Method for measuring patulin in apple juice
The technology of a patulin and an assay method, which is applied in the field of rapid detection of patulin in apple juice, can solve the problems of complicated operation steps, large amount of reagents, lengthy process and the like, achieves strong specificity, reduces detection limit, Strong anti-interference ability
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Embodiment 1
[0033] Weigh 5.00 g of apple juice into a centrifuge tube, shake, add 5 mL of ethyl acetate-n-hexane solution (95+5, V / V), shake, add 0.3 g of sodium bicarbonate, shake vigorously for 2 min, 4500 r / Centrifuge for 3 min; pipette 3.2 mL of the supernatant to an ethyl acetate-activated Carb / C18 mixed solid-phase extraction column, use a test tube with 30 μL of glacial acetic acid to receive the eluate, and elute with 4 mL of ethyl acetate at 40°C Blow dry slowly with nitrogen gas, add 240 μL of acetonitrile to dissolve, accurately pipette 150 μL of the solution into a 1.5 mL screw-top high-recovery sample bottle, add 50 μL of derivatization reagent, seal with a septum, react under high-grade microwave conditions of 800W for 1 min, and cool , for gas chromatography-mass spectrometry.
Embodiment 2
[0035] Weigh 5.00 g of apple juice into a centrifuge tube, shake, add 5 mL of ethyl acetate-n-hexane solution (95+5, V / V), shake, add 0.4 g of sodium bicarbonate, shake vigorously for 2 min, 4500 r / Centrifuge for 3 min; pipette 3.2 mL of the supernatant to an ethyl acetate-activated Carb / C18 mixed-type solid-phase extraction column, use a test tube added with 30 μL of glacial acetic acid to receive the eluate, and elute with 6 mL of ethyl acetate. Blow dry slowly with nitrogen, add 240
[0036] Dissolve in μL of acetonitrile, accurately pipette 150μL of the solution into a 1.5mL screw-top high-recovery sample bottle, add 50μL of derivatization reagent, seal with a septum, react under high-grade microwave conditions of 800W for 3min, cool down, and use for gas chromatography-mass spectrometry determination .
Embodiment 3
[0038] Weigh 5.00 g of apple juice into a centrifuge tube, shake, add 5 mL of ethyl acetate-n-hexane solution (95+5, V / V), shake, add 0.7 g of sodium bicarbonate, shake vigorously for 2 min, 4500 r / Centrifuge for 3 min; pipette 3.2 mL of the supernatant to an ethyl acetate-activated Carb / C18 mixed-type solid-phase extraction column, use a test tube added with 30 μL of glacial acetic acid to receive the eluate, and elute with 8 mL of ethyl acetate. Blow dry slowly with nitrogen gas, add 240 μL of acetonitrile to dissolve, accurately pipette 150 μL of the solution into a 1.5 mL screw-top high-recovery sample bottle, add 50 μL of derivatization reagent, seal with a septum, react under high-grade microwave conditions of 800W for 5 minutes, and cool , for gas chromatography-mass spectrometry.
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