A kind of hplc detection method of octocalid residue in food
A detection method, the technology of octoprodil, is applied in the field of HPLC detection of octoprodil residues in food, which can solve the problems of insufficient literature and achieve the effects of good repeatability, avoiding matrix interference and high practicability
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Embodiment 1
[0045] The HPLC detection of octocalid residual amount in the concentrated apple juice of embodiment 1:
[0046] (1) Weighing of the sample: Weigh 2 g of concentrated apple juice (accurate to 0.01 g), then add 2 mL of 1mol / L sodium bicarbonate, and shake to completely wet and disperse the sample.
[0047] (2) Extraction of the sample: Add 4 mL of 1 mol / L sodium bicarbonate solution and 4 mL of acetonitrile to the sample in step (1), shake well, and extract by ultrasonic for 30 min.
[0048] (3) Derivatization reaction: Add 0.3 mL of 0.1% Fmoc-Cl derivatization solution and shake well. If the acetonitrile layer is found to be less than 4 mL, about 2 g of sodium chloride should be added to the extract. Let stand for 10 minutes, shake twice in the middle, centrifuge at 3500 rpm / min for 3 minutes, filter the organic phase through a 0.22 µm filter membrane into a sample vial for HPLC analysis.
[0049] (4) Configuration of the standard curve: Standard stock solution: Accurately w...
Embodiment 2
[0059] The HPLC detection of octocalid residual amount in the apple powder of embodiment 2:
[0060] (1) Weighing of the sample: Weigh 1 g (accurate to 0.01 g) of apple powder, then add 2 mL of 1 mol / L sodium bicarbonate, shake to completely wet the sample, and soak overnight.
[0061] (2) Sample extraction: Add 4 mL of 1 mol / L sodium bicarbonate solution and 4 mL of acetonitrile to the sample soaked overnight in step (1), shake well, and extract by ultrasonic for 30 min.
[0062] (3) Derivatization reaction: Add 0.3 mL of 0.1% Fmoc-Cl derivatization solution and shake well. If the acetonitrile layer is found to be less than 4 mL, about 2 g of sodium chloride should be added to the extract. Let stand for 10 minutes, shake twice in the middle, centrifuge at 3500 rpm / min for 3 minutes, filter the organic phase through a 0.22 µm filter membrane into a sample vial for HPLC analysis.
[0063] The configuration of the standard curve, high-performance liquid chromatography (HPLC) d...
Embodiment 3
[0067] The HPLC detection of octocalid residual amount in embodiment 3 tomato paste:
[0068] (1) Weighing of the sample: Weigh 1 g of tomato paste (accurate to 0.01 g), then add 2 mL of 1 mol / L sodium bicarbonate, and shake to completely wet and disperse the sample
[0069] (2) Sample extraction: Add 4 mL of 1 mol / L sodium bicarbonate solution and 4 mL of acetonitrile to the sample soaked overnight in step (1), shake well, and extract by ultrasonic for 30 min.
[0070](3) Derivatization reaction: Add 0.3 mL of 0.1% Fmoc-Cl derivatization solution and shake well. If the acetonitrile layer is found to be less than 4 mL, about 2 g of sodium chloride should be added to the extract. Let stand for 10 minutes, shake twice in the middle, centrifuge at 3500 rpm / min for 3 minutes, filter the organic phase through a 0.22 µm filter membrane into a sample vial for HPLC analysis.
[0071] The configuration of the standard curve, high-performance liquid chromatography (HPLC) determination...
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