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Method for determination of flumethrin in garlic or garlic product

A technology of flufenthrin and a determination method, which is applied in the field of determination of pesticide residues in food, and can solve problems such as no literature report in detection.

Inactive Publication Date: 2013-12-11
JINAN CUSTOMS TECH CENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are also many detection methods, such as gas chromatography [9-12] , liquid chromatography [13] and gas chromatography-mass spectrometry [14-15] , but the detection in agricultural products and garlic and its products has not been reported in the literature

Method used

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  • Method for determination of flumethrin in garlic or garlic product
  • Method for determination of flumethrin in garlic or garlic product
  • Method for determination of flumethrin in garlic or garlic product

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0071] 1.1 Extraction

[0072] Weigh about 20.00g (accurate to 0.01g) fresh garlic sample, add 200uL of 1.0ug / mL bifenthrin standard solution, put it in a 150mL conical flask, microwave in a microwave oven at 640w for 50s, cut it into pieces, and add it accurately 50.0mL n-hexane: dichloromethane (1+1), 18000r / min homogeneous extraction for 3min. The sample liquid is filtered into a colorimetric tube with 5-10gNaCl in advance, covered with a stopper, vigorously shaken for 1min, and left standing for 30min , after the organic phase and the aqueous phase were separated, accurately pipette 25mL of the organic phase into a 25mL colorimetric tube, blow it in a 50°C water bath with nitrogen to nearly dry, dissolve the residue with 2.0mL of n-hexane, and wait for purification.

[0073] 2.3.2 Purification

[0074] Pre-wash the amino column with 3.0mL acetone and 5mL n-hexane in sequence (conditioning). When the solvent level reaches the surface of the column adsorption layer, immedia...

Embodiment 2

[0080] Weigh about 20.00g (accurate to 0.01g) of salted garlic, add 200uL of 1.0ug / mL bifenthrin standard solution, place it in a 150mL conical flask, and accurately add 50.0mL of n-hexane: dichloromethane (1+ 1), 18000r / min homogeneous extraction for 3min. The sample solution was filtered into a colorimetric tube with 5-10gNaCl in advance, covered with a stopper, shaken vigorously for 1min, and allowed to stand for 30min. After the organic phase and the aqueous phase were separated, accurate Pipette 25mL of the organic phase into a 25mL colorimetric tube, blow with nitrogen in a water bath at 50°C until nearly dry, dissolve the residue with 2.0mL of n-hexane, and wait for purification.

[0081] 2.3.2 Purification

[0082]Pre-wash the amino column with 3.0mL acetone and 5mL n-hexane in sequence. When the solvent level reaches the surface of the column adsorption layer, immediately pour the above-mentioned solution to be purified, use a 10mL pointed centrifuge tube to receive t...

Embodiment 3

[0088] Weigh about 20.00g (accurate to 0.01g) mashed garlic, add 200uL of 1.0ug / mL bifenthrin standard solution, put it in a 150mL conical flask, add 50.0mL n-hexane: dichloromethane (1+1) accurately , 18000r / min homogeneous extraction for 3min. The sample solution was filtered into a colorimetric tube with 5-10gNaCl in advance, covered with a stopper, shaken vigorously for 1min, and allowed to stand for 30min. After the organic and aqueous phases were separated, pipette accurately Put 25mL of organic phase in a 25mL colorimetric tube, blow with nitrogen gas in a 50°C water bath until nearly dry, dissolve the residue with 2.0mL of n-hexane, and wait for purification.

[0089] 2.3.2 Purification

[0090] Pre-wash the amino column with 3.0mL acetone and 5mL n-hexane in sequence. When the solvent level reaches the surface of the column adsorption layer, immediately pour the above-mentioned solution to be purified, use a 10mL pointed centrifuge tube to receive the eluate, and use ...

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Abstract

The invention provides a method for determination of flumethrin in garlic or a garlic product. The method comprises the following steps of 1, extraction comprising carrying out homogenization and / or centrifugation treatment on garlic or a garlic product by a normal hexane-dichloromethane mixture having a volume ratio of 1: 1, blow-drying an organic phase by nitrogen, and dissolving residues in normal hexane to obtain a solution needing to by purified, 2, purification comprising carrying out conditioning of an amino column, pouring the solution needing to by purified into the amino column, receiving an eluent, carrying out elution by a normal hexane-dichloromethane mixture having a volume ratio of 1: 1 to obtain a purified solution, blow-drying the purified solution by nitrogen, dissolving residues in an acetone-normal hexane mixture having a volume ratio of 10: 90, and filtering by a filter membrane having a aperture size of 0.22 microns, and 3, detection comprising determining flumethrin in the purified solution prepared from garlic or the garlic product by a gas chromatography or a gas chromatography / tandem mass spectrometry. The method adopts a gas chromatography or a tandem mass spectrometry. The method can be operated simply, has high sensitivity and good repeatability and can be widely used for residual detection of flumethrin in garlic or a garlic product.

Description

technical field [0001] The invention relates to a method for determining pesticide residues in food, in particular to a method for determining bifenthrin in garlic or its products. Background technique [0002] Bifenthrin is a synthetic pyrethroid ectoparasiticide. At present, the drug has been widely used as an acaricide in the process of bee rearing [1] , and pesticides in agriculture. However, the residues of such pesticides in honey and agricultural products will cause certain harm to the human body, which has aroused widespread concern. There are many literatures on the detection of bifenthrin residues in bee products (such as honey, royal jelly and bee pollen) at home and abroad. [2-5] and standard [6-8] . There are also many detection methods, such as gas chromatography [9-12] , liquid chromatography [13] and gas chromatography-mass spectrometry [14-15] , but the detection in agricultural products and garlic and its products has not been reported in the litera...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/06G01N30/88
Inventor 包海英高尧华李建勇李晓明王飞夏芳刘友清
Owner JINAN CUSTOMS TECH CENT
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