Method for determining quinolones in environmental water bodies and fishes

A quinolone, water technology, applied in measurement devices, instruments, scientific instruments, etc., can solve the problem that the ability to improve detection accuracy is difficult to meet people's needs.

A quinolone, water technology, applied in measurement devices, instruments, scientific instruments, etc., can solve the problem that the ability to improve detection accuracy is difficult to meet people's needs.

CN113075313AActive Publication Date: 2021-07-06武汉海关技术中心
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  • Method for determining quinolones in environmental water bodies and fishes
  • Method for determining quinolones in environmental water bodies and fishes
  • Method for determining quinolones in environmental water bodies and fishes

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] 1. Reagent and instrument preparation

[0034] 1.1 Reagents and standard solutions

[0035] In this example, the targeted antibiotics are: enrofloxacin, norfloxacin, ofloxacin, sarafloxacin, difloxacin, nalidixic acid, oxazolinic acid, flumequine, loxacin Mefloxacin and ciprofloxacin, the standard products of these antibiotics were purchased from Dr. Ehrenstorfer Company (Germany). All standards were stored in accordance with the recommendations of the certificate, and the concentration of the standard stock solution was 1.0 mg / mL. The working solution was obtained by diluting the stock solution in methanol to the appropriate concentration. Tris (0.020mol / L, pH=8.0) buffer solution was prepared using tris(hydroxymethyl)aminomethane and hydrochloric acid.

[0036] 1.2 Equipment

[0037] In this example, a liquid chromatography (LC) system (manufactured by Shimadzu Corporation) and an XSelect HSS T3 C18LC column (3.5 μm, 100×3.0mm, Waters, Ireland) to separate and d...

Embodiment 2

[0081] Comparative Experiment

[0082] The applicant synthesized SiO coated with IRMOF-3 2 / Fe 3 o 4 A variety of magnetic materials with similar functional groups were investigated, and the adsorption effect of these materials on 10 quinolone antibiotics was investigated. The results showed that other materials with similar functional groups could not achieve high-efficiency extraction of 10 quinolone antibiotics.

[0083] Here polyaniline modified SiO 2 / Fe 3 o 4 As an example for comparison.

[0084] Specifically, the inventors of the present application synthesized polyaniline-modified SiO 2 / Fe 3 o 4 Magnetic solid phase extraction material and SiO coated with IRMOF-3 2 / Fe 3 o 4 Compare the adsorption performance of 10 kinds of quinolone antibiotics (the synthesis of this material to SiO 2 / Fe 3 o 4 It is basically the same as the material synthesis process in Example 1 of the present invention, except that in the last step, aniline, (NH 4 ) 2 S 2 o 8 A...

Embodiment 3

[0087] Comparative Experiment

[0088] SiO covered by IRMOF-3 synthesized by the applicant 2 / Fe 3 o 4 is IRMOF-3 with SiO 2 / Fe 3 o 4 Composites of which, not just SiO 2 / Fe 3 o 4 The selection of two materials, IRMOF-3 (2-aminoterephthalic acid, zinc acetate dihydrate), is very important, and the synthesis ratio of the two will also have a great impact on the detection effect.

[0089] The inventors of the present application have carried out a large number of experiments, investigated the adsorption effect of these materials to 10 kinds of quinolone antibiotics, and found that only the proportioning relationship near the ratio shown in Example 1 has an excellent detection effect, and once it deviates from a certain degree, Then the detection effect is significantly reduced.

[0090] Two sets of examples are given below

[0091] Take 3.0g of SiO 2 / Fe 3 o 4 Disperse in 40mLN,N-dimethylformamide. Then 0.72 g of 2-aminoterephthalic acid was added and stirred for ...

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Abstract

The invention discloses an extraction material for quinolones in environmental water bodies and fishes and a corresponding detection method. The detection method comprises the following steps of: preparing magnetic Fe3O4 nanoparticles by a solvothermal reaction method; dispersing the magnetic Fe3O4 nanoparticles in a mixture of isopropanol, deionized water and concentrated ammoniacal liquor, and then adding tetraethoxysilane to prepare SiO2 / Fe3O4; dispersing the SiO2 / Fe3O4 in DMF(Dimethyl Formamide), and adding 2-aminoterephthalic acid; dissolving zinc acetate dihydrate in DMF , and dropwise adding the obtained solution into the solution obtained in the previous step, so as to obtain IRMOF-3 coated SiO2 / Fe3O4; adjusting a sample solution to a preset pH value by using diluted acetic acid and ammonium hydroxide, and adding the IRMOF-3 coated SiO2 / Fe3O4 for extraction; separating out a magnetic material by using a strong magnet, and eluting by using a solution; and analyzing the obtained product by using an LC-MS / MS (liquid chromatography-mass spectrometry / mass spectrometry) method. According to the method, the detection limit can be reduced by 3 orders of magnitude, and ciprofloxacin which cannot be detected by the Ministry of Agriculture 783 announcement 2-2006 can be detected by the method.

Description

technical field [0001] The invention relates to the field of food safety detection, in particular to a method for measuring quinolones in environmental water and fish with high precision. Background technique [0002] Quinolones have the advantages of broad antibacterial spectrum, good oral absorption, and low cost. They are an important and successful class of synthetic antibiotics and are widely used in humans, animal husbandry, and aquaculture. They act on bacterial DNA, inhibit topoisomerase, and have a strong and rapid antibacterial effect. At present, quinolones are also widely used in the treatment of various diseases, and their usage is increasing year by year. As a result, quinolones are excreted into the natural environment, contributing to antimicrobial resistance, a growing global public health threat. According to reports, quinolones are found in hospital wastewater, sewage treatment plants, rivers and even drinking water, not to mention meat and fish. Theref...

Claims

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Application Information

Patent Timeline
06 Jul 2021
Publication
CN113075313A
IPC
G01N30/02; G01N30/06
CPC
G01N30/02; G01N30/06; G01N2030/062
Inventors
王晗; 赵晓亚