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A method for determination of cyantraniliprole residues in fruits and vegetables by gc-nci-ms

A GC-NCI-MS, cyantraniliprole technology, applied in the field of cyantraniliprole residues, can solve problems such as low anti-interference ability and low sensitivity, and achieve the effects of avoiding matrix interference, good repeatability and high sensitivity

Active Publication Date: 2015-11-18
崔淑华
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Now various testing institutions and enterprises have purchased gas chromatography-mass spectrometers (GC-MS), and are generally equipped with negative chemical ion sources (NCI). Now many types of pesticides contain electronegative groups, organochlorines and pseudo Pyrethrin pesticide molecules mostly contain strong electronegative groups such as -F, -Cl, -Br or -COO-; organophosphorus pesticide molecules mostly contain =S, -OR, -P, -O-, -Cl, or -P=O and other electronegative groups; and most of the new pesticides developed in recent years contain -F groups. Therefore, the use of GC-NCI-MS can facilitate the multi-residue analysis of various pesticides. Compared with MS, it can obtain better anti-interference ability, lower sensitivity and better selectivity. Cytraniliprole is an electronegative compound, but so far no GC- The report of the NCI-MS detection method, therefore, it is of great significance to establish a gas chromatography-negative chemical ion source-mass spectrometry (GC-NCI-MS) detection method for the qualitative and quantitative analysis of cyantraniliprole residues in vegetables and fruits

Method used

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  • A method for determination of cyantraniliprole residues in fruits and vegetables by gc-nci-ms
  • A method for determination of cyantraniliprole residues in fruits and vegetables by gc-nci-ms
  • A method for determination of cyantraniliprole residues in fruits and vegetables by gc-nci-ms

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Example 1: Detection of cyantraniliprole residues in oranges

[0038] (1) Sample pretreatment

[0039] Weigh 10.0 g of well-mixed oranges into a 50 mL centrifuge tube, accurately add 20 mL of acetonitrile, extract homogeneously for 1 min, add 3 g of anhydrous magnesium sulfate and 2 g of sodium chloride, vortex for 1 min, and centrifuge at 7000 r / min for 5 min. After centrifugation, take 6mL of acetonitrile extract and transfer to a solution containing 900mg anhydrous magnesium sulfate, 300mgC 18 and 150mgPSA in a centrifuge tube, vortex for 1min, and centrifuge at 5000r / min for 5min. Take 4 mL of the supernatant in a nitrogen blowpipe, dry it with nitrogen at 40°C, add acetone / n-hexane mixed solvent with a volume ratio of 1 / 1 to dissolve the residue, vortex and mix evenly, pass through the membrane, and transfer it to the sample bottle for GC- NCI-MS assay.

[0040] (2) Preparation of standard working solution

[0041] Accurately weigh 25±0.1mg of the standard prod...

Embodiment 2

[0066] Example 2: Detection of cyantraniliprole residues in cabbage

[0067] (1) Sample pretreatment

[0068] Weigh 10.0 g of well-mixed cabbage into a 50 mL centrifuge tube, accurately add 20 mL of acetonitrile solution containing 1% acetic acid, extract homogeneously for 1 min, add 3 g of anhydrous magnesium sulfate and 2 g of sodium acetate, vortex for 1 min, and set the temperature at 7000 r / min Centrifuge for 5min. After centrifugation, take 6mL of acetonitrile extract and transfer to a solution containing 900mg anhydrous magnesium sulfate, 300mgC 18 and 150mgPSA in a centrifuge tube, vortex for 1min, and centrifuge at 5000r / min for 5min. After centrifugation, take 6mL of acetonitrile extract and transfer to a solution containing 900mg anhydrous magnesium sulfate, 300mgC 18 and 150mgPSA in a centrifuge tube, vortex for 1min, and centrifuge at 5000r / min for 5min. Take 4mL of the supernatant in a nitrogen blowpipe, dry it with nitrogen at 40°C, add acetone / n-hexane mixe...

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Abstract

The invention discloses a GC-NCI-MS (Gas Chromatography-Negative Chemical Ionization-Mass Spectrum) detecting method for the residual quantity of cyantraniliprole in fruits and vegetables. The GC-NCI-MS detecting method comprises the steps of homogenizing by using acetonitrile or an acetonitrile liquid containing 1% acetic acid to extract residual cyantraniliprole in a sample; dispersing by using a primary secondary amine (PSA) and octadecylsilane bonded-phase (C18) matrix to purify an extracting liquid; then, carrying out GC-NCI-MS detection; establishing a corrected standard curve by using a blank matrix liquid without a pesticide to be detected; and quantifying by using an external standard method. By using the GC-NCI-MS detecting method, the average recovery rate is 89.2-96.7%, the average relative standard deviation (RSD) is 3.5-8.8%, and the detection limit is lower than 0.53mu g / kg; and the GC-NCI-MS detecting method is simple and convenient to operate, rapid, high in sensitivity, good in repeatability and accurate in qualitation and quantitation. According to the GC-NCI-MS detecting method, the technical requirements of America, Canada, European union, Japan and other countries on security detection of corresponding products can be met, and the powerful technical support can be provided for ensuring Chinese food safety and the health development of foreign export trade.

Description

technical field [0001] The present invention relates to a kind of method of GC-NCI-MS determination cyantraniliprole residue in fruits and vegetables, more specifically adopt gas chromatography-negative chemical ion source-mass spectrometry (GC-NCI-MS) to qualitatively and quantitatively measure residues in vegetables and fruits The method for the content of cyantraniliprole belongs to the technical field of determination of pesticide residues. Background technique [0002] Cyantraniliprole, also known as cyantraniliprole (cyantraniliprole), is a second-generation ryanodine receptor inhibitor insecticide successfully developed by DuPont after chlorantraniliprole. Formed from various polar groups on the benzene ring, compared with chlorantraniliprole, it has a wider spectrum of insecticidal activity, excellent control effect on piercing-sucking pests, and has better systemic properties , the market prospect is broad. The chemical name is 3-bromo-1-(3-chloro-2-pyridyl)-{4-cya...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02
Inventor 崔淑华李瑞娟马惠贝峰
Owner 崔淑华
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