Pesticide residue solid phase extraction method in cereals, beans, nuts and seeds
a. Weigh 10g sample, add 20mL water, and place for 1 min;
b. Add 50mL acetonitrile, homogenize, suction filtration, rinse the residue on the filter paper with 20mL acetonitrile, combine the filtrate, and dilute to 100mL with acetonitrile;
c. Measure 20 mL of the filtrate, add 10 g of NaCl and 20 mL of 0.5 mol/L phosphate buffer (pH 7.0), shake well for 10 min, let stand for stratification, and discard the aqueous layer;
2. C18 SPE purification
a. Activation: Bond Elut C18 (1 g) column, rinsed with 10 mL of acetonitrile for activation;
b. Load: Add 20 mL of extract. Collecting the effluent solution;
c. Elution: elute with 2 mL of acetonitrile, receive the eluent, and combine all the effluent solutions;
d. Dehydration: The collected solution is passed through a funnel containing anhydrous sodium sulfate, and the funnel is rinsed with an appropriate amount of acetonitrile to collect the entire filtrate;
e. Concentration: At a temperature below 40 Â° C, concentrate near-dry and re-dissolve with 2 mL of acetonitrile / toluene (3:1) for further purification.
3. Carbon/NH2 SPE purification
a. Activation: Bond Elut Carbon/NH2 (500 mg/500 mg) column, rinsed with 10 mL acetonitrile/toluene (3:1) for activation;
b. Loading: 2 mL of the preliminary purified sample solution in the previous step is added to the Carbon/NH2 SPE column;
c. Elution: Rinse the SPE column with 20 mL of acetonitrile/toluene (3:1) and collect all the loading effluent and eluent;
d. Concentration: below 40 Â° C, concentrated near dry, then add 5mL of acetone to redissolve and concentrate near dry, dissolved in acetone / n-hexane (1:1), to a volume of 1mL.
4. GC-MS or GC-MS/MS detection
5. The sample contains hundreds of insecticides, fungicides, herbicides, feed additives, veterinary drugs, etc.
SPE column used in this method:
Bond Elut C18 (1g, 6mL, PN.12256001)
Bond Elut Carbon/NH2 (500 mg/500 mg, 6 mL, PN. 12252202).
The method satisfies the simultaneous detection requirements of residual pollutants in hundreds of foods such as insecticides, fungicides, herbicides, feed additives and veterinary drugs in the Japanese Pesticide Residue Regulations.
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