Method for determining desoxyquinocetone and 3-methylquinoxaline-2-carboxylic acid in seawater

A technology for removing quinocetone and methyl quinoxaline is applied in the field of pollutant detection in seawater, and can solve the problems of low detection sensitivity and the like

Pending Publication Date: 2021-06-08
山东省海洋资源与环境研究院
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The current relevant standards for MQCA detection, "Announcement No. 781 of the Ministry of Agriculture-3-2006 Determination of 3-methylquinoxaline-2-carboxylic acid and quinoxaline-2-carboxylic acid residues in food of animal origin by high performance liquid chromatography Chromatography", "Ministry of Agriculture Announcement No. 1077-5-2008 Determination of Residues of Olaquindox Metabolites in Aquatic Products High Performance Liquid Chromatography" all use high performance liquid chromatography to determine MQCA residues in samples, but the detection sensitivity is low

Method used

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  • Method for determining desoxyquinocetone and 3-methylquinoxaline-2-carboxylic acid in seawater
  • Method for determining desoxyquinocetone and 3-methylquinoxaline-2-carboxylic acid in seawater
  • Method for determining desoxyquinocetone and 3-methylquinoxaline-2-carboxylic acid in seawater

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0112] Acquisition of the standard curve:

[0113] The desdioxoquinone was dissolved in acetonitrile to prepare a desdioxoquinone stock solution with a concentration of 100 μg / mL;

[0114] 3-methylquinoxaline-2-carboxylic acid was dissolved in acetonitrile to prepare a 3-methylquinoxaline-2-carboxylic acid stock solution with a concentration of 100 μg / mL;

[0115] Take 1.0mL dedioxoquinone stock solution and 1.0mL 3-methylquinoxaline-2-carboxylic acid stock solution in a 100mL volumetric flask, and dilute to volume with acetonitrile to obtain dedioxoquinone and 3-methylquinoxaline Phenyl-2-carboxylic acid mixed standard stock solution 1.0 μg / mL;

[0116] Take 10 μL, 20 μL, 50 μL, 100 μL, and 200 μL of the concentration of 1.0 μg / mL dedioxoquinone and 3-methylquinoxaline-2-carboxylic acid mixed standard stock solutions, respectively, and dilute 100, 50, 20, 10 and 5 Times, to obtain desdioxoquinolone and 3-methylquinoxaline-2-carboxylic acid are respectively 10ng / mL, 20ng / mL,...

Embodiment 2

[0122] Limits of detection and limits of quantitation

[0123] According to the 3 times signal-to-noise ratio of dedioxoquinone and 3-methylquinoxaline-2-carboxylic acid, the detection limit of the concentration on the machine is determined, and then converted into dedioxoquinone and 3-methylquinoxaline in seawater The detection limit concentration of phenoline-2-carboxylic acid. The results were: the detection limit of dedioxoquinone was 5 ng / L, and the detection limit of 3-methylquinoxaline-2-carboxylic acid was 5 ng / L.

[0124] According to the 10 times signal-to-noise ratio of dedioxoquinone and 3-methylquinoxaline-2-carboxylic acid, determine the quantitative limit of its concentration on the machine, and then convert it into dedioxoquinone and 3-methylquinoxaline in seawater The limit of quantitation of -2-carboxylic acid. The results were: the limit of quantification of dedioxoquinone was 10 ng / L; the limit of quantification of 3-methylquinoxaline-2-carboxylic acid wa...

Embodiment 3

[0126] Method recovery and precision

[0127] The standard solution was added to the blank seawater sample to make 3 groups of standard addition samples with different concentrations, and 6 samples of each concentration were measured in parallel. The recovery rate and precision of the method were calculated. The results are shown in Tables 1 and 2.

[0128] Table 1 The recovery and precision test results of 3-methylquinoxaline-2-carboxylic acid

[0129]

[0130] As can be seen from Table 1: when the addition amount of 3-methylquinoxaline-2-carboxylic acid was 10.0~200.0ng / L, the rate of recovery of 3-methylquinoxaline-2-carboxylic acid was 72.3~91.8 %; the relative standard deviation within the batch was less than 8%, and the relative deviation between batches was less than 6%.

[0131] The rate of recovery and the precision test result of table 2 dedioxoquinone

[0132]

[0133] It can be seen from Table 2 that the recovery rate of dedioxoquinone is between 70.2% and ...

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Abstract

The invention provides a method for determining desoxyquinocetone and 3-methylquinoxaline-2-carboxylic acid in seawater, and belongs to the technical field of detection of pollutants in seawater. According to the method, the MAX column is adopted to enrich and purify the desoxyquinocetone and the 3-methylquinoxaline-2-carboxylic acid in the seawater, so that the determination of the low-concentration desoxyquinocetone and the 3-methylquinoxaline-2-carboxylic acid in the seawater can be realized; and according to the method, the adsorption column is eluted with water to remove most of water-soluble impurities, and then the adsorption column eluted with water is eluted with the ethyl acetate solution of formic acid, so that the content of other substances in the to-be-detected liquid can be reduced, interference on detection of desoxyquinocetone and 3-methylquinoxaline-2-carboxylic acid is avoided, and the detection sensitivity is improved.

Description

technical field [0001] The invention relates to the technical field of pollutant detection in seawater, in particular to a method for measuring dedioxoquinone and 3-methylquinoxaline-2-carboxylic acid in seawater. Background technique [0002] The modern aquaculture industry tends to be large-scale and intensive, and the use of antibiotics, vitamins, hormones, and metal trace elements has become an indispensable part of ensuring the development of the mariculture industry. Unfortunately, due to the lack of scientific knowledge and the drive of economic interests, the phenomenon of drug abuse in farming is widespread. The direct consequence of the abuse of veterinary drugs is the residue of veterinary drugs in animal food, which will affect human health after ingestion. The potential harm of veterinary drug residues in animal food to humans has attracted more and more attention. Only the establishment of a set of simple and efficient drug residue determination methods is th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/14G01N30/30G01N30/32G01N30/34G01N30/72G01N30/86
CPCG01N30/02G01N30/14G01N30/30G01N30/32G01N30/34G01N30/72G01N30/8675G01N2030/143G01N2030/324
Inventor 田秀慧刘小静徐英江张秀珍任传博崔艳梅黄会姜芳韩典峰王玮云宫向红李佳蔚
Owner 山东省海洋资源与环境研究院
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