Method for simultaneous detection of various antibiotic residues in vegetables
A technology of antibiotics and vegetables, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of high detection limit, few types of antibiotics, and high cost, and achieve the effect of overcoming high cost
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Embodiment 1
[0038] The determination of embodiment 1 standard curve, detection limit and limit of quantification
[0039] (1) Preparation of standard stock solution:
[0040] Accurately weigh 1mg of each of the 11 target antibiotic standards in a 10ml brown volumetric flask, dissolve and dilute to volume with the initial mobile phase (0.1% formic acid solution and acetonitrile, the ratio is 8:2), and prepare a 0.1mg / ml single standard stock solution, stored at 4°C.
[0041] Accurately pipette 10 μl of the 11 single-standard stock solutions into the same 10ml brown volumetric flask to make up the volume with the initial mobile phase, mix evenly after ultrasonication, and prepare a mixed standard solution with each antibiotic content of 100 μg / L ①.
[0042] Accurately pipette 5ml of the mixed standard solution into a 10ml brown volumetric flask with the initial mobile phase to make up the volume, mix evenly after ultrasonication, and prepare a mixed standard solution with each antibiotic c...
Embodiment 2
[0058] Embodiment 2 verification, add recovery detection experiment
[0059] (1) Experimental steps
[0060] The collected antibiotic-free organic vegetable samples (leek, celery, lentils, beans, cauliflower), freeze-dried, ground through a 2mm sieve, accurately weighed 1g of the ground sample, mixed the antibiotic mixed standard solution in the vegetable sample to obtain 0.05 Fortified vegetable samples at μg / g, 0.1 μg / g and 0.5 μg / g. Then add 10ml of acetonitrile:hydrochloric acid (125:4, v / v) extractant, vortex for 30s, sonicate at room temperature for 15min, centrifuge at 8000rpm for 15min, and transfer the supernatant to another brown container. Then use the same method to extract the precipitate again, the steps are the same as above, combine the extracts and pass through a 0.45 μm membrane filter. Concentrate the combined extracts to 3-5 ml using a rotary evaporator.
[0061] Activation of the HLB column: first pass through the column naturally with 5ml of methanol, ...
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