1, 3, 5-triacetylbenzene and 12mg of potassium hydroxide were weighed and put into 1.92g of a reaction solvent, which was o-xylene.
Adding the prepared reactants into a test tube, uniformly mixing, sealing, and reacting in a constant-temperature oil bath at 100 ℃ for 18 hours to obtain a polymer;
the polymer prepared above was washed with an ethanol solution having an acetic acid volume fraction of 10%, and dried under vacuum at 60 ℃ to obtain 312mg of a covalent organic polymer.
Example 4
The sealant was uniformly coated on the surface of the stainless steel needle wire with a length of 2 cm, and the covalent organic polymer prepared in example 1 was adhered to the stainless steel needle wire by the sealant to obtain a solid phase microextraction probe.
FIG. 2 is an electron microscope scanning image of the solid phase microextraction probe of example 4, and it can be known from FIG. 2 that the covalent organic polymer is uniformly loaded on the outer surface of the stainless steel needle wire.
Example 5
For the detection of the traditional Chinese medicinal materials, the honeysuckle is taken as an example in this embodiment to explain the detection effect.
Weighing 1g of honeysuckle, crushing, adding 9.5mL of acetonitrile, performing vortex extraction for 0.4 hour, filtering, and collecting filtrate. Adding the solid phase microextraction probe prepared in the example 4 into the honeysuckle extract, carrying out solid phase microextraction adsorption on the honeysuckle extract, and carrying out gas chromatography-tandem mass spectrometry detection on the solid phase microextraction probe adsorbing pyrethroid, wherein the detection method is GB/T5009.146-2008, and the gas chromatography thermal desorption temperature is 280 ℃.
The result shows that the tetramethrin content in the honeysuckle flower obtained by the method is 2ng/g, and the bifenthrin content is 6.9 ng/g.
Example 6
The covalent organic polymer prepared in example 2 was coated on a stainless steel wire to prepare a solid phase microextraction probe, which was prepared in the same manner as in example 4.
Example 7
For the detection of vegetable samples, the detection effect will be described in this embodiment by taking leeks as an example.
Weighing 1g of Chinese cabbage, pulverizing, adding 10mL of acetonitrile, performing vortex extraction for 0.5 hour, filtering, and collecting filtrate. Adding the solid phase microextraction probe prepared in example 6 into leek extract, performing solid phase microextraction adsorption on the leek extract, and performing gas chromatography-tandem mass spectrometry detection on the solid phase microextraction probe with adsorbed pyrethroid by GB/T5009.146-2008, wherein the gas chromatography thermal desorption temperature is 290 deg.C
The result shows that the content of cyfluthrin in the honeysuckle flower obtained by the method is 2ng/g, the content of cypermethrin is 4.2ng/g and the content of the cyfluthrin is 2.2 ng/g.
Example 8
The covalent organic polymer prepared in example 3 was coated on a stainless steel wire to prepare a solid phase microextraction probe, which was prepared in the same manner as in example 4.
Example 9
For the detection of fruit samples, the present embodiment takes apple as an example to illustrate the detection effect.
Weighing 1g of apple, crushing, adding 10.5mL of acetonitrile, performing vortex extraction for 0.6 hour, filtering, and collecting filtrate. Adding the solid phase microextraction probe prepared in example 8 into apple extract, performing solid phase microextraction adsorption on the apple extract, and performing gas chromatography-tandem mass spectrometry detection on the solid phase microextraction probe with adsorbed pyrethroid by GB/T5009.146-2008, wherein the gas chromatography thermal desorption temperature is 285 deg.C
The result shows that the content of cyhalothrin, the content of pentofenfluthrin and the content of prallethrin in the honeysuckle flower obtained by the method are respectively 2ng/g, 7.2ng/g and 5.2 ng/g.
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 (24)
1. A covalent organic polymer characterized by: the repeating unit is shown as a formula I,
2. a method of preparing a covalent organic polymer, comprising: the method comprises the steps of taking 1, 3, 5-mesitylene triformal and p-1, 3, 5-triacetylbenzene as reaction functional monomers, taking alkali as a catalyst, and carrying out condensation reaction in a solvent to obtain the covalent organic polymer.
3. The method of claim 2, wherein the catalyst is one of sodium oxide, potassium hydroxide, and sodium bicarbonate.
4. The method of claim 2, wherein the molar ratio of 1, 3, 5-mesitylene-trioxaldehyde, 1, 3, 5-triacetylbenzene, and catalyst is 1: 2: (0.1-0.3).
