Determination method for residual amount of metrafenone
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A method for determination, the technology of metrafenone, applied in the field of determination of metrafenone residues, achieves high sensitivity, easy operation, and the effect of ensuring people's food safety
Inactive Publication Date: 2014-05-07
崔淑华
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[0008] So far, there is no report on the detection method of metrafenone residues in food at home and abroad, so it is of great significance to establish a simple, fast, accurate qualitative and quantitative analysis method for the detection of metrafenone residues in cereal crops such as vegetables, fruits and wheat. important meaning
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Embodiment 1
[0042] Example 1: Detection of Metrafenone Residues in Eggplant
[0043] (1) Sample pretreatment
[0044] Weigh 10.0 g of eggplant that has been thoroughly mixed into a 50 mL centrifuge tube, accurately add 20 mL of acetonitrile, extract homogeneously 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 1mL of acetonitrile extract and transfer to a solution containing 150mg of anhydrous magnesium sulfate, 50mg of C 18and 25mg PSA in a centrifuge tube, vortex for 1min, and centrifuge at 7000r / min for 5min. Take the supernatant and pass it through a 0.22 μm filter membrane, and wait for determination.
[0045] (2) Preparation of standard working solution
[0046] Accurately weigh 25±0.1mg of the standard product in a 25mL volumetric flask, dissolve it with acetonitrile, and dilute to obtain a 1000.0μg / mL standard stock solution; pipette 1.0mL of the standard stock sol...
Embodiment 2
[0079] Embodiment 2: the detection of metrafenone residue in wheat
[0080] (1) Sample pretreatment
[0081] Weigh 5.0g of well-mixed wheat (ground into flour) into a 50mL centrifuge tube, add 10mL of water to resuscitate for 30min, add 20mL of 1% acetic acid acetonitrile accurately, shake and extract for 30min, ultrasonically extract for 3min, add 3g of anhydrous magnesium sulfate, 2g Sodium acetate and 2mL water, vortex for 1min, put the centrifuge tube in -18°C refrigerator for 30min, freeze and centrifuge at 7000r / min for 5min, divide 1.5-2mL extract into 2.0mL centrifuge tube, Refrigerate and centrifuge at a speed of 12000r / min for 10min. After centrifugation, take 2mL of acetonitrile extract and transfer to a solution containing 300mg anhydrous magnesium sulfate, 100mg C 18 and 50mg PSA in a centrifuge tube, vortex for 1min, centrifuge at 7000r / min for 5min, pass through a 0.22μm filter membrane into a brown sampling vial, and wait for LC-MS / MS determination.
[0082]...
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Abstract
The invention discloses a determination method for the residual amount of metrafenone. The determination method comprises the following steps: homogenizing by using acetonitrile or 1% acetonitrile acetate to extract residual metrafenone in a sample; dispersing and purifying an extracting solution by ethylenediamine-N-propoxysilane (PSA) and an octadecyl silane bonded phase (C18) base material; carrying out liquid chromatogram-mass spectrum/mass spectrum (LC-MS/MS) detection; establishing a corrected standard curve by adopting a blank base material solution diluting standard; and quantifying by an external standard method. According to the method, the average recycling rate is 80.2%-94.9%; the average relative standard deviation (RSD) is 4.0%-6.8%; the detection limit is lower than 0.10 microgram/kilogram; the determination method has the advantages of simplicity and convenience in operation, rapidness, high sensitivity, good repeatability and accuracy in qualifying and quantifying. The technical requirements of corresponding product safety detection by countries including European Union, America, Korea, Japan and the like can be met and the powerful technical supports are provided for guaranteeing the food safety of people in China and the healthy development of export trades.
Description
technical field [0001] The present invention relates to a method for determining the residual amount of metrafenone, more specifically, it uses high performance liquid chromatography-tandem mass spectrometry (LC-MS / MS) to qualitatively and quantitatively determine the residual amount of metrafenone in cereal crops such as vegetables, fruits and wheat. The invention discloses a method for ketone content, belonging to the technical field of determination of pesticide residues. Background technique [0002] Powdery mildew, commonly known as white hair disease, is a worldwide disease that occurs widely. The pathogen is mainly transmitted through airflow. It has the characteristics of incubation period, frequent re-infection, strong epidemic, and rapid development of resistance. It is harmful to vegetables in my country (such as eggplant , tomatoes, etc.), fruit (such as grapes, citrus, etc.) [0003] In the comprehensive management system of powdery mildew, disease-resistant var...
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