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Method for determining 47 pesticide residues in honey and bee pollen

A technology for pesticide residues and determination methods, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve problems that have not yet occurred, achieve high accuracy, solve matrix effect problems, and improve the recovery rate

Pending Publication Date: 2022-01-04
NANJING INST OF ENVIRONMENTAL SCI MINIST OF ECOLOGY & ENVIRONMENT OF THE PEOPLES REPUBLIC OF CHINA
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] However, studies have shown that there are as many as 47 pesticide residues in bee products, and a method that can simultaneously measure these 47 pesticide residues has not yet appeared in the prior art.

Method used

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  • Method for determining 47 pesticide residues in honey and bee pollen
  • Method for determining 47 pesticide residues in honey and bee pollen
  • Method for determining 47 pesticide residues in honey and bee pollen

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Embodiment 1: 47 kinds of pesticide residue assay methods in a kind of honey and bee pollen, comprise the following steps:

[0042] S1, extraction;

[0043] S1-1. Mix the honey sample and bee pollen sample with deionized water at a volume ratio of 1:3 to obtain the honey sample aqueous solution and the bee pollen sample aqueous solution; then mix the honey sample aqueous solution and the bee pollen sample aqueous solution with acetonitrile according to the volume ratio Mix 1:2 evenly to obtain mixed solution A and mixed solution B;

[0044] S1-2. Cool the mixed solution A and the mixed solution B obtained in step S1-1 respectively at -15°C for 8 minutes, then treat them under 200W ultrasonic power for 15 minutes, then let them stand for 10 minutes, and collect the acetonitrile layer , to obtain extract A and extract B;

[0045] S2, purification;

[0046] S2-1 filter the extract A and extract B obtained in step S1-2 respectively through a 0.10 μm filter membrane, and ...

Embodiment 2

[0065] Embodiment 2: 47 kinds of pesticide residue assay methods in a kind of honey and bee pollen, comprise the following steps:

[0066] S1, extraction;

[0067] S1-1. Heat the honey sample to 45°C, and then filter it with a 50-mesh filter. By heating and filtering the honey sample, it can effectively remove the mixed beeswax, bee corpses and other substances in the honey sample, so as to exclude the honey sample The interference of irrelevant impurities in the medium to the measurement results, and then the honey sample and the bee pollen sample were mixed with deionized water according to the volume ratio of 1:5 to obtain the honey sample aqueous solution and the bee pollen sample aqueous solution; then the honey sample aqueous solution and the bee pollen The sample aqueous solution and acetonitrile are mixed uniformly according to the volume ratio of 1:24 to obtain mixed solution A and mixed solution B; wherein, the specific operation of mixing is as follows: place the mi...

Embodiment 3

[0089] Embodiment 3: 47 kinds of pesticide residue assay methods in a kind of honey and bee pollen, comprise the following steps:

[0090] S1, extraction;

[0091] S1-1. Mix the honey sample and bee pollen sample with deionized water at a volume ratio of 1:6 to obtain honey sample aqueous solution and bee pollen sample aqueous solution; then mix the honey sample aqueous solution and bee pollen sample aqueous solution with acetonitrile according to the volume ratio 1:5 mixed evenly to obtain mixed solution A and mixed solution B;

[0092] S1-2. Place the mixed solution A and the mixed solution B obtained in step S1-1 respectively at -30°C for 15 minutes, and then treat them for 40 minutes at an ultrasonic power of 800 W, and then let them stand for 20 minutes. Adding a sodium chloride solution with a mass concentration of 15% into A and mixed solution B, stirring and mixing evenly, and then carrying out salting-out treatment; wherein, the added amount of sodium chloride soluti...

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Abstract

The invention provides a method for determining 47 pesticide residues in honey and bee pollen. The method comprises the following steps: S1, uniformly mixing a honey sample and a bee pollen sample with deionized water and acetonitrile respectively, then cooling, and carrying out ultrasonic treatment to obtain an extracting solution A and an extracting solution B; S2, respectively carrying out filtering, purification treatment and nitrogen blowing on the extracting solution A and the extracting solution B to obtain a to-be-detected solution A and a to-be-detected solution B; S3, preparing a standard stock solution and a standard working solution, drawing a standard working curve, substituting the measured values in the to-be-detected solution A and the to-be-detected solution B into the standard curve, and calculating the content of the pesticide residues in the to-be-detected solution A and the to-be-detected solution B; and S4, quantifying the to-be-detected solution A and the to-be-detected solution B by using a single-ion external standard method by using the standard working curve, and finally determining the nature by using the retention time of chromatographic peaks appearing in the to-be-detected solution A and the to-be-detected solution B and the accurate mass number of qualitative ions. The method is high in measuring efficiency, good in reliability and suitable for large-scale popularization.

Description

technical field [0001] The invention relates to the technical field of pesticide residue detection in bee products, in particular to a method for measuring 47 kinds of pesticide residues in honey and bee pollen. Background technique [0002] my country is the largest beekeeping country in the world. Pesticide residues in bees come from nectar plants polluted by pesticides and acaricides. These pesticide residues in honey pose a threat to human health, and people are paying more and more attention to control. In addition to strictly restricting the use of highly toxic and high-residue pesticides, it is also very important to establish a monitoring method for multi-residue pesticides in honey. In the past ten years, in order to achieve the purpose of reducing sample processing steps, improving detection accuracy, and reducing the generation of toxic waste, researchers have developed a variety of sample pretreatment methods. These methods include: solvent extraction (SE), super...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/06G01N30/88
CPCG01N30/06G01N30/88
Inventor 李菊颖豆叶枝曹莉余佳何健孔德洋张悦清许静
Owner NANJING INST OF ENVIRONMENTAL SCI MINIST OF ECOLOGY & ENVIRONMENT OF THE PEOPLES REPUBLIC OF CHINA
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