A method for determining the residual content of hymexazol pesticides

A hamexamol and triple quadrupole technology, which is applied in the field of pesticide detection, can solve the problems of reducing the detection accuracy, unable to accurately determine the content of hamexamol pesticide residues, and difficult to meet the accuracy requirements of hamexamol pesticide residues.

Active Publication Date: 2016-09-28
CHINA TOBACCO FUJIAN IND
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, the electrochemical analysis method is mainly used for the quantitative analysis of the hymexazol production process, which has low sensitivity and poor specificity, and it is difficult to meet the accuracy requirements for the detection of hymexazol pesticide residues; the gas chromatography method has high sensitivity and strong specificity , but due to the thermal instability of hymexazol, it needs to be derivatized before gas chromatography detection. Derivatization not only increases the complexity and cost of detection, but also incomplete derivatization will reduce the accuracy of detection; as for liquid phase Chromatography-ultraviolet absorption method, due to the high polarity of hymexazol, it is suitable to use this method for detection, but there are many impurity absorption wavelengths near the ultraviolet absorption wavelength (200nm) of hymexazol, which interferes with the detection of hymexazol , and the sensitivity of the UV detector to hymexazol is low, which cannot meet the accuracy requirements for the detection of hymexazol residues
[0006] The above-mentioned multiple techniques are all unable to accurately measure the content of hymexazol pesticide residues; and, so far, those skilled in the art have been unable to find a method that can accurately measure the content of hymexazol pesticide residues in animals and plants

Method used

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  • A method for determining the residual content of hymexazol pesticides
  • A method for determining the residual content of hymexazol pesticides
  • A method for determining the residual content of hymexazol pesticides

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0089] Example 1: Detection of Hymexazol Pesticide Residues in Tobacco Samples

[0090] 1) Sample extraction steps:

[0091] Weigh about 2g (accurate to 0.1mg) of Burley tobacco into a 50mL capped centrifuge tube and add 10mL of water, oscillate until the sample is fully infiltrated by water, let stand for 10min; pipette 10mL of acetone into the centrifuge tube, and place Shake at 2000r / min for 2min on a vortex mixer; store the centrifuge tube in the freezer (-18°C) for 10min and then take it out. Add 4g of anhydrous magnesium sulfate, 1g of sodium chloride, 1g of sodium citrate, and 0.5g of disodium hydrogen citrate into the centrifuge tube, and immediately oscillate on a vortex mixer at a speed of 2000r / min for 2min to prevent anhydrous sulfuric acid Magnesium reacts with water to cause local overheating and agglomeration, and then centrifuge at 4000r / min for 5min. Pipette 1.5 mL of the supernatant of the extract into a 2 mL centrifuge tube, add 150 mg of anhydrous magne...

Embodiment 2

[0103] Example 2: Detection of Hymexazol Pesticide Residues in Vegetable Samples

[0104] 1) The extraction steps of the sample: with embodiment 1.

[0105] 2) Sample detection steps:

[0106] High-performance liquid chromatography-triple quadrupole mass spectrometer (Agilent 1290 high performance liquid chromatograph from Agilent Company of the United States and API5500 triple quadrupole tandem mass spectrometer from AB SCIEX Company of the United States) was used to detect samples, and the determination conditions were as follows: :

[0107] Chromatographic conditions: injection volume: 25 μL, chromatographic column: Agilent ZORBAX ultra-high pressure rapid high resolution 300SB-C8 (specification: 2.1×100 mm, 1.8 μm), ethanol-water elution program: 0 to 3.5 minutes, ethanol and water The volume ratio of ethanol and water is 5:5, 3.5 to 15 minutes, the volume ratio of ethanol and water is 8:1, the flow rate is 300 μL / min, and the column temperature is 40°C.

[0108] Mass...

Embodiment 3

[0115] Example 3: Detection of Hymexazol Pesticide Residues in Tea Samples

[0116] 1) The extraction steps of the sample: with embodiment 1.

[0117] 2) Sample detection steps:

[0118] High-performance liquid chromatography-triple quadrupole mass spectrometer (Agilent 1290 high performance liquid chromatograph from Agilent Company of the United States and API5500 triple quadrupole tandem mass spectrometer from AB SCIEX Company of the United States) was used to detect samples, and the determination conditions were as follows: :

[0119] Chromatographic conditions: injection volume: 50 μL, chromatographic column: Agilent ZORBAX ultra-high pressure rapid high resolution 300SB-C8 (specification: 2.1×100mm, 1.8 μm), ethanol-water elution program: 0 to 3 minutes, ethanol and water The volume ratio is 4:6, 3 to 5 minutes, the volume ratio of ethanol and water is 8.5:1, the flow rate is 400 μL / min, and the column temperature is 50°C.

[0120] Mass spectrometry conditions: atomi...

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Abstract

The invention belongs to the field of pesticide detection and relates to a method for determining the residual content of hymexazol pesticides. Specifically, the present invention relates to a method for detecting hymexazol, comprising the following steps: (1) using liquid chromatography to separate hymexazol from a sample, (2) using triple quadrupole mass spectrometry to detect hymexazol. The method for detecting hymexazol of the present invention has high sensitivity, short detection period, simple operation, less matrix interference, and has good application prospects.

Description

technical field [0001] The invention belongs to the field of pesticide detection and relates to a method for determining the residual content of hymexazol pesticides. Background technique [0002] Hymexazol, commonly known as Luheng No. 1, Tujunxiao, Tujunke or Lvjiabao, is a high-efficiency broad-spectrum fungicide, which is effective against pathogens of various soil-borne diseases of plants such as Pythium, seedling rot, Fusarium, Both Rhizoctonia and Rhizoctonia have strong killing and control effects. Its active ingredient is 3-hydroxy-5-methylisoxazole (hymexazol), and its structural formula is shown in the following formula I: [0003] [0004] With the expansion of the scope of application of hymexazol, the toxic effects of hymexazol residues in plants and the accumulation of pesticide residues in animals on the human body have gradually attracted attention. Some data show that hymexazol residues will not only damage the human body. Stomach, kidney organs, and t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/88
Inventor 张建平谢卫黄朝章许寒春吴清辉黄华发邓其馨叶仲力苏明亮刘江生
Owner CHINA TOBACCO FUJIAN IND
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