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Method for rapidly detecting florfenicol and florfenicol amine in honey

The technology of florfenicol and florfenicol is applied in the field of rapid detection of florfenicol and florfenicol in honey, and can solve the problems of long test period, complicated pretreatment of solid-phase extraction column, and the like, To achieve the effect of simple and fast detection operation, good linear relationship, accurate qualitative and quantitative analysis

Pending Publication Date: 2021-06-22
淄博市疾病预防控制中心
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AI Technical Summary

Problems solved by technology

[0003] At present, the methods for detecting chloramphenicol residues mainly include high performance liquid chromatography, gas chromatography, gas chromatography-mass spectrometry, liquid chromatography-mass spectrometry, ultra-high performance liquid chromatography, ultra-high performance liquid chromatography- Mass spectrometry and enzyme-linked immunoassay, etc., but the solid-phase extraction column leads to cumbersome pre-treatment and long test cycle

Method used

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  • Method for rapidly detecting florfenicol and florfenicol amine in honey
  • Method for rapidly detecting florfenicol and florfenicol amine in honey
  • Method for rapidly detecting florfenicol and florfenicol amine in honey

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Embodiment 1

[0030] A kind of rapid detection method of florfenicol and florfenicol amine in honey, comprises the steps:

[0031] S1, standard solution preparation;

[0032] S1.1. Standard stock solution: Accurately weigh 10.0 mg of florfenicol, florfenicol amine, and chloramphenicol-d5 standard substance respectively, dissolve in methanol and dilute to 10 mL, and the mass concentration of the standard stock solution is 1.0 mg / mL, store in the dark below -20°C, and reserve, the purity of florfenicol, florfenicol amine and chloramphenicol-d5 is >99.0%;

[0033] S1.2. Standard intermediate solution: Accurately measure 100 μL of florfenicol and florfenicol amine standard stock solution respectively, dilute to 10 mL with methanol, the mass concentration of the standard intermediate solution is 10 μg / mL, and the internal standard standard intermediate solution: Accurately measure 100 μL of chloramphenicol-d5 standard stock solution, dilute to 10 mL with methanol, and the mass concentration of ...

Embodiment 2

[0045] 1. Materials and methods

[0046] 1.1 Reagents

[0047] Florfenicol and florfenicol amine standard products, and D5-chloramphenicol standard product were purchased from Dr. Ehrenstorfer GmbH in Germany, with a purity >99.0%; D3-florfenicol amine standard solution, with a fixed concentration of 5 mg / L, The customization unit is the Agricultural Product Quality Standard Research Center of the Ministry of Agriculture and Rural Affairs. Methanol, formic acid, acetonitrile, ethyl acetate, and acetone are chromatographically pure reagents from Merck, Germany; ammonia water is analytically pure reagents from Sinopharm. PSA and C18 solid phase extraction materials were purchased from Agilent Technologies Co., Ltd.;

[0048] For the selection of purification materials, the influence of purification materials on the recovery efficiency was investigated experimentally, and the purification effect was determined by the recovery rate of the negative honey sample added with the sta...

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Abstract

The invention discloses a method for rapidly detecting florfenicol and florfenicol amine in honey. The method comprises the following steps: S1, preparing a standard solution; s2, carrying out sample pretreatment; s3, carrying out experiment result and analysis; according to the method, a sample is extracted through ammoniated acetonitrile, the sample is purified through a QuEChERs method, the content of florfenicol and florfenicol amine in honey is measured at the same time through liquid chromatography-triple quadrupole tandem mass spectrometry, and quantification is conducted through an internal standard method. The result shows that the linear relation of florfenicol and florfenicol amine is good in the experimental concentration range, the detection limit ranges from 0.05 microgram / kg to 0.2 microgram / kg, the adding standard recovery rate ranges from 96.5% to 105%, and the relative standard deviation (RSD) ranges from 3.8% to 5.3%. According to the conclusion, the method is simple, convenient and rapid in detection operation, and accurate qualitative and quantitative analysis can be carried out on trace florfenicol and florfenicol amine in honey.

Description

technical field [0001] The invention belongs to the field of biological detection, and more specifically relates to a rapid detection method for florfenicol and florfenicol amine in honey. Background technique [0002] Honey is produced by bees brewing nectar or honeydew, etc. It is a natural nutrient and is very popular among people. Bees, like other organisms, are susceptible to bacterial infection, viral invasion, etc. Certain bee diseases, such as brood disease, can be treated with antibiotics. However, misuse of antibiotics (for example, with excessive doses for treatment or use as growth promoters) may lead to the accumulation of antibiotics in honey. Coupled with its longer half-life, it is more likely to cause residue and accumulation, and increase human resistance to pathogenic bacteria. As a new type of broad-spectrum antibacterial drug of chloramphenicol, florfenicol is also a special antibiotic drug for animals. Broad-spectrum antibacterial effect, and signifi...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/14G01N30/72
CPCG01N30/02G01N30/06G01N30/14G01N30/72G01N2030/027G01N2030/062G01N2030/146
Inventor 邢燕王勤王钟高慧李婷婷于俊丽王敏
Owner 淄博市疾病预防控制中心
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