Method for determining multiple residues of veterinary drugs in aquatic products

Abstract

The invention provides a method for determining multiple residues of veterinary drugs in aquatic products. The method comprises the following steps: (1) preparing a standard series of working solutions, namely respectively weighing 0.1 g of four malachite green drugs, transferring the malachite green drugs into a volumetric flask, fixing the volume by using acetonitrile, respectively weighing 0.1g of eight quinolone drugs, transferring the quinolone drugs into a volumetric flask, and fixing the volume by using 2% acetonitrile acetate; (2) preparing a sample; and (3) weighing the crushed sample, adding an internal standard working solution, adding 20-30mL of acidified acetonitrile (containing 1-5% of acetic acid or 0.5-5% of formic acid), shaking for uniform mixing and homogenization, adding 5g of neutral aluminum oxide powder, oscillating for uniform mixing, carrying out ice-bath ultrasonic treatment, centrifuging at a low temperature, taking the obtained supernatant, blowing with inert gas until the supernatant is nearly dry to obtain a to-be-purified solution, adding 1-2 mL of acetonitrile + aqueous solution to dissolve the to-be-purified solution, adding n-hexane, uniformly mixing, leaching to remove n-hexane, filtering by using a polyether sulfone filter membrane, then determining chromatographic and mass spectrometric conditions, and setting chromatographic and mass spectrometric parameters. The method has the beneficial effects that the detection precision is high, the credibility is high, the harm caused by chemical reagents can be reduced, and the cost is saved.

Description

technical field [0001] The invention relates to a technique for detecting multiple residues of veterinary drugs, in particular to a method for determining multiple residues of veterinary drugs in aquatic products. Background technique [0002] Veterinary drug residues refer to the prototype drugs, metabolites or residues of impurities related to veterinary drugs accumulated or stored in the cells, tissues or organs of the body and their products (milk, eggs, etc.) after livestock, poultry and aquatic animals have been treated with drugs. Drugs left in food are transferred to the human body through the food chain and continuously enriched in it, thus causing chronic poisoning of the human body. [0003] Among them, veterinary drugs commonly used in aquatic products include quinolones and malachite green. [0004] Quinolones (QNs), also known as pyridone acids, are a new class of antibacterial drugs artificially synthesized with a 1,4-dihydro-4-oxoquinoline-3-carboxylic acid ...

AI Technical Summary

Problems solved by technology

However, there are also methods that can simultaneously determine malachite green and quinolones in aquatic products, including patent number: 201710101179.3, a patent named the method for determining malachite green, quinolones, and sulfonamides in aquatic products. There are / colorless malachite green, deuterated have / colorless malachite green, norfloxacin, ciprofloxacin, enrofloxacin, deuterated ciprofloxacin are detected, as can be seen from the examples of this patent, The recovery rate that has data in this detection method exceeds 100%, for example the recovery rate of enrofloxacin is 101.3%, so the recovery rate of this detection method has certain error, and accuracy rate is not accurate enough; In large cases, the detection results are more inaccurate and unreliable

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