Purification and adsorption material, and application thereof in simultaneous detection of ten insecticide residues in tomatoes
A technology for adsorption materials and pesticides, which is applied to the purification of adsorption materials and its application in the simultaneous detection of ten kinds of pesticide residues in tomatoes, can solve the problems of large detection errors, and the recovery rate of addition does not meet the requirements, etc., to achieve The effect of improving detection efficiency, improving the accuracy of results, and reducing detection costs
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Embodiment 1
[0063] Embodiment 1 UPLC-MS / MS optimal analysis condition optimization
[0064] Accurately weigh a certain amount of 10 kinds of pesticide technicals, use acetonitrile as a solvent, prepare a single standard solution of 0.5 mg / L for mass spectrometry tuning, and obtain suitable analysis conditions by liquid chromatography and mass spectrometry. Accurately weigh a certain amount of 10 kinds of insecticides to the same volumetric flask, dissolve and constant volume with chromatographically pure acetonitrile solvent, obtain 10 kinds of insecticides mixed standard samples, the concentration is 500mg / L, and then dilute step by step, 100, 50, 10, 5, 1, 0.5 μg / L mixed standard samples were obtained, and after analysis and detection, standard curves of 10 pesticides were obtained.
[0065] Pump 0.5 mg / L standard solution for tuning into the mass spectrometer, and use ESI+ mode to determine the parent ions and product ions of 10 pesticides to be tested respectively; select two ion pair...
Embodiment 2
[0073] 9 kinds of pretreatment method screening of 10 kinds of insecticides in embodiment 2 tomato
[0074] Crush the tomato sample, accurately weigh 10.00g of the tomato sample into a 50mL centrifuge tube, add 10 kinds of insecticide mixed standard samples, so that the addition level in each centrifuge tube is 0.02mg / kg, after standing for 2h, respectively Add 20mL of acetonitrile as the extraction solvent, vortex and mix to form a uniform sample solution, so that the sample is fully dissolved and extracted; add 2g of anhydrous Na 2 SO 4 and 3gNaCl, vortexed for 10s, centrifuged at 4000rpm for 5min, took 1.5mL supernatant, used 9 different adsorbent combinations for QuEChERS purification treatment, vortexed and mixed, centrifuged at 12000rpm for 5min, took the supernatant and filtered it with a 0.22μm organic filter membrane, to be tested. The addition recoveries corresponding to the 9 adsorbent combinations were compared, and each adsorbent combination was repeated twice. ...
Embodiment 3
[0082] The matrix effect of ten kinds of insecticides in the tomato of embodiment 3
[0083] In order to evaluate the matrix effect of 10 insecticides in tomato, a blank matrix solution (as a solvent for dilution) was prepared with the best adsorbent combination material screened out, and mixed standard samples of 10 insecticides were used to obtain 0.5, 1, 5 , 10, 50, and 100 μg / L matrix mixed standard samples, calculate the matrix standard curves of 10 pesticides respectively, and make the solvent standard curves (acetonitrile samples) of 10 pesticides at the same time, using the matrix standard curve and solvent standard curve The slope ratio of is used as the matrix effect (ME) evaluation index. Generally speaking, when ME is between 0.8 and 1.2, it is considered that there is no obvious matrix effect. The closer the ratio is to 1, the weaker the matrix effect is; when the ratio is greater than 1, it is a matrix enhancement effect;
[0084] The acetonitrile solution stand...
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