cableties的部落格

1. Sample extraction

Accurately weighed shower gel 0.2 g (accurate to 0.01 g) in 10 mL stoppered plastic centrifuge tube, add 3 mL of saturated sodium chloride solution, vortex oscillation 1 min to disperse the sample, accurately add 2 mL of acetonitrile, Spin the extraction of 2 min, 5000 r / min centrifugal 10 min, aspiration of the supernatant in another 50 mL stoppered plastic centrifuge tube, the lower sodium chloride solution with 2 mL of acetonitrile repeated extraction step once, combined with the second acetonitrile extract, 40 mL of high purity water was added to the extract, mixed with 0.2 mL of 10% potassium ferrocyanide solution, mixed with 0.2 mL of 20% aqueous solution of zinc acetate, centrifuged at 5000 r / min for 10 min, supernatant To be purified.

2. SPE Cartridge Purification

(1) activation: HLB solid phase extraction column before use in order to use 5 mL of methanol and 10 mL of water activation.
(2) loading and elution: the sample solution to be purified solution added to the activated solid phase extraction column, the flow rate of 1 mL / min column, discard the filtrate. The solid phase extraction column was rinsed with 2 x 5 mL of acetonitrile-water solution (10:90 v / v), the eluent was discarded and the residue was removed from the column with a suction ear. The solid phase extraction column was eluted with 4 mL of methanol and the eluate was collected.
(3) Re-dissolve: The eluate was blown dry at 40 ° C and filtered through 2 mL of a methanol-water solution (5: 5, v / v) and 0.22 μm microporous filter for HPLC testing.

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