GC-NCI-MS (gas chromatography-negative chemical ionization-mass spectrometry) determination method of residual amount of metrafenone in fruits and vegetables
A GC-NCI-MS and metrafenone technology, applied in the field of determination of pesticide residues, can solve the problems of low sensitivity of anti-interference ability, achieve the effect of avoiding matrix interference, ensuring people's food safety, and good repeatability
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Embodiment 1
[0033] Example 1: Detection of Metrafenone Residues in Apples
[0034] (1) Sample pretreatment
[0035]Weigh 10.0 g of well-mixed apples into a 50 mL centrifuge tube, accurately add 20 mL of acetonitrile, homogeneously extract 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 6mL of acetonitrile extract and transfer to a solution containing 900mg anhydrous magnesium sulfate, 300mg C 18 and 150mg PSA in a centrifuge tube, vortex for 1min, and centrifuge at 5000r / min for 5min. Take 4 mL of the supernatant in a nitrogen blowpipe, dry it with nitrogen at 40°C, add acetone / n-hexane mixed solvent with a volume ratio of 1 / 1 to dissolve the residue, vortex and mix evenly, pass through the membrane, and transfer it to the sample bottle for GC- NCI-MS assay.
[0036] (2) Preparation of standard working solution
[0037] Accurately weigh 25±0.1mg of the standard product in...
Embodiment 2
[0062] Example 2: Detection of Metrafenone Residues in Eggplant
[0063] (1) Sample pretreatment
[0064] Weigh 10.0g of eggplant that has been thoroughly mixed into a 50mL centrifuge tube, add 8mL of water, accurately add 20mL of acetonitrile solution containing 1% acetic acid, extract homogeneously for 1min, add 3g of anhydrous magnesium sulfate and 2g of sodium acetate, and vortex for 1min After that, centrifuge at 7000r / min for 5min. After centrifugation, take 6mL of acetonitrile extract and transfer to a solution containing 900mg anhydrous magnesium sulfate, 300mg C 18 and 150mg PSA in a centrifuge tube, vortex for 1min, and centrifuge at 5000r / min for 5min. Take 4mL of the supernatant in a nitrogen blowpipe, dry it with nitrogen at 40°C, add acetone / n-hexane mixed solvent with a volume ratio of 1 / 1 to dissolve the residue, vortex and mix well, then transfer it to the sample bottle to wait for GC-NCI - MS determination.
[0065] (2) Preparation of standard working sol...
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