Measurement method for cyenopyrafen residue amount
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A technology of fenpyroximate and a determination method, which is applied in the field of determination of fenpyroximate residues, and achieves the effects of good repeatability, avoiding matrix interference and high sensitivity
Active Publication Date: 2014-04-23
崔淑华
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[0006] So far, there are no domestic and foreign reports on the detection method of pyrazafen residues in food. Therefore, it is of great importance to establ
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Embodiment 1
[0038] Embodiment 1: the detection of the residual amount of pyraclofen in oranges
[0039] (1) Sample pretreatment
[0040] Weigh 10.0 g of well-mixed oranges 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 2mL of acetonitrile extract and transfer to a solution containing 300mg anhydrous magnesium sulfate, 100mg C 18 , 50mg PSA and 15mgCarb in a centrifuge tube, vortex for 1min, and centrifuge at 5000r / min for 5min. Take the supernatant and pass it through a 0.22 μm filter membrane, and wait for determination.
[0041] (2) Preparation of standard working solution
[0042] Weigh 10g orange blank sample, prepare a blank matrix solution through the above pretreatment steps, dilute the 100ng / mL standard solution with acetonitrile into a 10ng / mL standard intermediate solution,...
Embodiment 2
[0075] Embodiment 2: the detection of the residual amount of pyrazafen in tea
[0076] (1) Sample pretreatment
[0077] Weigh 1.0g of fully mixed tea into a 50mL centrifuge tube, add 3mL of water to revive for 30min, then accurately add 20mL of 1% acetic acid acetonitrile, extract homogeneously for 1min, add 3g of anhydrous magnesium sulfate, 2g of sodium acetate and 2mL of water, vortex After 1min, centrifuge at 7000r / min for 5min. After centrifugation, take 2mL of acetonitrile extract and transfer to a solution containing 300mg anhydrous magnesium sulfate, 100mg C 18 , 50mg PSA and 15mgCarb in a centrifuge tube, vortex for 1min, centrifuge at 5000r / min for 5min, pass through 0.22 μ m filter membrane in a brown injection vial, to be determined by LC-MS / MS.
[0078] (2) Preparation of standard working solution
[0079] Weigh 2g tea blank sample, prepare blank matrix solution through the above pretreatment steps, and use it to dilute and prepare 0.5, 1, 2, 5, 10, 20, 50ng / m...
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Abstract
The invention discloses a measurement method for cyenopyrafen residue amount. The measurement method comprises the following steps: homogeneously extracting residual cyenopyrafen in a sample by using acetonitrile or 1 percent acetic acid-acetonitrile so as to obtain extracted liquid, performing LC-MS/MS (liquid chromatography-mass spectrometry/mass spectrometry) detection after the extracted liquid is dispersed and purified by a bonded phase (C18) of ethylenediamine-N-propyl silane (PSA) and an octadecylsilane and graphitized carbon (Carb) substrate; establishing a corrected standard curve by adopting a blank matrix solution dilution standard, and fixing the quantity by adopting an external standard method. According to the method, the average recovery rate is 87.6 to 94.5 percent, the average relative standard deviation (RSD) is 3.7 to 6.4 percent, the detection limit is lower than 0.42mu g/kg; the measurement method has the advantages of convenience and rapidness in operation, high sensitivity, and high repeatability, and the qualitative and quantitative accuracy is high. The technical requirements on corresponding product safety detection in countries, such as Korea, Japan, and the European Union, can be met; the powerful technical support is provided for guaranteeing the food security of Chinese people and the sustainable development on foreign export trade.
Description
technical field [0001] The present invention relates to a method for determining the residual amount of pyraclofen, more specifically, it is a qualitative and quantitative determination of the residual pyrazafen in vegetables, fruits and tea leaves by using high performance liquid chromatography-tandem mass spectrometry (LC-MS / MS) The method for content belongs to the technical field of determination of pesticide residues. Background technique [0002] Cyenopyrafen (Cyenopyrafen) is a new type of pyrazole acaricide developed by Nissan Chemical Company in 2009. It is mainly used to control harmful mites such as red spiders on fruit trees, vegetables and tea. The chemical name is (E)-2-( 4-tert-butylphenyl)-2-cyano-1-(1,3,4-trimethylpyrazol-5-yl)alkenyl 2,2-dimethylpropionate, English chemical name (E)-2-(4-tert-butylphenyl)-2-cyano-1-(1,3,4-trimethylPyrazol-5-yl)vinyl2,2-imethylpropionate, CAS accession number is 560121-52-0, The molecular weight is 393.52, and the structur...
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