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Method for detecting phenolic compounds in fish

A technology of phenolic compounds and compounds, applied in the field of aquatic product pollution detection, can solve the problems of separation and detection of interfering target compounds, waste of solvent and equipment investment, complex derivation operations, etc., achieve high accuracy, simple method, and improve analysis speed effect

Active Publication Date: 2021-04-09
宁波市产品食品质量检验研究院(宁波市纤维检验所)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, these techniques are time-consuming, wasteful of solvents and high investment in equipment
There are few reports on the detection of nitrophenols and bromophenols in fish in current research, and most of the current detection methods for phenolic compounds require derivatization, but the derivation operation is complicated, the reaction conditions are harsh, and the by-products and excessive derivatization reagents may Will interfere with the separation and detection of target compounds, etc.
At the same time, derivatization also limits the simultaneous determination of several phenolic compounds by GC-MS / MS

Method used

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  • Method for detecting phenolic compounds in fish
  • Method for detecting phenolic compounds in fish
  • Method for detecting phenolic compounds in fish

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] (1) Preparation of standard solution

[0030] Firstly, each phenolic compound was dissolved in methanol to prepare a standard stock solution, and secondly, methanol was used to dilute the standard stock solution to a final concentration of 10 / 100 mg / L to prepare a mixed standard intermediate solution. Accurately draw appropriate amounts of 18 kinds of mixed standard solutions, and dilute with blank matrix to obtain the concentration of the first type of phenolic substance as 0.10, 0.30, 0.50, 1.00, 1.50, 2.00 mg / L, and the concentration of the second type of phenolic substance as 1.00, 3.00, 5.00, 10.00, 15.00, 20.00mg / L mixed standard solution.

[0031]Wherein, the first type of phenolic substance is: nonylphenol (Nonylphenol, NP), bisphenol A (Bisphenol A, BPA), 2-bromophenol (2-Bromophenol, 2-BP), 4-bromophenol ( 4-Bromophenol, 4-BP), 2,4-Dibromophenol (2,4-Dibromophenol, 2,4-DBP), 2,6-Dibromophenol (2,6-Dibromophenol, 2,6-DBP) , 2,4,6-tribromophenol (2,4,6-Tribrom...

Embodiment 2

[0044] Embodiment 2: A method for detecting phenolic compounds in fish

[0045] (1) Sample pretreatment: enrichment of phenolic compounds

[0046] Accurately weigh 10 g of the crushed fish sample into a 50 ml plastic centrifuge tube. Then, add 2ml of water and 10ml of acetonitrile, vortex for 3min, and sonicate for 5min, then, add 2g of NaCl and 4g of MgSO to the test tube 4 . The sample solution was then vortexed for 5 min and then sonicated for 10 min. Followed by centrifugation at a speed of 4500r / min for 5min, the supernatant was collected and added to the 18 (500mg) in a 15mL centrifuge tube. After vortexing for about 10 minutes, transfer 5 mL of the supernatant to a plastic centrifuge tube. Next, nitrogen was blown to about 0.8 mL in a 40 °C water bath, and the volume was fixed to 1 mL with methanol. Finally, the supernatant was filtered with an organic filter membrane and determined by GC-MS / MS.

[0047] (2) Gas chromatography tandem mass spectrometry conditions:...

Embodiment 3

[0050] Embodiment 3: the optimization of pretreatment condition

[0051] (1) Selection of extraction solvent

[0052] Acetone, n-hexane, acetonitrile, and ethyl acetate were respectively selected as extraction solvents, and pretreatment was carried out according to the corresponding experimental procedures. The results obtained after determination are shown in Table 2. figure 2 . The results show that the extraction effect of acetone is the worst, and the recovery rate is only 31.3%. When ethyl acetate is used as the extraction solvent, a large impurity peak interference will be found near the target peak. We reasoned that the sample matrix was not easily dispersed due to the immiscibility of ethyl acetate and water. In addition, the recoveries of 18 phenolic compounds in ethyl acetate were lower than those in acetonitrile. However, using acetonitrile as the extraction solvent can obtain the highest recovery rate of 18 kinds of phenolic compounds, with an average recovery ...

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Abstract

The invention discloses a method for detecting phenolic compounds in fish, and belongs to the technical field of aquatic product pollution detection. According to the method for detecting phenolic compounds in fish of the invention, an improved QuEChERS method is adopted to extract, enrich and purify a plurality of phenolic compounds in fish; a gas chromatography tandem mass spectrometry method is adopted to qualitatively and quantitatively determine the phenolic compounds in the fish, so that a high-efficiency detection method capable of simultaneously detecting 18 phenolic compounds is established. A method which does not need derivation and can simultaneously and accurately detect a plurality of different phenolic compounds, especially alkylphenol and bromophenol compounds, in fish is developed. With the method disclosed by the invention adopted, 18 phenolic compounds can be simultaneously detected, the average adding standard recovery rate is 81.3%-115.7%, the relative standard deviation is 1.1%-11.3%, and the detection limit is 0.002-0.01 mg / kg.

Description

technical field [0001] The invention relates to a method for detecting phenolic compounds in fish, belonging to the technical field of aquatic product pollution detection. Background technique [0002] Due to the properties of surfactants, phenolic compounds are widely used in chemical, pharmaceutical, agricultural and other fields. Such compounds include highly toxic, corrosive substances derived from coal tar and plastics, dyes, pharmaceuticals, fungicides, preservatives and preservatives. These phenolic compounds are released into the aquatic environment through direct or industrial discharges, and due to their hydrophobic nature, they may bind to particulate matter deposited at the bottom of rivers or lakes. Phenolic compounds are considered to be very harmful to humans and the environment, and they are listed as priority pollutants by the US Environmental Protection Agency. Phenolic compounds can not only directly enter the human body through polluted drinking water, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/72
CPCG01N30/02G01N30/06G01N30/72G01N2030/062
Inventor 邢家溧李杨郑睿行沈坚毛玲燕徐晓蓉承海路静萍林津如
Owner 宁波市产品食品质量检验研究院(宁波市纤维检验所)
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