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Method for detecting residual amount of abamectin in tobacco

A technology of abamectin and detection method, which is applied in the detection field to achieve the effects of good reproducibility, high sensitivity and accuracy

Active Publication Date: 2014-06-04
YUNNAN ACAD OF TOBACCO AGRI SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, the international requirements for the maximum residue limit (MRL) of abamectin are very strict, and the detection of its residue is very important. At present, there is no detection method for abamectin pesticide residues in tobacco at home and abroad.

Method used

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  • Method for detecting residual amount of abamectin in tobacco
  • Method for detecting residual amount of abamectin in tobacco
  • Method for detecting residual amount of abamectin in tobacco

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Accurately weigh 4.0 g of No. 1 tobacco leaf sample, place it in a 40ml plastic centrifuge tube, add 0.04μg of abamectin pesticide standard, add 8ml of acetonitrile, shake for 2min, add 4.0g of anhydrous sodium sulfate, vortex for 2min, and centrifuge for 8min , the residue was extracted once more with 8ml of acetonitrile, and the supernatant was combined; take a small column of basic alumina, add 3g of anhydrous sodium sulfate, and add 8mL of acetonitrile for pre-leaching, pass the supernatant through the column, and collect the filtrate into a concentrated bottle , then eluted with 8mL of acetonitrile, collected in the same concentrating bottle, and the filtrate in the concentrating bottle was evaporated to dryness at 30°C, then 0.5ml of acetonitrile was added, placed on an ultrasonic wave for 1min to fully dissolve, and 0.5ml was placed in Put it in a brown bottle for later use; under the condition of avoiding light and room temperature, take the above brown bottle an...

Embodiment 2

[0037] Accurately weigh 6.0 g of No. 2 tobacco leaf sample, put it in a 60ml glass centrifuge tube, add 0.06μg of abamectin pesticide standard, add 12ml of methanol, shake for 4min, add 6.0g of anhydrous magnesium sulfate, ultrasonically shake for 4min, and centrifuge for 12min , the residue was repeatedly extracted twice with 12ml of methanol, and the supernatant was combined; take a C18 small column, add 5g of anhydrous sodium sulfate, and add 12mL of methanol for pre-leaching, pass the supernatant through the column, collect the filtrate into a concentrated bottle, and then Elute with 12mL of methanol and collect in the same concentrated bottle. Rotate the filter in the concentrated bottle to dryness at 50°C, then add 1.5ml of acetonitrile, place it on an ultrasonic wave for 3 minutes to fully dissolve, take 1ml and put it in a brown bottle Standby; under the condition of avoiding light and room temperature, take the above brown bottle and add 0.2mL methylimidazole-acetonitr...

Embodiment 3

[0039] Accurately weigh 5.0 g of No. 3 tobacco leaf sample, add 0.05 μg of avermectin pesticide standard substance, place in a 50ml glass or plastic centrifuge tube, add 10ml of dichloromethane, vortex for 3min, add 5.0g of anhydrous magnesium sulfate, shake 3min, centrifuged for 10min, the residue was extracted once more with 10ml of dichloromethane, and the supernatant was combined; take a silica gel column, add 4g of anhydrous sodium sulfate, and add 10mL of acetone for pre-drenching, pass the supernatant through the column, and collect the filtrate into the concentrated bottle, then eluted with 10mL of acetone, collected in the same concentrated bottle, and the filtrate in the concentrated bottle was evaporated to dryness at 40°C, then 1ml of acetonitrile was added, placed on an ultrasonic wave for 2min to fully dissolve, and 0.8 ml is placed in a brown bottle for later use; under the condition of avoiding light and room temperature, take the above brown bottle and add 0.15...

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Abstract

The invention discloses a method for detecting a residual amount of abamectin in tobaccos. The method comprises steps of extraction, purification, derivatization and detection and specifically comprises the following steps of: accurately weighing a tobacco sample into a centrifugating pipe, adding acetonitrile, oscillating, adding anhydrous sodium sulfate, oscillating again, centrifuging, repeatedly extracting the residues by the acetonitrile, and combining supernate; filtering the supernate through an alkaline aluminium oxide small column, collecting a filtrate into a concentration bottle, diluting by using an organic solvent, evaporating the filtrate in a rotatable manner until the filtrate is dried, adding the organic solvent, putting the mixture under ultrasonics, performing ultrasonic treatment, fully dissolving the organic solvent, and putting 0.5 to 2ml of the solution into a brown bottle; and under a condition of a shaded and room temperature environment, adding a derivatization reagent into the brown bottle for mixing and spinning, after reaction is finished, adding methyl alcohol, stewing, filtering the action solution by a filter membrane, and injecting the solution into a high performance liquid chromatograph for quantitative analysis and calculation to obtain the residual amount of the abamectin. The method is high in sensitivity, accuracy and reproducibility and is suitable for analysis of the trace residual amount of the abamectin in the tobaccos.

Description

technical field [0001] The invention belongs to the technical field of detection, and in particular relates to a method for detecting residual abamectin in tobacco. Background technique [0002] Avermectin (AVM for short) is a macrolide antibiotic isolated from the fermentation product of Streptomyces avermitilis. It has strong insecticidal activity and wide insecticidal spectrum, and is widely used in the production of vegetables, fruit trees, rice, tobacco and other crops. [0003] Although avermectin belongs to the microbial source pesticide, its effect on LD in rats 50 It is 10mg / kg, which is a highly toxic pesticide. Therefore, the international requirements for the maximum residue limit (MRL) of abamectin are very strict, and the detection of its residue is very important. At present, there is no detection method for abamectin pesticide residues in tobacco at home and abroad. In recent years, with the increasing use of abamectin and emamectin emamectin in tobacco pr...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/06
Inventor 师君丽逄涛孔光辉李勇刘彦红
Owner YUNNAN ACAD OF TOBACCO AGRI SCI
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