Method for simultaneously detecting residual quantities of oxamyl and oxamyl oxime in vegetable/fruits

A kind of technology of Xanthicarb and Xanthicarb, which is applied to the detection of Xanthicarb and its metabolite Xanthicarb residues in fruits, and in the detection field of vegetables, pesticides and their metabolite residues at the same time, can solve the problem of unsolved problems. Issues such as the detection method of Xanthicarb metabolites were mentioned to achieve the effect of ensuring people's food safety, easy operation and high sensitivity

Inactive Publication Date: 2016-05-04
INST OF PLANT PROTECTION SHANDONG ACAD OF AGRI SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These two standards only have the detection method of Xanthicarb, but do not mention the detection method of Xanthicarb metabolite Xanthicarb oxime

Method used

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  • Method for simultaneously detecting residual quantities of oxamyl and oxamyl oxime in vegetable/fruits
  • Method for simultaneously detecting residual quantities of oxamyl and oxamyl oxime in vegetable/fruits
  • Method for simultaneously detecting residual quantities of oxamyl and oxamyl oxime in vegetable/fruits

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] Example 1 Detection of the residual amount of saxacarb and saxacarb in pepper

[0043] (1) Sample pretreatment: Take the pepper sample to be tested, cut into small pieces about 1cm in length, and mix thoroughly; weigh 10.0 g of the processed pepper sample, add 10mL acetonitrile, homogenize for 1min, add 5g sodium chloride, Homogenize again for 1min, centrifuge at 3800r / min for 5min; take 6mL of supernatant, transfer to a 15mL centrifuge tube containing 0.6gPSA, 0.3gC18 and 0.06gGCB, vortex at 3000r / min for 1min, centrifuge at 5000r / min at 4℃ for 5min, Take 5mL of the supernatant and put it in a 10mL centrifuge tube, dry it with nitrogen at 40℃, add 1mL of mobile phase to dissolve the residue, mix well, pass through a 0.22μm filter membrane to obtain a sample solution, transfer it to a sample bottle for HPLC-MS / MS determination .

[0044] (2) Preparation of matrix standard working solution:

[0045] Preparation of matrix standard working solution: accurately weigh 50±0.1mg of...

Embodiment 2

[0065] Example 2 Detection of the residual amount of oxaprocarb and oxaprocarb in apples

[0066] (1) Sample pretreatment: Take the apple sample to be tested, cut into small pieces of about 1 cm in length, width and height, and mix them thoroughly. Weigh 10.0 g of the processed apple sample, add 5 mL of distilled water, add 10 mL of acetonitrile, homogenize for 1 min, add 5 g of sodium chloride, homogenize again for 1 min, centrifuge at 3800 r / min for 5 min; take 6 mL of the supernatant, and transfer to 0.6 In a 15mL centrifuge tube containing gPSA, 0.3gC18 and 0.06gGCB, vortex at 3000r / min for 1min, centrifuge at 5000r / min at 4℃ for 5min, take 5mL of the supernatant in a 10mL centrifuge tube, dry with nitrogen at 40℃, and add 1mL of mobile phase Dissolve the residue, mix well, and pass through a 0.22μm filter membrane to obtain a sample solution, which is transferred to a sample bottle for HPLC-MS / MS determination.

[0067] (2) Preparation of standard working solution:

[0068] Pr...

Embodiment 3

[0082] Example 3 Detection of the residual amount of oxacarb and oxacarb in rape and grape

[0083] Take the rapeseed and grape samples to be tested, cut the rapeseed into small pieces about 1cm in length, and cut the grapes into small pieces about 1cm in length, width and height, and mix them thoroughly. Weigh 10.0 g of the processed sample, add 10 mL of acetonitrile, homogenize for 1 min, add 5 g of sodium chloride, homogenize again for 1 min, centrifuge at 3800 r / min for 5 min; take 6 mL of the supernatant, and transfer to 0.6g PSA, 0.3g C18 and In a 15mL centrifuge tube with 0.06gGCB, vortex at 3000r / min for 1min, centrifuge at 5000r / min at 4℃ for 5min, take 5mL of the supernatant in a 10mL centrifuge tube, dry with nitrogen at 40℃, add 1mL of mobile phase to dissolve the residue, and mix well After passing through a 0.22 μm filter membrane, the sample solution was obtained, and transferred to a sample bottle for HPLC-MS / MS determination (the detection method is the same as i...

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Abstract

The invention discloses a method for simultaneously detecting residual quantities of oxamyl and oxamyl oxime in vegetable/fruits. The method comprises the following steps: (1) extraction: vegetable/fruit samples to be detected are taken, acetonitrile and NaCl are added, and homogenizing and centrifugation are carried out; (2) purification: an upper layer acetonitrile phase is taken and placed in a centrifuge tube containing a matrix solid-phase dispersion extractant, centrifugation is carried out, supernatant is taken, drying is carried out with nitrogen, volumetric flask preparation is carried out for a mobile phase, a 0.22[mu]m organic filter membrane is used for filtering, and a sample liquid is obtained; (3) determination and result calculation: HPLC-MS/MS is used for detecting the sample liquid, chromatographic peak area of oxamyl or oxamyl oxime is detected, the value is substituted into a standard curve, and content of oxamyl or oxamyl oxime in the sample liquid is obtained by calculation. The solid-phase dispersion extraction technology is used, the simple and rapid pre-treatment method is established, and detection limits of oxamyl and oxamyl oxime are 0.002mg/kg and 0.001 mg/kg respectively; the method has the advantages of simple operation, fast speed, accuracy, high sensitivity, and good repeatability.

Description

Technical field [0001] The invention relates to a detection method for pesticides and their metabolite residues, in particular to a detection method for simultaneously detecting the residues of sacprocarb and the metabolite sacprocarb in vegetables and fruits, belonging to the technical field of pesticide residues determination . Background technique [0002] Saxacarb is a carbamate nematicide, acaricide and insecticide. Its common name is OXAMYL and its chemical name is N,N-dimethyl-2-methylcarbamoyl oxoimide-2. -Methylthioacetamide. The insecticidal mechanism is to achieve the purpose of prevention and control by inhibiting the activity of acetylcholinesterase. The medicine can control thrips, aphids, potato ladybugs, mites, etc. It is widely used in citrus, cotton, soybeans, tobacco, fruit trees, vegetables and some ornamental crops. The drug is a broad-spectrum nematocide, which can be treated with foliar or soil. It can be absorbed and transmitted in plants, and it can al...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88
CPCG01N30/88
Inventor 于建垒李瑞娟宋国春刘同金戴争
Owner INST OF PLANT PROTECTION SHANDONG ACAD OF AGRI SCI
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