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Method for determining residual amount of canthaxanthin pigment in eggs

A cantharidin yellow pigment and residual amount technology, which is applied in the directions of measuring devices, instruments, scientific instruments, etc., can solve the problems of increasing the risk of consumer health hazards, poor accuracy of cantharidin yellow pigment, and accumulation of pigments.

Inactive Publication Date: 2020-01-10
贵州省兽药饲料监察所
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  • Summary
  • Abstract
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  • Claims
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AI Technical Summary

Problems solved by technology

[0002] At present, there are national standards and industry standard methods for the detection of veterinary drug residues in poultry eggs in my country, mainly using liquid chromatography and liquid chromatography-tandem mass spectrometry, but there is no national standard or industry standard for the detection methods of pigment residues in poultry eggs method, resulting in a blank detection of pigments in poultry eggs, increasing the quality and safety of poultry egg products and unfavorable supervision
Especially in the production process of poultry eggs, in order to cater to the psychology of consumers, some unscrupulous farmers and enterprises arbitrarily add coloring agents to change the yolk color of eggs and use them as native eggs to pursue high returns, while ignoring product quality and safety, resulting in pigments in poultry eggs. A large amount of accumulation and residue in the medium increases the risk of health hazards to consumers
[0003] At present, in the detection of poultry egg pigment, especially the detection of cantharidin, due to the interference of lipids and proteins in the sample, and the instability of cantharidin itself, the detection accuracy of cantharidin in poultry eggs is poor. , low sensitivity, slow analysis speed, etc.

Method used

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  • Method for determining residual amount of canthaxanthin pigment in eggs
  • Method for determining residual amount of canthaxanthin pigment in eggs
  • Method for determining residual amount of canthaxanthin pigment in eggs

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Embodiment 1: the assay method of cantharidin residual amount in poultry eggs,

[0026] The methods for determining the residual amount of canthaxanthin in poultry eggs include the following:

[0027] 1. Pretreatment

[0028] Weigh 2±0.05g poultry egg sample to be tested, put it in a centrifuge tube, add 0.2g pyrogallic acid, add 10.0mL acetonitrile extract, vortex mix for 1.0min, ultrasonically extract for 30min, and centrifuge at 10000r / min for 5min. Transfer the supernatant to a 20mL volumetric flask.

[0029] Add 8.0mL acetonitrile extract solution again and repeat the extraction once;

[0030] Combine the supernatants extracted twice into the same volumetric flask, and dilute to the mark with acetonitrile, and mix well.

[0031] Take 5.0 mL of the supernatant in a 10 mL centrifuge tube, dry it under nitrogen at 45°C, dissolve the residue with 1.0 mL of acetonitrile, centrifuge at 10,000 r / min for 5 min, and pass through a 0.22 μm microporous membrane to obtain t...

Embodiment 2

[0051] Embodiment 2: repeatability, accuracy, sensitivity verification

[0052] (1) Repeatability verification

[0053] Get a test sample solution, repeat sample injection 6 times, measure the peak area of ​​cantharidin, calculate the RSD of cantharidin peak area to be 0.1%. It can be seen that the repeatability of the method of the present invention is very good.

[0054] (2) Accuracy verification

[0055] Cantharidin was added to egg blank samples to prepare test solutions with cantharidin additions of 0.5 μg / kg, 1.0 μg / kg, 10.0 μg / kg, and 30.0 μg / kg, and each addition was prepared in parallel in 3 copies, according to the implementation The pretreatment method in Example 1 prepares the test solution, and it is measured on the machine, and each sample is measured 2 times. The measurement results are shown in Table 3.

[0056] Table 3 cantharidin recovery rate assay result

[0057]

[0058]

[0059] As can be seen from Table 1, the cantharidin recovery rate is 79.3...

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Abstract

The invention discloses a method for determining the residual amount of a canthaxanthin pigment in eggs. The method comprises the following steps: (1) weighing an egg sample to be determined, adding pyrogallic acid, adding an acetonitrile extracting solution, carrying out vortex mixing and ultrasonic extraction in sequence, and transferring the supernatant; fixing the volume with acetonitrile after combining the supernatant extracted in two times, and mixing uniformly; drying a part of the supernatant under nitrogen, dissolving the residue with the acetonitrile, and centrifuging and filteringto obtain a sample solution; (2) analyzing the sample solution on a liquid chromatograph to determine the canthaxanthin peak area; and (3) determining the canthaxanthin peak area with multiple groupsof canthaxanthin solutions with known mass concentration, performing linear regression by taking the canthaxanthin mass concentration as a horizontal axis and taking the corresponding peak area as a longitudinal axis, and establishing a canthaxanthin linear regression equation; and calculating the residual amount of the canthaxanthin pigment on the egg to be determined according to the canthaxanthin peak area of the egg sample to be determined. The method has the characteristics of easiness, fastness, accuracy and sensitivity, and is suitable for the detection and analysis of the residual amount of canthaxanthin pigment in eggs.

Description

technical field [0001] The invention relates to a method for determining the residual amount of canthaxanthin in poultry eggs, and belongs to the technical field of cantharidin detection. Background technique [0002] At present, there are national standards and industry standard methods for the detection of veterinary drug residues in poultry eggs in my country, mainly using liquid chromatography and liquid chromatography-tandem mass spectrometry, but there is no national standard or industry standard for the detection methods of pigment residues in poultry eggs method, resulting in a blank detection of pigments in poultry eggs, increasing the quality and safety of poultry egg products and unfavorable supervision. Especially in the production process of poultry eggs, in order to cater to the psychology of consumers, some unscrupulous farmers and enterprises arbitrarily add coloring agents to change the yolk color of eggs and use them as native eggs to pursue high returns, wh...

Claims

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Application Information

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IPC IPC(8): G01N30/88G01N30/06
CPCG01N30/06G01N30/88G01N2030/047G01N2030/884
Inventor 黄鑫金晓峰栾庆祥赵贵焦仁刚罗永成周艺林郭萍陈锡龙周泽晓黄瑾古海廖欢
Owner 贵州省兽药饲料监察所
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