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Method for detecting sulfonamide antibiotics in biogas slurry and sample treatment method

A sample processing and sulfonamide technology, applied in measuring devices, instruments, scientific instruments, etc., can solve the problems of serious interference in the detection of sulfa antibiotics, clogging of solid phase extraction columns, complex components, etc., and achieve simple and fast enrichment and separation process. The effect of increasing the contact area and high extraction efficiency

Active Publication Date: 2021-06-25
ZHEJIANG ACADEMY OF AGRICULTURE SCIENCES
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The composition of the biogas slurry is complex, and the detection of sulfonamide antibiotics directly using the biogas slurry as a sample has serious interference and is difficult to detect
For samples with complex components, it is generally pre-extracted and purified by using a solid-phase extraction column filled with adsorbent materials before subsequent instrumental analysis. You can refer to the pretreatment method for the detection of sulfa antibiotics in water, but during the purification process, solid-phase extraction The column is clogged seriously, reducing the quality of the sample and failing to meet the detection limit standard; and the solid phase extraction column has serious compound loss, poor repeatability of test results, time-consuming, laborious and high cost, cannot detect large quantities of samples, and has low efficiency question

Method used

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  • Method for detecting sulfonamide antibiotics in biogas slurry and sample treatment method
  • Method for detecting sulfonamide antibiotics in biogas slurry and sample treatment method
  • Method for detecting sulfonamide antibiotics in biogas slurry and sample treatment method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] Dissolve 20mg 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;

[0050] 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.

[0051] UIO-67@GO@Fe 3 o 4 -1 The particle size is between 2...

Embodiment 2

[0053] Accurately weigh 10mg, 15mg, and 25mg of GO and dissolve them in 20mL N,N-dimethylformamide solution for 6 hours by ultrasonic, and 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.

[0054] 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 T...

Embodiment 3

[0056] Dissolve 20mg 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;

[0057] 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.

[0058] UIO-67@GO@Fe ...

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Abstract

The invention discloses a method for detecting sulfonamide antibiotics in biogas slurry 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 biogas slurry sample to 3-7, carrying out magnetic solid-phase extraction by using UIO-67@GO@Fe3O4 powder, and blow-drying desorbed eluent to obtain a treated biogas slurry sample. The treated biogas slurry sample is directly determined by one or more of the existing sulfonamide 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 sulfonamide antibiotics in biogas slurry and a sample processing method thereof. Background technique [0002] The biogas slurry is the waste water produced by breeding and the manure water soaked in water. After dry-wet separation, the fecal residue is separated, and then the waste water is subjected to precipitation treatment, further dry-wet separation, and then anaerobic treatment (UASB reactor). Decompose part of the impurities, and then perform aerobic treatment (SBR reactor), and further decompose the impurities to produce organic fertilizer water that meets agricultural irrigation standards. At present, in order to promote animal growth and prevent diseases in livestock and poultry breeding, a variety of veterinary drugs such as tetracycline antibiotics and sulfonamide antibiotics are often used. The use of drugs causes more drug residue...

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 汪建妹钱鸣蓉徐彦吉小凤章虎周敏
Owner ZHEJIANG ACADEMY OF AGRICULTURE SCIENCES
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