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Method for extracting and purifying hymexazol pesticide residues in tobacco and composition used

A technology of hymexazol and its composition, which is applied in the field of extraction and detection of pesticide residues, can solve problems such as increasing the difficulty of separation and purification, interference of detection instruments, and toxicity of hymexazol, so as to improve detection sensitivity and accuracy, avoid interference, The effect of solving pollution

Active Publication Date: 2016-04-13
CHINA TOBACCO FUJIAN IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] There have been reports on the extraction of hymexazol residues from soil samples or watermelon samples, but the extraction rate is not high
More importantly, due to the particularity of tobacco samples, such as a very complex matrix, a large number of impurities and pigments may interfere with the detection instrument
In addition, hymexazol itself is toxic, which also increases the difficulty of separation and purification
[0008] Therefore, there is no effective method for extracting and purifying hymexazol residues from tobacco samples

Method used

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  • Method for extracting and purifying hymexazol pesticide residues in tobacco and composition used
  • Method for extracting and purifying hymexazol pesticide residues in tobacco and composition used
  • Method for extracting and purifying hymexazol pesticide residues in tobacco and composition used

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] Example 1: Detection of Hymexazol Pesticide Residues in Burley Tobacco Samples

[0045] 1. Extraction and purification of hymexazol residues

[0046] (1) Weigh about 2g of Burley tobacco sample into a 50mL capped centrifuge tube, add 10mL of sodium hydroxide aqueous solution with a pH value of 8.5, shake until the sample is fully infiltrated by water, and let stand for 5min. Add 10 mL of ethyl acetate to the centrifuge tube, and place it on a vortex mixer at a speed of 2000 r / min for 2 min to obtain the primary extract.

[0047] (2) Add the following reagents to the primary extract: 8g of anhydrous magnesium sulfate, 2g of sodium chloride, 1g of sodium citrate and 0.5g of disodium hydrogen citrate, and vibrate on a vortex mixer at a speed of 2000r / min for 2min , stand still.

[0048] (3) After standing still, pipette the supernatant into a centrifuge tube, add 150 mg of graphitized carbon black, shake on a vortex mixer at a rate of 2000 r / min for 2 min, and after st...

Embodiment 2

[0069] Example 2: Detection of Hymexazol Pesticide Residues in Flue-cured Tobacco Samples

[0070] Weigh about 2g of flue-cured tobacco sample into a 50mL centrifuge tube with a cover, add 15mL of sodium hydroxide aqueous solution with a pH value of 8.6, shake until the sample is fully infiltrated by water, and let stand for 10min. Add 15 mL of ethyl acetate to the centrifuge tube, and place it on a vortex mixer at a speed of 2500 r / min for 5 min to obtain the primary extract;

[0071] Add 9g of anhydrous magnesium sulfate and 3g of sodium chloride to the primary extract, immediately oscillate on a vortex mixer at a speed of 2500r / min for 5min, and let stand.

[0072] After standing still, pipette the supernatant into a centrifuge tube, add 100 mg of graphitized carbon black, shake on a vortex mixing oscillator at a rate of 2200 r / min for 3 minutes, and take the supernatant to constant volume after standing to obtain an extract.

[0073] The content of hymexazol in the flue...

Embodiment 3

[0077] Example 3: Detection of Hymexazol Pesticide Residues in Oriented Tobacco Samples

[0078] (1) Weigh about 3g of oriental tobacco sample into a 50mL capped centrifuge tube, add 12.5mL of sodium hydroxide aqueous solution with a pH value of 9, shake until the sample is fully infiltrated by water, and let stand for 7.5min. Add 12 mL of ethyl acetate to the centrifuge tube, place it on a vortex mixer and vibrate at a speed of 2400 r / min for 3 min to obtain the primary extract;

[0079] (2) Add 6g of magnesium sulfate, 1g of sodium acetate and 0.12g of 100v.% acetic acid to the primary extract, immediately vibrate on a vortex mixer at a speed of 2300r / min for 4min, and let stand.

[0080] After standing still, pipette the supernatant into a centrifuge tube, add 200 mg of graphitized carbon black, shake on a vortex mixing oscillator at a rate of 2500 r / min for 5 min, and after standing still, take the supernatant to constant volume to obtain an extract.

[0081] The hymexa...

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Abstract

The invention belongs to the field of detection of pesticide residues and relates to a method for extracting and purifying hymexazol pesticide residues in a tobacco sample, a method for detecting hymexazol pesticide residues and a composition or a kit for extracting and purifying hymexazol or detecting hymexazol. Specifically, the method for extracting and purifying the hymexazol pesticide residues in the tobacco sample comprises the following steps: (1) soaking the tobacco sample in an alkaline solution, adding ethyl acetate and oscillating to obtain a primary extraction solution; and (2) mixing the obtained primary extraction solution with any one of reagent groups A-C, standing the mixture, and extracting a supernatant solution 1, wherein the reagent group A comprises magnesium sulfate and sodium chloride, the reagent group B comprises magnesium sulfate, sodium chloride, sodium citrate and disodium hydrogen citrate sesquihydrate, and the reagent group C comprises magnesium sulfate, sodium acetate trihydrate and acetic acid. The method for extracting and purifying the hymexazol pesticide residues in the tobacco sample is high in hymexazol extraction rate, small in pollution and low in cost.

Description

technical field [0001] The invention belongs to the technical field of extraction and detection of pesticide residues, and relates to a method for extracting and purifying hymexazol pesticide residues in tobacco and a used composition. The invention also relates to a method for detecting hymexazol pesticide residues in tobacco. 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] The bactericidal mechanism of hymexazol is: after application, hymexazol is absorbed by the soil and combined with metal ions in the soil to form a substance tha...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/06G01N30/88
Inventor 张建平邓其馨吴清辉谢卫黄朝章刘泽春周培琛李巧灵方钲中
Owner CHINA TOBACCO FUJIAN IND
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