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Method for detecting pesticide residues in bee pollen

A technology of pesticide residues and detection methods, applied in the field of liquid chromatography detection, to achieve the effect of accurate detection

Active Publication Date: 2018-10-12
BEE RES INST CHINESE ACAD OF AGRI SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, because bee hives are exposed to many residual crops, and other pesticides such as acaricides and fungicides are used in the hive to reduce the harm of mites and microsporidia

Method used

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  • Method for detecting pesticide residues in bee pollen
  • Method for detecting pesticide residues in bee pollen
  • Method for detecting pesticide residues in bee pollen

Examples

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Embodiment 1

[0042] This embodiment relates to the detection of pesticide residues in bee pollen, comprising the following steps:

[0043] A. Sample pretreatment

[0044] 1) Weigh 2g of the pollen to be tested and place it in a 50mL centrifuge tube, add 5mL of pure water to the centrifuge tube, vortex for 1min, and obtain the aqueous solution of bee pollen;

[0045] 2) Add 15 mL of acetonitrile to the aqueous solution of bee pollen, extract under ultrasonic power of 100 W for 20 min, add salt bag (sodium chloride or magnesium sulfate) into a 50 mL centrifuge tube, vortex and shake for 1 min, and take the acetonitrile layer;

[0046] 3) The acetonitrile layer was placed at -80°C for 4min, centrifuged at 3800rpm at 4°C for 5min, and the supernatant was taken.

[0047] 4) Pass the supernatant through the Cleanert NANO CARB small column for a total of 2 pushes to complete the pretreatment of the sample.

[0048] B. Chromatographic analysis

[0049] The pretreated samples were analyzed by LC...

experiment example

[0064] This experimental example verifies the accuracy of the method of the present application. Add 150, 375 and 750 μg / kg 3 different levels of mixed standard solutions to the blank rape pollen sample to carry out the recovery experiment, and each addition concentration is repeated 5 times in parallel. Calculate recovery and relative standard deviation (RSD). The results are shown in Table 3, the average recovery of 9 pesticides in rapeseed pollen is between 82.5%-112.9%, and the relative standard deviation (RSD) is between 1.6-10.8%, the method has a good recovery and reproducibility.

[0065] Table 3 The sample recovery (n=5) and relative deviation (RSD) of 9 pesticides

[0066]

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Abstract

The invention relates to a method for detecting pesticide residues in bee pollen. The main improvement of the method is characterized in that bee pollen to be detected is pretreated by adopting a technology; and the technology comprises the following steps: 1) fully extracting pesticide residues in the bee pollen to be detected by using acetonitrile to obtain a pesticide residue-dissolved acetonitrile solution, 2) standing the pesticide residue-dissolved acetonitrile solution at -75 to -80 DEG C for 3-8 min to remove fat substances, and 3) purifying the fat substance-removed acetonitrile solution by a purifying column to obtain a sample to be detected. The optimization of the extraction process of pesticide residues in the bee pollen makes the pesticide residues in the bee pollens fully extracted, so a foundation is laid for subsequent accurate detection; and the detection method is further optimized in order to realize accurate detection.

Description

technical field [0001] The invention relates to the technical field of liquid chromatography detection, in particular to the detection of common pesticide residues in bee pollen. Background technique [0002] At present, there are few analytical methods for various pesticide residues in bee pollen, and most of the reported methods are used to detect neonicotinoid pesticide residues. However, because the bee hives are exposed to many residual crops, and other pesticides such as acaricides and fungicides are also used in the hives to reduce the harm of mites and microsporidia. The data indicated the presence of insecticides, fungicides and herbicides at varying levels in the hive. Therefore, it is necessary to develop a simple and sensitive method for the analysis of common pesticide residues. [0003] Since the rich lipids (10-20%) and proteins (30-40%) in bee pollen will interfere with the determination of residue analysis, if you want to accurately determine the pesticide...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/14G01N30/34G01N30/72
CPCG01N30/02G01N30/06G01N30/14G01N30/34G01N30/72G01N2030/062
Inventor 赵柳微梁馨文吴黎明薛晓锋万正瑞
Owner BEE RES INST CHINESE ACAD OF AGRI SCI
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