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A kind of assay method of pyrifluquinazon residue
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A method of determination and technology of residues, applied in complex fields, can solve problems such as low sensitivity of anti-interference ability, and achieve the effects of avoiding matrix interference, good repeatability, and easy operation
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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. Pyrifluquinazon is an electronegative compound, but so far there is no GC-NCI-MS detection of Pyrifluquinazon residues in vegetables and fruits In the report of the method, due to the complex matrix of food and agricultural products such as grains and animal-derived foods, it is necessary to establish a sample pretreatment method and instrument analysis conditions with good purification effects to meet the detection requirements. Therefore, the establishment of gas chromatography-negative chemical ion source-mass spectrometry (GC-NCI-MS) method for the qualitative and quantitative analysis of Pyrifluquinazon residues in grains and foods of animal origin is of great significance
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Embodiment 1
[0033] Example 1: Detection of Pyrifluquinazon residues in pork
[0034] (1) Sample pretreatment
[0035] extract
[0036] 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.
[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 column for elution, all the eluat...
Embodiment 2
[0062] Embodiment 2: the detection of Pyrifluquinazon residue in wheat
[0063] (1) Sample pretreatment
[0064] extract
[0065] Weigh 5g of wheat 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.
[0066] purify
[0067] 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...
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Abstract
The invention discloses a determination method for Pyrifluquinazon residual quantity. The method is mainly used for determining the content of residual Pyrifluquinazon in complex matrix food and agricultural products such as cereal grains and animal derived foods. Homogeneous extraction of residual Pyrifluquinazon in samples is carried out by using acetonitrile or an acetonitrile solution containing 1% of acetic acid, after purification and concentration with a C18 / PSA solid-phase extraction column, gas chromatography-negative chemical ion source-mass spectrometry (GC-NCI-MS) detection is carried out, a corrected standard curve is established by adopting a blank substrate solution which does not contain a pesticide to be tested, and quantization is carried out by an external standard method. According to the method, the average recovery rate is 75.1%-80.2%, the average relative standard deviation (RSD) is 4.8%-8.0%, the detection limit is lower than 2.77 microg / kg, and the determination method has the advantages of easiness, convenience and quickness in operation, good impurity removal effect, high sensitivity, marked characteristics, good repeatability, and accurate qualification and quantization. The determination method can meet the technical requirement of countries such as Japan, European Union and South Korea for 0.01mg / kg residue limit in corresponding food safety testing, namely 'uniform standard', so as to provide powerful technical support for guaranteeing the food safety of Chinese people and the healthy development of export trade.
Description
technical field [0001] The present invention relates to a kind of determination method of Pyrifluquinazon residue, more specifically adopt gas chromatography-negative chemical ion source-mass spectrometry (GC-NCI-MS) to qualitatively and quantitatively measure grain, pork, beef, mutton, chicken and other animal muscles The invention discloses a method for residual Pyrifluquinazon content in animal and plant-derived foods with complex matrices, such as products and products, and belongs to the technical field of determination of pesticide residues. Background technique [0002] Pyrifluquinazon is a new quinazoline insecticide with a bisamide structure invented by Japan Pesticide Company and jointly developed by Japan Combination Chemical Company. It is mainly used to control aphids, whiteflies and mealybugs on vegetables, fruit trees and tea. , leafhoppers, thrips and other piercing-sucking pests. The chemical name is 1-acetyl-3,4-dihydro-3-[(3-pyridylmethyl)amino]-6-[1,2,2,...
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