Method for detecting residue of seven synthetic antibacterial agents in aquatic products

A technology for aquatic products and neutral alumina, which is applied in the preparation of test samples, measuring devices, instruments, etc., to ensure food safety, reduce testing cycles, and reduce testing costs.

Inactive Publication Date: 2010-01-13
吴光红 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The detection of veterinary drug residues in fish tissues is basically a single detection method, but for the simultaneous detection of different types of synthetic antibacterial agent residues, my country is still in a blank stage

Method used

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  • Method for detecting residue of seven synthetic antibacterial agents in aquatic products
  • Method for detecting residue of seven synthetic antibacterial agents in aquatic products
  • Method for detecting residue of seven synthetic antibacterial agents in aquatic products

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Since sulfonamides contain amino and benzenesulfonamide structures, they are weakly basic, quinolones are acid-base amphoteric compounds, and furazolidone also contains amphoteric groups, so adjusting the pH in the mobile phase can inhibit the dissociation of weak bases , thereby changing the retention time of the chromatographic peak. The ratio of acetonitrile to aqueous acetic acid also affects retention time and peak shape.

[0033] If the mobile phase isocratic elution with acetonitrile+0.08mol / L acetic acid aqueous solution (30+70), although the analysis time can be shortened, the separation degree of sulfadiazine, sulfamethazine and sulfamethazine is not ideal enough, each drug The peak shape is broad, and the sulfadiazine elutes too early, making it difficult to completely separate from the impurity peak (Figure 2).

[0034] Therefore, in order to ensure good separation effect and chromatographic peak shape of each target substance, this method adopts acetonitri...

Embodiment 2

[0036] Many documents are processed to degreasing and purification, then concentrate, constant volume, and test on the machine. This study also did a lot of experiments in this area, and found that the presence of some substrates interfered with the qualitative and quantitative peaks of the target drug and reduced the detection sensitivity when detecting low-concentration drugs (Figure 3). Therefore, it is not enough to degrease and purify only by n-hexane, because n-hexane only removes most of the non-polar impurity components, and many polar substances, such as phospholipids, glycoproteins, etc., still exist in the extraction solvent, so further SPE purification is required . Due to the many types of drugs analyzed in this test, it is difficult to achieve a good purification effect and recovery rate for each target compound through the SPE column purification of one packing. Based on the purification effect of the extraction column on these seven target compounds, it is con...

Embodiment 3

[0038] Take a certain amount of 1.0μg / mL standard intermediate solution, dilute it successively with acetonitrile to form mixed standard working solutions with serial concentrations of 0.05, 0.1, 0.2, 0.5, and 1.0μg / mL, and carry out each mass concentration according to the above chromatographic conditions. Sample 20μL. Carry out linear regression analysis, linear regression equation and correlation coefficient (Table 3) to the mass concentration X (μg / mL) of standard working solution with the peak area Y of each component respectively. The results showed that the linear relationship of each component was good within the concentration range of 0.05μg / mL~1.0μg / mL.

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Abstract

A detection method simultaneously detects residue of multiple synthetic antibacterial agents in aquatic products by a high performance liquid chromatography. The synthetic antibacterial agents mainly comprise sulfadiazine SD, sulfamerazine SMR, sulfadimidine SDD, sulfadimethoxine SDM, furazolidone FZD, oxolinic acid OXA, nalidixic acid NAA and the like. The multiple synthetic antibacterial agents in an aquatic product sample are extracted by acetonitrile, degreased by normal hexane, concentrated, purified by a solid phase extraction column (alumina neutral) or a C18 solid phase extraction column, analyzed by a liquid chromatograph, detected by an ultraviolet detector, and quantified by an external standard method. The method can quickly, sensitively and accurately detect multiple target compounds to greatly reduce detection cost and shorten detection time.

Description

technical field [0001] The invention relates to a detection technology for simultaneously detecting the residual amounts of seven synthetic antibacterial agents in aquatic products. Background technique [0002] Drug residues in aquatic products are mainly due to the residues of original drugs, metabolites and related impurities of drugs contained in any edible part of aquatic products that are accumulated and stored in any edible part of aquatic products after the use of drugs for disease prevention and treatment in the process of aquaculture, which also includes drugs Residues in the ecological environment and in other aquatic animals and plants. The main residual drugs in aquatic products are antibiotics, sulfonamides, furans, quinolones and certain hormones. However, due to the unknown of the drug history of the analysis sample, that is, the unknown of the pollution source and the diversity of sample types, to determine the safety of a food often requires multiple tests...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N1/34G01N30/06
Inventor 吴光红孟勇杨洪生张美琴朱晓华
Owner 吴光红
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