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GC-NCI-MS (gas chromatography-negative chemical ionization-mass spectrometry) determination method of residual amount of tetrachlorantraniliprole

A technology of GC-NCI-MS and tetrachlorantraniliprole is applied in the field of GC-NCI-MS determination of tetrachlorantraniliprole residues, and achieves the effects of simple operation, high sensitivity and avoiding matrix interference.

Active Publication Date: 2015-04-22
INSPECTION & QUARANTINE TECH CENT SHANDONG ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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-NCI-MS) equipped with a negative chemical ionization source has great advantages in the analysis of pesticide residues in food and agricultural products. Negative chemical ion source (NCI source) is called the "soft ionization source" of mass spectrometry. It has high selectivity and high sensitivity for analytes containing electronegative groups. Due to its strong characteristics, matrix interference Rarely, the qualitative and quantitative analysis of the target can be carried out very accurately

Method used

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  • GC-NCI-MS (gas chromatography-negative chemical ionization-mass spectrometry) determination method of residual amount of tetrachlorantraniliprole
  • GC-NCI-MS (gas chromatography-negative chemical ionization-mass spectrometry) determination method of residual amount of tetrachlorantraniliprole
  • GC-NCI-MS (gas chromatography-negative chemical ionization-mass spectrometry) determination method of residual amount of tetrachlorantraniliprole

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Example 1: Detection of Tetrachlorantraniliprole residues in rice

[0034] (1) Sample pretreatment

[0035] extract

[0036] Weigh 5g of rice sample that has been thoroughly mixed into a 50mL centrifuge tube, add 5mL of water to mix, let it stand for 30min, add 20mL of acetonitrile accurately, extract homogeneously for 2min, add 3g of anhydrous magnesium sulfate and 2g of sodium chloride, and vortex for 1min , 7000r / min centrifugal 5min. After centrifugation, take 8 mL of the acetonitrile extract at 40°C for rotary steaming or nitrogen blowing to about 1 mL for purification.

[0037] purify

[0038] Pre-wash C with 5 mL of acetonitrile 18 / PSA solid phase extraction column, when the liquid level reaches the top of the adsorbent, transfer the above extraction solution into the column, wash the test tube with 2mL acetonitrile, and transfer the washing liquid into the SPE column, when the solution reaches the top of the adsorbent, add Add 4mL of acetonitrile to the col...

Embodiment 2

[0064] Example 2: Detection of Tetrachlorantraniliprole residues in pork

[0065] (1) Sample pretreatment

[0066] extract

[0067] Weigh 5g of pork sample (ground into flour) that has been thoroughly mixed into a 50mL centrifuge tube, add 20mL of water to resuscitate for 30min, then accurately add 20mL of acetonitrile solution containing 1% acetic acid, shake and extract for 20min, ultrasonically extract for 5min, add 3g of anhydrous Magnesium sulfate and 2g sodium acetate, after vortexing for 1min, centrifuge at 7000r / min for 5min. After centrifugation, take 8 mL of acetonitrile extract and rotate it at 40 °C or blow it with nitrogen until it is nearly dry, add 1 mL of acetonitrile and vortex it, and wait for purification.

[0068] purify

[0069] Pre-wash C with 5 mL of acetonitrile 18 / PSA solid phase extraction column, when the liquid level reaches the top of the adsorbent, transfer the above extraction solution into the column, wash the test tube with 2mL acetonitril...

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Abstract

The invention discloses a GC-NCI-MS (gas chromatography-negative chemical ionization-mass spectrometry) determination method of residual amount of tetrachlorantraniliprole. The method is mainly used for determining the residual amount of tetrachlorantraniliprole in cereal grains, animal-derived foods and other complex matrix food agricultural products. The method comprises the following steps: homogenizing and extracting residual tetrachlorantraniliprole in a sample with acetonitrile or an acetonitrile solution containing 1% of acetic acid, performing purification and concentration by a C18 / PSA solid-phase extraction column, performing GC-NCI-MS detection, adopting a blank matrix solution without a pesticide to be detected to establish a standard curve for correction, and quantifying by an external standard method. According to the method, the average recovery rate is 83.3%-90.3%, the average relative standard deviation (RSD) is 3.5%-6.9%, and the detection limit is lower than 1.43mu g / kg; and the method has the advantages of simplicity in operation, high speed, good impurity removal effect, high sensitivity, strong characteristic feature, good repeatability and accurate quantitative and qualitative properties. According to the method, the technical requirement of 'being standard without exceptions' of the residual limit of 0.01mg / kg can be met, and the powerful technical support is provided for ensuring food safety of people in China and health development of export trades.

Description

technical field [0001] The present invention relates to a kind of GC-NCI-MS determination method of tetrachlorantraniliprole residual amount, more specifically adopt gas chromatography-negative chemical ion source-mass spectrometry (GC-NCI-MS) to qualitatively and quantitatively measure grain, pork, The invention discloses a method for residual tetraclotraniliprole content in animal and plant-derived foods with complex matrices such as beef, mutton, chicken and other animal muscles and products, and 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 ne...

Claims

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Application Information

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IPC IPC(8): G01N30/88
Inventor 崔淑华孙涛林超赵峰
Owner INSPECTION & QUARANTINE TECH CENT SHANDONG ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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