Method for detecting dioxin and dioxin polychlorinated biphenyl in poultry eggs

A technology of dioxins and polychlorinated biphenyls, which is applied in measuring devices, instruments, scientific instruments, etc., can solve the problems of interference, cumbersome pretreatment purification methods, complex substrates, etc., and achieves the effect of safe and environmentally friendly extraction of solvents.

Active Publication Date: 2018-03-20
GUANGDONG TESTING INST OF PROD QUALITY SUPERVISION
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] my country's current standards for detecting dioxins and dioxin-like PCBs in food include the US Environmental Protection Agency's "Method 1613 Tetra-through Octa-Chlorinated Dioxins and Furans by IsotopeDilution HRGC / HRMS" and "GB 5009.205-2013 Food Safety National Standard Food Determination of Toxic Equivalents of Dioxins and Their Analogues in Dioxins and Their Analogues", however, the pretreatment and purification methods of the above standards are tedious and time-consuming, especially for poultry egg samples, where the matrix is ​​complex and the interference is serious, so it is difficult to obtain a satisfactory purification effect

Method used

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  • Method for detecting dioxin and dioxin polychlorinated biphenyl in poultry eggs
  • Method for detecting dioxin and dioxin polychlorinated biphenyl in poultry eggs
  • Method for detecting dioxin and dioxin polychlorinated biphenyl in poultry eggs

Examples

Experimental program
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Effect test

Embodiment 1

[0045] The method for detecting dioxins and dioxins-like polychlorinated biphenyls in poultry eggs provided in this embodiment includes the following steps:

[0046] (1) Sample preparation

[0047] Collect egg samples (including eggs, duck eggs, goose eggs, pigeon eggs, quail eggs and snake eggs), and mark and number them. The samples collected on site are packed with light-proof materials such as aluminum foil, and are transported to the experiment in a small freezer Store at room temperature.

[0048] Place the sample in an oven at 90-100°C, wait for the egg whites to solidify, remove the shell with tweezers, place it on tin foil, and bake it in an oven at 90-100°C for 21 to 33 hours. Use a meat grinder to crush the shelled samples, mix them, and store them in a dry box.

[0049] The best oven temperature is 90~100℃. If the temperature is lower than 90℃, it will take a long time to dry the samples. If the temperature is higher than 100℃, the eggs will burst and splash. The baking t...

Embodiment 2

[0114] The difference from Example 1 is that when preparing the sample in step (1), place the sample in an infrared desiccator at 90-100°C. After the egg whites are solidified, use tweezers to remove the shells and place them on tin foil. Bake in an infrared dryer at 90~100℃ for 21~33h. The test results are shown in Table 8 and Table 9. Compared with Example 1, the relative error is less than 10%.

[0115] Table 8 Comparison of the total dioxin toxicity equivalent of Example 2 and Example 1

[0116]

[0117]

[0118] Table 9 Comparison of the total toxicity equivalent of dioxin-like PCBs in Example 2 and Example 1

[0119]

Embodiment 3

[0121] The difference from Example 1 is that when preparing the test substance in step (2), the rapid extraction apparatus is used to extract the test substance in the test sample.

[0122] Test conditions of fast extraction instrument:

[0123] Apparatus: Fast solvent extraction instrument, 34ml stainless steel extraction cell; extraction collection bottle (40mL; 60mL)

[0124] Solvent: n-hexane (pesticide grade), methylene chloride (pesticide residue grade).

[0125] Extraction conditions: pressure 1500-2000psi; temperature 80℃~150℃; heating time 5min~20min; static time 5min~15min; solvent, n-hexane: dichloromethane (ratio range 1:0.5~1.5); washing volume 45%~ 75% (volume of extraction tank);

[0126] The range of N2 purge time is 60s~150s; the static cycle is 2~6 times; the total extraction time is 17min~45min for each sample.

[0127] Sample Preparation:

[0128] 10g of the sample is uniformly mixed with 5-10g of sodium sulfate, then ground and dried. Fill 5g alumina through the fib...

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Abstract

The invention discloses a method for detecting dioxin and dioxin polychlorinated biphenyl in poultry eggs. The method comprises the following steps: (1) preparing a sample; (2) preparing a to-be-detected object; (3) purifying by virtue of an acid silica gel, (4) purifying by virtue of a multi-section silica gel column; (5) purifying by virtue of a gel chromatographic column; (6) purifying by virtue of an alkaline alumina column and a Florisil column or an activated carbon chromatographic column; and (7) carrying out machine testing. The method has the beneficial effects that the pretreatment is rapid and safe, and the matrix interference is slight; and by utilizing a high-resolution gas chromatography / double focusing magnetic mass spectrometer HRGC / HRMS in detection, the contents of dioxinand dioxin polychlorinated biphenyl in the poultry eggs can be relatively accurately acquired.

Description

Technical field [0001] The invention belongs to the technical field of food-related product detection, and specifically relates to a detection method of dioxins and dioxins-like polychlorinated biphenyls in poultry eggs. Background technique [0002] Persistent Organic Pollutants (POPs for short) are highly toxic, difficult to degrade after entering the environment, and bioaccumulate. They can migrate long distances across the border through air, water, and migratory species and deposit them far away from their discharge locations. Natural or synthetic organic matter that subsequently accumulates in the terrestrial and water ecosystems there and has a serious negative impact on the local environment and organisms. It has persistence, bioaccumulation, long-distance migration ability and high Toxic characteristics. [0003] Dioxins and dioxin-like PCBs are a type of persistent organic pollutants. Dioxins usually refer to a group of polychlorinated substituted planar aromatic compou...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/045G01N2030/062G01N2030/065
Inventor 唐穗平邱启东綦艳陈满英李锦清
Owner GUANGDONG TESTING INST OF PROD QUALITY SUPERVISION
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