Pretreatment method and residual quantity detection method for diquat in food
A detection method, Diquat technology, applied to measuring devices, instruments, scientific instruments, etc., can solve the problems of inaccurate qualitative and quantitative, poor anti-interference, poor quality control, etc., to simplify the pre-treatment process and target the operation Sexuality and cost reduction effect
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Embodiment 1
[0041] High-sugar and high-protein samples were pretreated by the sulfuric acid reflux method, and the specific steps were as follows:
[0042](1) After chopping or crushing samples such as dehydrated garlic, raisins, wolfberry, chili powder, nuts, purple sweet potato powder, tea leaves, protein powder, syrup, etc., weigh 4g of the sample into a 250mL flat-bottomed flask, and add 40mL of 25% Sulfuric acid solution, mix well, heat at 100°C and reflux for 3h;
[0043] (2) After the flask is cooled to room temperature, rinse the reflux tube with 100mL of water, combine the solution and filter it with glass fiber filter paper;
[0044] (3) Take 5mL of filtrate, adjust the pH value to 6-7 with 1mol / L sodium carbonate solution, centrifuge at 9000r / min for 3min; wait for purification;
[0045] (4) Use 5mL of methanol and 5mL of water to sequentially wash the activated strong cation exchange column, transfer all the above-mentioned solution to be purified to the activated strong cati...
Embodiment 2
[0048] Pretreatment of vegetables, fruits, concentrated fruit juices, and milk powder samples by acid extraction and purification method, the specific steps are as follows:
[0049] (1) Weigh 2g of sample into a 50mL centrifuge tube, add 10mL of 50% methanol solution containing 2% formic acid, shake for 30min; centrifuge at 9000r / min at 4°C for 3min, take the supernatant and pass it through a 0.45μm nylon filter membrane, to be purified ;
[0050] (2) Use 5mL of methanol and 5mL of water to sequentially rinse the activated strong cation exchange column, transfer all the above-mentioned solution to be purified to the activated strong cation exchange column, sequentially use 10mL of water and 5mL of methanol to rinse, and vacuum dry; Then accurately add 2 mL of 25% acetonitrile solution containing 1 mol / L ammonium acetate, and vacuum dry for elution;
[0051] (3) The sample solution obtained above was vortex mixed, diluted 5 times with 10 mmol / L ammonium acetate solution, passe...
Embodiment 3
[0053] Samples of edible oil, wine, and clarified fruit juice were pretreated by direct extraction, and the specific steps were as follows:
[0054] Weigh 2g of sample into a 50mL centrifuge tube, add 10mL of 50% methanol solution containing 2% formic acid, shake for 30min; centrifuge at 9000r / min at 4°C for 3min, take the supernatant and pass it through a 0.45μm nylon filter membrane, and wait for the test on the machine.
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