Liquid chromatography-mass spectrometry/mass spectrometry (LC-MS/MS) measuring method for Si lv chong xian'an residue quantity

A tetrachlorantraniliprole, LC-MS technology, applied in measuring devices, instruments, scientific instruments, etc., can solve complex problems, achieve the effects of easy operation, ensure people's food safety, and avoid matrix interference

Active Publication Date: 2015-04-08
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. The use of LC-MS / MS to determine pesticide residues in food and agricultural products has the advantages of rapidity, simplicity, and high sensitivity. The matrix of food and agricultural products such as sexual food is relatively complex, and it is necessary to establish a sample pretreatment method with good purification effect to meet the detection requirements. The LC-MS / MS detection method is of great significance

Method used

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  • Liquid chromatography-mass spectrometry/mass spectrometry (LC-MS/MS) measuring method for Si lv chong xian'an residue quantity
  • Liquid chromatography-mass spectrometry/mass spectrometry (LC-MS/MS) measuring method for Si lv chong xian'an residue quantity
  • Liquid chromatography-mass spectrometry/mass spectrometry (LC-MS/MS) measuring method for Si lv chong xian'an residue quantity

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Example 1: Detection of Tetrachlorantraniliprole residues in pork

[0038] (1) Sample pretreatment

[0039] extract

[0040] Weigh 5g of fully mixed pork sample into a 50mL centrifuge tube, add 5mL of water to mix, let stand for 30min, accurately add 20mL of acetonitrile, 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.

[0041] purify

[0042] 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 column for elution, all ...

Embodiment 2

[0075] Example 2: Detection of Tetrachlorantraniliprole residues in rice

[0076] Sample pretreatment

[0077] extract

[0078] Weigh 5g of rice 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 8mL of the extract solution at 40°C by rotary steaming or blowing with nitrogen until it is nearly dry, add 1mL of acetonitrile and vortex, and wait for purification.

[0079] purify

[0080] 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, an...

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Abstract

The invention discloses a liquid chromatography-mass spectrometry / mass spectrometry (LC-MS / MS) measuring method for the Si lv chong xian'an residue quantity. The LC-MS / MS measuring method is mainly used for measuring the quantity of residual Si lv chong xian'an in complex matrix food agricultural products such as cereal grain food and animal derived food. The residual Si lv chong xian'an in a sample is homogeneously extracted through acetonitrile or an acetonitrile solution containing 1% acetic acid, LC-MS / MS testing is conducted after purification is conducted through a C18 / PSA solid-phase extraction column, a corrected standard curve is established through a blank matrix solution without containing pesticide to be tested, and quantification is conducted through an external standard method. According to the LC-MS / MS measuring method, the average recovery rate ranges from 84.9% to 93.6%, the average relative standard deviation (RSD) ranges from 4.1% to 6.5%, the detection limit is smaller than 0.69 microgram per kilogram, and the LC-MS / MS measuring method has the advantages that operation is easy, convenient and rapid, the impurity removal effect is good, sensitivity is high, repeatability is good, and qualitative and quantitative operation is accurate; the technical requirement of 0.01mg / kg residual limit for the uniform limit can be met, and powerful technical support is provided for food safety of people in China and healthy development of foreign export trade.

Description

technical field [0001] The present invention relates to a kind of LC-MS / MS determination method of tetrachlorantraniliprole residual amount, more specifically adopt liquid chromatography tandem mass spectrometry (LC-MS / MS) to qualitatively and quantitatively measure grain, pork, beef, mutton, The invention discloses a method for residual tetraclotraniliprole content in animal and plant-derived foods with complex matrices such as 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 new product developed b...

Claims

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Application Information

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IPC IPC(8): G01N30/88G01N30/06
Inventor 崔淑华谭乐义王宇韩伟
Owner INSPECTION & QUARANTINE TECH CENT SHANDONG ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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