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Method for determining SYP-9080 residue in fruits and vegetables by employing gas chromatography-electron impact ion source-mass spectrum (GC-EI-MS)

A GC-EI-MS, tetrachlorantraniliprole technology, applied in the field of tetrachlorantraniliprole residues, to achieve the effect of ensuring people's food safety, avoiding matrix interference, and good repeatability

Active Publication Date: 2015-04-29
INSPECTION & QUARANTINE TECH CENT SHANDONG ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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Problems solved by technology

[0005] So far, there are no domestic and foreign reports on the detection method of tetrachlorantraniliprole residues in food and agricultural products. Gas chromatography-mass spectrometry (GC-EI-MS) equipped with an electron bombardment ionization source has great advantages in the analysis of pesticide residues in food and agricultural products. Since the electron bombardment ionization source mass spectrometer is a universal detector, it can realize multi-residue analysis of hundreds of pesticides, can be qualitative and quantitative at the same time, and the price is moderate. Therefore, various testing institutions and enterprises are equipped with gas chromatography-electron bombardment ion source- Mass spectrometry (GC-EI-MS) detects pesticide residues in food and agricultural products. Therefore, gas chromatography-electron bombardment ion source-mass spectrometry (GC-EI-MS) is established to qualitatively and quantitatively analyze tetrachlorantraniliprole in vegetables and fruits. The detection method of residue is of great significance

Method used

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  • Method for determining SYP-9080 residue in fruits and vegetables by employing gas chromatography-electron impact ion source-mass spectrum (GC-EI-MS)
  • Method for determining SYP-9080 residue in fruits and vegetables by employing gas chromatography-electron impact ion source-mass spectrum (GC-EI-MS)
  • Method for determining SYP-9080 residue in fruits and vegetables by employing gas chromatography-electron impact ion source-mass spectrum (GC-EI-MS)

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Example 1: Detection of Tetrachlorantraniliprole residues in apples

[0033] (1) Sample pretreatment

[0034] Weigh 10.0 g of well-mixed apples 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 4mL of supernatant in a nitrogen blowpipe, dry it with nitrogen at 40°C, add 1mL of acetone / n-hexane mixed solvent with a volume ratio of 1 / 1 to dissolve the residue, vortex and mix evenly to pass through the membrane, then transfer it to an injection bottle for GC - EI-MS determination.

[0035] (2) Preparation of standard working solution

[0036] Accurately weigh 25±0.1...

Embodiment 2

[0061] Example 2: Detection of Tetrachlorantraniliprole residues in dehydrated green peppers

[0062] (1) Sample pretreatment

[0063] Weigh 2.0 g of fully mixed dehydrated green peppers into a 50 mL centrifuge tube, add 5 mL of water for resuscitation for 30 min, accurately add 20 mL of acetonitrile solution containing 1% acetic acid, extract homogeneously for 1 min, add 3 g of anhydrous magnesium sulfate, 2 g of sodium acetate and 2mL of water, vortexed for 1min, centrifuged at 7000r / min 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 an injection bottle for GC-EI - MS determin...

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Abstract

The invention discloses a method for determining a SYP-9080 residue in fruits and vegetables by employing gas chromatography-electron impact ion source-mass spectrum (GC-EI-MS). The method comprises the following steps: extracting residual SYP-9080 from a sample with acetonitrile or an acetonitrile solution containing 1% acetic acid in a manner of homogenization; dispersing and purifying extract liquid with ethidene diamine-N-propyl silane (PSA) and octadecyl silane bonded-phase (C18) matrix, and then carrying out GC-EI-MS detection; and building a corrected standard curve with a blank matrix solution free of a to-be-detected pesticide, and quantifying by an external standard method. According to the method, the average recovery rate is 86.3%-93.2%; the relative average standard deviation (RSD) is 4.2%-7.6%; the detection limit is lower than 7.85 microg / kg; and the method has the advantages of simplicity, convenience and fastness in operation, high sensitivity, good repeatability and accurate qualify and quantify, and can meet the technical requirements of uniform standard of 0.01mg / kg of residue limit; and a powerful technical support is provided for guarantee of the food safety for people in China and health development of foreign export trade.

Description

technical field [0001] The present invention relates to a kind of method of GC-EI-MS determination tetrachlorantraniliprole residue in fruits and vegetables, more specifically adopts gas chromatography-electron bombardment ion source-mass spectrometry (GC-EI-MS) to qualitatively and quantitatively determine the residues in vegetables and fruits The method for the content of residual tetraclotraniliprole belongs to the technical field of determination of pesticide residues. Background technique [0002] Bisamide insecticides are popular insecticide products in the world in recent years. They can be widely used in the pest control of rice, vegetables, cotton and other crops. They have the advantages of low toxicity, environmental safety and high activity, including chlorantraniliprole , cyantraniliprole, flubendiamide and other varieties, tetrachlorantraniliprole (SYP-9080) is a new product developed by Shenyang Research Institute of Chemical Industry, a subsidiary of Sinochem ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
Inventor 崔淑华程刚赵峰刘润珠
Owner INSPECTION & QUARANTINE TECH CENT SHANDONG ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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