Solid phase extraction equipment for carbamate insecticides
method:
Column: SPEBond-elut amino-propyl bonded silica gel column 1ml / 100mg. GilsonASPEC system, 402 diluter, extraction column rack, sample rack and elution rack.
Sample Preparation:
1. Fruits and vegetables: 15ml mashed, add 30ml acetone homogenate, then centrifuge for 30 seconds, add 30ml dichloromethane, 30ml light petroleum ether, mix and homogenize, centrifuge (4000RPM) for 2 minutes, take the supernatant (organic phase ).
Take 2ml of the above extraction solution into the sample tube of ASPEC, place it on the rack of the sample tube of ASPEC, evaporate to dryness at 60 ℃ in water, and dissolve the residue in 1ml of dichloromethane for inspection.
2. Food: Weigh 25g of sample in the flask, add 100ml of acetone-dichloromethane, soak overnight (more than 16 hours) for extraction, transfer 1ml of extract to the ASPEC sample bottle, the following steps are the same as fruit and vegetable processing procedures. ASPEC SPE purification procedure steps:
1) Move the extraction column rack (DEC rack) to the discharge position;
2) Column aging: add 1ml of methylene chloride to the SPE column;
3) Add samples;
4) Move the DEC rack to the collection position;
5) Elution steps:
A. Add 1ml of extraction solution to the SPE column;
B. Fractions are collected in the collection tube;
C. Move the DEC rack to the discharge position;
6) Evaporation steps:
A. Switch the three-way valve to the N2 position;
B. Dry with N2 gas under heating;
7) Redissolution steps:
A. Add 100ul of acetonitrile to the collection tube, wait for 0.5 minutes and add 900ul of water to extract;
B. Pipette the mixed solution for Hplc analysis.
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