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Method for detecting nitroimidazole antibiotics in honey and sample treatment method

A nitroimidazole and sample processing technology, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of easy clogging of solid phase extraction columns, loss of compounds, and reduction of sample quality, so that the enrichment and separation process is simple, fast, and efficient. The effect of increasing the contact area and high extraction capacity

Active Publication Date: 2021-06-25
ZHEJIANG UNIV OF TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the complexity of the components in honey, traditional adsorption material solid-phase extraction column is used for extraction. During the purification process, the solid-phase extraction column is easily blocked, and the quality of the sample is reduced and cannot reach the detection limit standard; and the solid-phase extraction column has serious compound loss and detection Technical issues with poor reproducibility of results, time-consuming, labor-intensive and high cost

Method used

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  • Method for detecting nitroimidazole antibiotics in honey and sample treatment method
  • Method for detecting nitroimidazole antibiotics in honey and sample treatment method
  • Method for detecting nitroimidazole antibiotics in honey and sample treatment method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] Dissolve 15mg GO in 20mL N,N-dimethylformamide solution ultrasonically for 6h, add 75mg Fe 3 o 4 (Particle size 100nm-150nm) Ultrasonic treatment for 10 minutes to disperse evenly to obtain a suspension;

[0049] Mix 112.5mg of zirconium tetrachloride in the above suspension, apply ultrasonication for 30min, and mechanically stir for 12h to disperse evenly, then add 100mg of 4,4'-biphenyldicarboxylic acid and stir for 30min, then mix evenly to obtain a mixed solution; put the mixed solution in Put it into an autoclave lined with polytetrafluoroethylene, put it in an oven and heat it at 120°C for 24h, wash the synthesized solid with ethanol and deionized water several times, and then separate it from the solution by magnetic separation; Freeze-dry at -50°C for 10 hours to obtain an off-white solid, and grind it sufficiently to obtain UIO-67@GO@Fe 3 o 4 Powder material, denoted as UIO-67@GO@Fe 3 o 4 -1.

[0050] UIO-67@GO@Fe 3 o4 -1 The particle size is between 200...

Embodiment 2

[0052] Accurately weigh 10mg, 20mg, and 25mg of GO and dissolve them in 20mL of N,N-dimethylformamide solution for 6 hours with ultrasound. The rest of the operations are the same as in Example 1 to obtain three kinds of UIO-67@GO@Fe 3 o 4 Powder material, recorded as UIO-67@GO@Fe in turn 3 o 4 -2, UIO-67@GO@Fe 3 o 4 -3. UIO-67@GO@Fe 3 o 4 -4.

[0053] UIO-67@GO@Fe 3 o 4 -2, UIO-67@GO@Fe 3 o 4 -3. UIO-67@GO@Fe 3 o 4 -4 The particle size is in the range of 200nm-250nm. UIO-67@GO@Fe 3 o 4 -2, UIO-67@GO@Fe 3 o 4 -3. UIO-67@GO@Fe 3 o 4 -4 XRD characteristic map with figure 1 The same, the XRD characteristic map shows: UIO-67@GO@Fe 3 o 4 There are 8 binary phases at 10°, 30°, 35°, 43°, 50°, 53°, 57°, 63°, proving that UIO-67, GO and Fe 3 o 4 Tight combination, successfully synthesized UIO-67@GO@Fe 3 o 4 . UIO-67@GO@Fe 3 o 4 -2, UIO-67@GO@Fe 3 o 4 -3. UIO-67@GO@Fe 3 o 4 The infrared spectrum of -4 and figure 2 Same, UIO-67 at 3423cm -1 、1370cm -1 ...

Embodiment 3

[0055] Dissolve 15mg GO in 20mL N,N-dimethylformamide solution ultrasonically for 5h, add 110mg Fe 3 o 4 (Particle size 100nm-150nm) Ultrasonic treatment for 10 minutes to disperse evenly to obtain a suspension;

[0056] Mix 100mg of zirconium tetrachloride in the above suspension, ultrasonically act for 30min, and mechanically stir for 12h to disperse evenly, then add 110mg of 4,4'-biphenyldicarboxylic acid and stir for 30min, then mix uniformly to obtain a mixed solution; put the mixed solution into In an autoclave lined with polytetrafluoroethylene, put it in an oven and heat it at 130°C for 24 hours. The synthesized solid is washed with ethanol and deionized water several times, and then separated from the solution by magnetic separation; the separated solid is subjected to - Freeze-dried at 45°C for 12 hours to obtain an off-white solid, which was thoroughly ground to obtain UIO-67@GO@Fe 3 o 4 Powder material, denoted as UIO-67@GO@Fe 3 o 4 -5.

[0057] UIO-67@GO@Fe ...

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Abstract

The invention discloses a method for detecting nitroimidazole antibiotics in honey and a sample treatment method. The sample treatment method comprises the following steps of: taking UIO-67@GO@Fe3O4 powder obtained by synthesizing graphene oxide, ferroferric oxide, zirconium tetrachloride and 4, 4'-diphenyldicarboxylic acid as an adsorption material; and adjusting the pH value of a honey sample to 3-7, carrying out magnetic solid-phase extraction by using the UIO-67@GO@Fe3O4 powder, and blow-drying desorbed eluent to obtain a treated honey sample. The treated honey sample is directly determined by adopting one or more of the existing nitroimidazole antibiotic determination methods. The method is simple and convenient to operate, time-saving and rapid, the adsorption material can be recycled, the detection result is accurate, and the method can be widely popularized and applied.

Description

technical field [0001] The invention relates to the technical field of antibiotic detection, in particular to a detection method of nitroimidazole antibiotics in honey and a sample processing method thereof. Background technique [0002] Rich in sugars, vitamins and minerals, honey has been used as food and medicine for thousands of years. Like all living things, bees are subject to diseases such as American larval rot and European hay fever. Due to the intensive and large-scale bee breeding mode, once an epidemic occurs in the bee farm, the infection speed is fast and the treatment is difficult, often causing huge economic losses. Although many veterinary medicines can be effectively treated, due to the particularity of bees, they can only be treated by feeding. It is difficult to control the dosage and time, and it is easy to cause veterinary medicine residues in honey. For example, nitroimidazole antibiotics and macrolide antibiotics, which are often used, will cause gr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/72
CPCG01N30/02G01N30/06G01N30/72G01N2030/062
Inventor 李祖光徐彦钱鸣蓉汪建妹章虎吉小凤周敏
Owner ZHEJIANG UNIV OF TECH
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