Detecting method for residual quantity of flubendiamide in fruits and vegetables

The invention relates to a technology for the determination of flubendiamide and a determination method, which is applied in the field of determination of flubendiamide residues, can solve problems such as low sensitivity of anti-interference ability, and achieve the effect of avoiding matrix interference, ensuring people's food safety, and having good repeatability.

Active Publication Date: 2015-04-08
云南通标检测有限公司
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  • 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. Flubendiamide is an electronegative compound. GC-NCI-MS detection method is reported, 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 flubendiamide residues in vegetables and fruits

Method used

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  • Detecting method for residual quantity of flubendiamide in fruits and vegetables
  • Detecting method for residual quantity of flubendiamide in fruits and vegetables
  • Detecting method for residual quantity of flubendiamide in fruits and vegetables

Examples

Experimental program
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Effect test

Embodiment 1

[0035] Example 1: Detection of flubendiamide residues in grapes

[0036] (1) Sample pretreatment

[0037] Weigh 10.0 g of fully mixed grapes into a 50 mL centrifuge tube, accurately add 20 mL of acetonitrile, homogeneously extract 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, 300mg C 18 and 150mg PSA 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.

[0038] (2) Preparation of standard working solution

[0039] Accurately weigh 25±0.1mg of the standard produc...

Embodiment 2

[0064] Example 2: Detection of flubendiamide residues in Chinese cabbage

[0065] (1) Sample pretreatment

[0066] Weigh 10.0g of well-mixed cabbage into a 50mL centrifuge tube, accurately add 20mL of acetonitrile solution containing 1% acetic acid, extract homogeneously for 1min, add 3g of anhydrous magnesium sulfate and 2g of sodium acetate, vortex for 1min, and then 7000r / min Centrifuge for 5min. After centrifugation, take 6mL of acetonitrile extract and transfer to a solution containing 900mg anhydrous magnesium sulfate, 300mg C 18 and 150mg PSA 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 mixed solvent with a volume ratio of 1 / 1 to dissolve the residue, vortex and mix well, then transfer it to the sample bottle to wait for GC-NCI - MS determination.

[0067] (2) Preparation of standard working solution

[0068] Dilute the 10μg / mL stan...

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Abstract

The invention discloses a detecting method for the residual quantity of flubendiamide in fruits and vegetables. The detecting method comprises the steps of homogenizing by using acetonitrile or an acetonitrile liquid containing 1% acetic acid to extract residual flubendiamide 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 gas chromatography-negative chemical ionization-mass spectrum (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 detecting method, the average recovery rate is 93.2-103.1%, the average relative standard deviation (RSD) is 4.6-7.4%, and the detection limit is lower than 1.15mu g/kg; and the detecting method is simple and convenient to operate, rapid, high in sensitivity, good in repeatability and accurate in qualitation and quantitation. According to the detecting method, the technical requirements of America, Japan, European union 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 invention relates to a method for determining the residual amount of flubendiamide in vegetables and fruits, more specifically, it uses gas chromatography-negative chemical ion source-mass spectrometry (GC-NCI-MS) to qualitatively and quantitatively determine the residual amount of flubendiamide in vegetables and fruits. A method for flubendiamide content belongs to the technical field of pesticide residue determination. Background technique [0002] Flubendiamide (Flubendiamide), trade name Longge, is a new type of phthalamide insecticide developed by Japanese pesticide company (known as Co., Ltd.), which has good activity against almost all lepidopteran pests , not only has excellent activity on both adults and larvae, but also has a fast acting speed and a long lasting effect. The effect on rice stem borer and leaf roller is absolutely top-notch. The toxicity to bees is very low, and the toxicity to carp (a representative of aquatic organisms)...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
Inventor 郭庆龙许美玲张丽杨娟
Owner 云南通标检测有限公司
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