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Method for simultaneously determining six pyrethroid pesticide residues in poultry eggs

A technology for pyrethroids and poultry eggs, which is applied in the field of chemical detection, can solve problems such as difficult application, cumbersome and complicated operation, etc., and achieves the effects of improving efficiency, using less amount, and eliminating matrix interference.

Active Publication Date: 2019-03-12
广电计量检测集团股份有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the high content of fat and protein in poultry eggs, it is necessary to remove the fat and protein after extraction, which makes the pretreatment operation more complicated and difficult to apply.

Method used

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  • Method for simultaneously determining six pyrethroid pesticide residues in poultry eggs
  • Method for simultaneously determining six pyrethroid pesticide residues in poultry eggs
  • Method for simultaneously determining six pyrethroid pesticide residues in poultry eggs

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] Embodiment 1 QuEChERs pretreatment method optimization

[0048] Eggs are pre-treated by QuEChERs dispersive extraction and purification method, and optimized by the following methods

[0049] 1. Comparison of purification effect of solid phase extraction column on oil and protein

[0050] (1) By comparing C 18 , PSA, Si and ALN solid-phase extraction column for the purification effect of oil, to find out a better purification packing of 6 kinds of pyrethroid pesticides in eggs. Gained oils and fats were methylated after the concentration of the acetonitrile extract, compared with the area normalization method (%), and the results were as follows figure 1 and as shown in Table 1:

[0051] Table 1 Effect of different dispersive extraction fillers on the purification effect of oil

[0052]

[0053]

[0054] From the above data, it can be seen that the solid-phase extraction fillers with the best purification effect on egg oil are: C 18 >PSA>ALN>Si.

[0055] (2)...

Embodiment 2

[0067] Example 2 Determination of six pyrethroid pesticide residues in eggs by QuEChERs liquid chromatography tandem triple quadrupole mass spectrometry

[0068] 1. Preparation of standard solution

[0069] (1) Mixed stock solution 1 of 6 kinds of pesticides (for dilution curve and detection limit verification): Weigh an appropriate amount of each standard substance into the same volumetric flask, dissolve and dilute into phenothrin, fenpropathrin, The concentrations of etofenprox and tetramethrin are about 50 μg / mL, and the remaining items are stock solutions of 5 μg / mL.

[0070] (2) Mixed stock solution 2 of 6 kinds of pesticides (for standard recovery test): Weigh an appropriate amount of each standard substance into the same volumetric flask, dissolve and dilute the stock solution with a concentration of 5 μg / mL with acetonitrile.

[0071] 2. Preparation of sample solution

[0072] (1) Remove the egg shell, stir the egg white and egg yolk evenly, take 10g sample in a 50m...

Embodiment 3

[0094] Embodiment 3 detection method performance verification

[0095] Analyze the linearity of the detection method standard curve described in Example 2, the lowest detection limit of the method, the lowest quantitative limit, recovery (accuracy) and repeatability, reproducibility (precision) etc.

[0096] 1. Linear range (μg / mL)

[0097] Mixed stock solution 1 of 6 kinds of pesticides (for dilution curve and detection limit verification): Weigh an appropriate amount of each standard substance into the same volumetric flask, dissolve and dilute into phenothrin, fenpropathrin, and etofenproxil with acetonitrile , Tetramethrin concentration is about 50 μg / mL, and other items are stock solutions of 5 μg / mL, as shown in Table 8 below:

[0098] The results show that the six pyrethroid pesticides of the present invention have a good linear relationship in the range of 0.02-0.400 μg / mL, and the correlation coefficients are all greater than 0.996. The linear relationship is shown i...

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Abstract

The invention discloses a method for simultaneously determining six pyrethroid pesticide residues in poultry eggs. The method comprises the following steps that S1, a sample to be tested is weighed, dispersion extraction is performed by QuEChERs, after supernatant is filtered, the sample to be tested is obtained, and a matrix standard curve is drawn; S2, the sample to be tested obtained in the step S1 is simultaneously subjected to determination of the residual amount of six pyrethroid pesticides by liquid chromatography tandem mass spectrometry, and retention time and ion fragment abundanceratio are used for qualitative analysis, and according to the area of an ion peak, an external standard method is used for quantitative analysis; the poultry egg samples are subjected to QuEChERS purification, the matrix interfering the measurement in the samples is effectively removed, blank sample matrix calibration is performed, the six pyrethroids pesticide residues are determined simultaneously by using liquid chromatography tandem triple quadrupole, using retention time and ion fragment abundance ratio for qualitative analysis and using an external standard method for quantitative analysis according to the area of the ion peak. After optimization, the recovery rate of the target pesticide compound in eggs reaches 77.1%-109.4%, the precision and stability test RSD within 24h is less than or equal to 15%, and the linear range is within 0.005mg / kg-0.200mg / kg.

Description

technical field [0001] The invention relates to the technical field of chemical detection, in particular to a method for simultaneously measuring six pyrethroid pesticide residues in poultry eggs. Background technique [0002] In poultry breeding, such as laying hen breeding, hens will suffer from parasites, lice, mites and other pathogens, which will have varying degrees of harm to the growth and development of chickens, resulting in a decline in egg production. In order to treat these diseases, chicken farmers usually use insecticides to prevent the spread of diseases; currently, besides the insecticides reported first by fipronil, more commonly used insecticides are pyrethroid pesticides , used to dilute with water and spray for disinfection. [0003] Pyrethroid pesticides are a class of biomimetic synthetic insecticides widely used at present, which are similar in structure or biological activity to natural pyrethrum. This type of pesticide was considered to be highly ...

Claims

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Application Information

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IPC IPC(8): G01N30/88G01N30/06
CPCG01N30/06G01N30/88
Inventor 曹小彦蓝梦哲周九林李金连周敏
Owner 广电计量检测集团股份有限公司
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