Method for determination of flumethrin in garlic or garlic product
A technology of flufenthrin and a determination method, which is applied in the field of determination of pesticide residues in food, and can solve problems such as no literature report in detection.
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Embodiment 1
[0071] 1.1 Extraction
[0072] Weigh about 20.00g (accurate to 0.01g) fresh garlic sample, add 200uL of 1.0ug / mL bifenthrin standard solution, put it in a 150mL conical flask, microwave in a microwave oven at 640w for 50s, cut it into pieces, and add it accurately 50.0mL n-hexane: dichloromethane (1+1), 18000r / min homogeneous extraction for 3min. The sample liquid is filtered into a colorimetric tube with 5-10gNaCl in advance, covered with a stopper, vigorously shaken for 1min, and left standing for 30min , after the organic phase and the aqueous phase were separated, accurately pipette 25mL of the organic phase into a 25mL colorimetric tube, blow it in a 50°C water bath with nitrogen to nearly dry, dissolve the residue with 2.0mL of n-hexane, and wait for purification.
[0073] 2.3.2 Purification
[0074] Pre-wash the amino column with 3.0mL acetone and 5mL n-hexane in sequence (conditioning). When the solvent level reaches the surface of the column adsorption layer, immedia...
Embodiment 2
[0080] Weigh about 20.00g (accurate to 0.01g) of salted garlic, add 200uL of 1.0ug / mL bifenthrin standard solution, place it in a 150mL conical flask, and accurately add 50.0mL of n-hexane: dichloromethane (1+ 1), 18000r / min homogeneous extraction for 3min. The sample solution was filtered into a colorimetric tube with 5-10gNaCl in advance, covered with a stopper, shaken vigorously for 1min, and allowed to stand for 30min. After the organic phase and the aqueous phase were separated, accurate Pipette 25mL of the organic phase into a 25mL colorimetric tube, blow with nitrogen in a water bath at 50°C until nearly dry, dissolve the residue with 2.0mL of n-hexane, and wait for purification.
[0081] 2.3.2 Purification
[0082]Pre-wash the amino column with 3.0mL acetone and 5mL n-hexane in sequence. When the solvent level reaches the surface of the column adsorption layer, immediately pour the above-mentioned solution to be purified, use a 10mL pointed centrifuge tube to receive t...
Embodiment 3
[0088] Weigh about 20.00g (accurate to 0.01g) mashed garlic, add 200uL of 1.0ug / mL bifenthrin standard solution, put it in a 150mL conical flask, add 50.0mL n-hexane: dichloromethane (1+1) accurately , 18000r / min homogeneous extraction for 3min. The sample solution was filtered into a colorimetric tube with 5-10gNaCl in advance, covered with a stopper, shaken vigorously for 1min, and allowed to stand for 30min. After the organic and aqueous phases were separated, pipette accurately Put 25mL of organic phase in a 25mL colorimetric tube, blow with nitrogen gas in a 50°C water bath until nearly dry, dissolve the residue with 2.0mL of n-hexane, and wait for purification.
[0089] 2.3.2 Purification
[0090] Pre-wash the amino column with 3.0mL acetone and 5mL n-hexane in sequence. When the solvent level reaches the surface of the column adsorption layer, immediately pour the above-mentioned solution to be purified, use a 10mL pointed centrifuge tube to receive the eluate, and use ...
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