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A kind of lc-ms/ms determination method of fluoxetin residue
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A technology of fluoxybactam and LC-MS, which is applied in the field of LC-MS/MS determination of fluoxybactam residues, can solve complex problems, achieve simple operation, ensure people's food safety, and avoid matrix interference
Active Publication Date: 2016-08-17
崔淑华
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[0005] So far, there have been no domestic and foreign reports on the detection method of fluoxetin 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
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Embodiment 1
[0037] Example 1: Detection of Fluorapyramide 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 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.
[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 the elu...
Embodiment 2
[0076] Example 2: Detection of Fluorapyramide Residues in Rice
[0077] Sample pretreatment
[0078] extract
[0079] 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.
[0080] purify
[0081] 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...
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Abstract
The invention discloses an LC-MS / MS determination method of the residual quantity of fluoroether bacteria amide. The method is mainly used for determining the content of fluoroether bacteria amide remaining in complex matrix food and agricultural products such as grains and animal derived foods. The method comprises the following steps: homogenizing and extracting fluoroether bacteria amide remaining in a sample by using acetonitrile or acetonitrile solution containing 1% of acetic acid, purifying by using a C18 / PSA solid-phase extraction column, detecting by adopting LC-MS / MS, setting a corrected standard curve by adopting a blank matrix solution which does not contain the pesticide to be determined, and determining the residual content of fluoroether bacteria amide by adopting an external standard method. By adopting the method, the average recovery rate can be 83.1-89.5%, the average relative standard deviation (RSD) can be 4.0-6.3%, and the detection limit can be less than 0.12mu g / kg. The method is easy to operate, can be used for rapid, quantitative, qualitative and accurate determination, has high sensitivity, good repeatability and a good impurity removal effect, can meet the technical equipment of uniform residue limit of 0.01mg / kg and can provide a powerful technical support to guarantee the food security and the sound development of the export trade in China.
Description
technical field [0001] The invention relates to a LC-MS / MS method for determining the residual amount of fluoxetin, more specifically, qualitative and quantitative determination of grains, pork, beef, mutton, The invention relates to a method for the content of fluoxetyram residues 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, fluroxystamide (LH-2010A) is a new product developed by Shenyang Research Institute of Chemical Industry, a subsidiary of Sinochem Group, and operated...
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