5. The method of claim 4, wherein the molar ratio of 1, 3, 5-mesitylene-trioxaldehyde, 1, 3, 5-triacetylbenzene, and catalyst is 1: 2: (0.1-0.2).
6. The method of claim 2, wherein the solvent is one of toluene, o-xylene, and mesitylene.
7. The method for preparing the covalent organic polymer according to claim 2, wherein the mass ratio of the solvent to the functional monomer 1, 3, 5-mesitylene-trioxal is (10-15): 1.
8. the method for preparing the covalent organic polymer according to claim 7, wherein the mass ratio of the solvent to the functional monomer 1, 3, 5-mesitylene-trioxal is (10-13): 1.
9. the method as claimed in claim 2, wherein the condensation reaction is carried out at a temperature of 100 ℃ and 120 ℃ for a period of 16-24 hours.
10. Use of the covalent organic polymer of claim 1 as a solid phase microextraction adsorbent.
11. Use of the covalent organic polymer of claim 1 in the preparation of a solid phase microextraction probe.
12. A solid phase micro-extraction probe is characterized in that: comprises a carrier, a solid phase microextraction adsorbent and a sealant, wherein the amount of the solid phase microextraction adsorbent loaded on each square centimeter of the carrier is 1-5 mg;
the solid phase microextraction adsorbent is a covalent organic polymer as described in claim 1 or prepared by the preparation method as described in any one of claims 2-9.
13. The solid phase microextraction probe according to claim 12, wherein said sealant is epoxy resin glue or polyurethane sealant, and the mass ratio of sealant to solid phase microextraction adsorbent is (0.5-1): 9.
14. The solid phase microextraction probe according to claim 12, wherein said carrier is stainless steel wire.
15. The method for preparing a solid phase microextraction probe according to any one of claims 12 to 14, characterized in that: and uniformly coating the sealant on the surface of the stainless steel needle wire, and adhering the covalent organic polymer microspheres to the stainless steel needle wire through the sealant to obtain the solid-phase microextraction probe.
16. The method of claim 15, wherein the reaction process is at room temperature.
17. Use of a solid phase microextraction probe according to any of claims 12 to 14 for detecting pyrethroid insecticides in a product.
18. Use of a solid phase microextraction probe according to claim 17 for the detection of pyrethroid insecticides in products characterized by: the product comprises fruits and vegetables, tea and Chinese medicinal materials.
19. The use of a solid phase microextraction probe according to claim 18 for detecting pyrethroid insecticides in products, wherein said fruits and vegetables include spinach, cabbage, canola, leek, tomato, apple, grape, citrus, cabbage, eggplant, hawthorn; the Chinese medicinal materials include Mel, flos Lonicerae, flos Rosae Rugosae, fructus Lycii, flos Chrysanthemi, and herba Taraxaci; the tea leaf comprises green tea.
20. Use of a solid phase microextraction probe according to claim 17 for detecting a pyrethroid pesticide in a product, wherein the pyrethroid pesticide comprises tetramethrin, bifenthrin, fenpropathrin, phenothrin, cyhalothrin, cyfluthrin, permethrin, cyfluthrin, cypermethrin, cyfluthrin, tralomethrin, deltamethrin.
21. A method for detecting pyrethroid agricultural chemicals in a product by using the solid phase micro extraction probe as claimed in any one of claims 12 to 14, characterized by: the method comprises the following specific steps of extracting a product to be detected by using an organic solvent, adsorbing an extracting solution by using a solid phase microextraction probe, taking out the solid phase microextraction probe, detecting by using a gas chromatography-tandem mass spectrometry, and carrying out thermal desorption on the solid phase microextraction probe in the gas chromatography detection process.
22. The method for detecting pyrethroid pesticide in the product by the solid phase micro extraction probe according to claim 21, characterized in that the organic solvent is one of acetonitrile, methanol and ethanol.
23. The method for detecting pyrethroid pesticide in product by solid phase microextraction probe according to claim 21, characterized in that the method for extracting the product to be detected is as follows: mixing the product to be detected with the organic solvent, and then swirling for 0.4-0.6h, wherein the amount of the organic solvent in 1g of the product to be detected is 9-11 mL.
24. The method of detecting a pyrethroid pesticide in a product according to claim 21, characterized by: the temperature of thermal desorption is 280-300 ℃.
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