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Method for determining seven indicative polychlorinated biphenyls in fish scales

A polychlorinated biphenyl and determination method technology, applied in the field of organic pollutants, can solve complex and cumbersome problems, cannot meet the detection requirements of large batches of samples, and has not been reported, so as to improve purification efficiency, meet daily use requirements, and improve the extraction effect. Enhanced effect

Active Publication Date: 2021-08-27
GUANGDONG TESTING INST OF PROD QUALITY SUPERVISION
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, most of the existing studies have used solid-phase extraction column purification, such as basic alumina column purification. This method is complicated and cumbersome to operate and cannot meet the detection requirements of large-scale samples.
[0009](3) Instrument detection methods. At present, there are seven indicative methods for the determination of PCBs, including gas chromatography-electron capture detector (ECD) method, gas chromatography-mass spectrometry method, gas chromatography-tandem mass spectrometry, high-resolution gas chromatography-high-resolution magnetic mass spectrometry, but due to the particularity of fish scales, there is no report applicable to the method for indicating PCBs in fish scale matrix samples

Method used

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  • Method for determining seven indicative polychlorinated biphenyls in fish scales
  • Method for determining seven indicative polychlorinated biphenyls in fish scales
  • Method for determining seven indicative polychlorinated biphenyls in fish scales

Examples

Experimental program
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Effect test

Embodiment 1

[0064] The present embodiment comprises the following contents to the test of seven polychlorinated biphenyls in grass carp fish scales:

[0065] The collected 6 batches of grass carp scales were freeze-dried and pulverized evenly. Weighed 2g samples into a 50mL Teflon tube, added 50μL (1000ng / mL) PCB198 as an internal standard, and used 5mL HNO 3 :H 2 o 2 (1:1, V:V) mixed solution digested hard fish scales at 60°C, added ultrapure water, and accelerated solvent extraction with 10mL n-hexane-ethyl acetate (1:1, volume ratio) (temperature 50°C, pressure 1800psi, time 18min), purified with concentrated sulfuric acid (95%, mass percentage), then purified with 9g of basic alumina-magnesia-anhydrous sodium sulfate (5:2:1) mixed particles, centrifuged, and transferred the extract Put it in a heart-shaped bottle, concentrate it by rotary evaporation, make it up to 1mL with nonane, detect it by gas chromatography-electron capture detector (ECD), and quantify it by internal standard ...

Embodiment 2

[0093] The present invention comprises the following contents to the test of seven polychlorinated biphenyls in carp fish scales:

[0094] The collected 6 batches of carp scales were freeze-dried and pulverized evenly. Weighed 2g samples into a 50mL Teflon tube, added 50μL (1000ng / mL) PCB198 as an internal standard, and added 5mL HNO 3 :H 2 o 2 (1:1, V:V) mixed solution digested hard fish scales at 60°C, added ultrapure water, and accelerated solvent extraction with 10mL n-hexane-ethyl acetate (1:1, volume ratio) (temperature 50°C, pressure 1800psi, time 18min), purified with concentrated sulfuric acid (95%, mass percentage), then purified with 9g of basic alumina-magnesia-anhydrous sodium sulfate (5:2:1) mixed particles, centrifuged, and transferred the extract Put it in a heart-shaped bottle, concentrate it by rotary evaporation, make it up to 1mL with nonane, detect it by gas chromatography-electron capture detector (ECD), and quantify it by internal standard method.

[...

Embodiment 3

[0102] The collected 6 batches of tilapia fish scales were tested according to the pretreatment method and instrument conditions of Example 1, and the test results are shown in Table 4:

[0103] Table 4 Test results of seven PCBs in tilapia fish scales

[0104]

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Abstract

The invention discloses a method for determining seven indicative polychlorinated biphenyls in fish scales, which comprises the following steps of selecting the fish scales, freeze-drying, crushing, placing in a Teflon container, adding an internal standard, digesting the hard fish scales by using an HNO3: H2O2 mixed solution, then adding ultrapure water, then adding n-hexane-ethyl acetate for accelerated solvent extraction, purifying an extract by concentrated sulfuric acid, adding alkaline aluminum oxide-magnesium oxide-anhydrous sodium sulfate mixed particles, purifying, centrifuging, taking supernate, carrying out rotary evaporation concentration, fixing the volume, detecting by adopting a gas chromatography-electron capture detector method, and quantifying by adopting an internal standard method, thereby obtaining the content of the seven indicative polychlorinated biphenyls in the fish scales. According to the method, the accelerated solvent is adopted for extraction after the fish scales are nitrified, the extraction efficiency is high, the extract is purified by concentrated sulfuric acid and alkalized silica gel, the purification efficiency is improved, the gas chromatography-electron capture detection method is adopted for determination, the sampling representativeness is enhanced, the extraction, purification and detection time is short, and the method is suitable for batch detection.

Description

technical field [0001] The invention belongs to the technical field of organic pollutants, in particular to a method for determining seven kinds of indicative polychlorinated biphenyls in fish scales. Background technique [0002] Polychlorinated biphenyls (PCBs) are a class of chlorides formed by replacing the hydrogen atoms on the biphenyl ring with chlorine, also known as chlorinated biphenyls. There are 209 homologue isomers. Animal experiments have shown that PCBs can affect the fertility of rats, and long-term exposure to small doses of drugs can produce chronic toxic effects, manifested as periorbital edema, hair loss, and acne-like skin lesions. Severely poisoned animals may have symptoms such as diarrhea, blood and tears, ataxia, progressive dehydration, depression of the central nervous system, and even death. The physical and chemical properties of PCBs are extremely stable, not easy to decompose, and can exist in soil, atmosphere, water quality, animals and pla...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/70
CPCG01N30/02G01N30/06G01N30/70G01N2030/045
Inventor 邱启东陈满英唐穗平綦艳李锦清
Owner GUANGDONG TESTING INST OF PROD QUALITY SUPERVISION
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