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Detection method of tetracycline antibiotics in water sample

A technology of tetracyclines and detection methods, applied in the direction of measuring devices, instruments, scientific instruments, etc.

Inactive Publication Date: 2017-06-20
ZHEJIANG RES INST OF CHEM IND CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Existing studies on tetracycline residues focus on analytical detection

Method used

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  • Detection method of tetracycline antibiotics in water sample
  • Detection method of tetracycline antibiotics in water sample
  • Detection method of tetracycline antibiotics in water sample

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Embodiment 1, the preparation of standard solution

[0037] Six kinds of 1000mg·L -1 Standard stock solution of tetracycline antibiotics: take epitetracycline (ETC), oxytetracycline (OTC), tetracycline (TC), demeclocycline (DMC), chlortetracycline (CTC), anhydrotetracycline (ATC) respectively ) each 10mg (accurate to 0.0001g) in a 10mL brown volumetric flask, dissolved in methanol to the mark, and shake well. All standard stock solutions were stored in a dark, -4°C refrigerator for later use.

[0038] 1000μg·L -1 Mixed standard stock solution of six tetracycline antibiotics: 1000mg·L -1 Standard stock solutions of epitetracycline (ETC), oxytetracycline (OTC), tetracycline (TC), demeclocycline (DMC), chlortetracycline (CTC), and anhydrotetracycline (ATC) were diluted step by step with methanol to 10mg·L -1 , to obtain standard stock solutions of epitetracycline (ETC), oxytetracycline (OTC), tetracycline (TC), demeclocycline (DMC), chlortetracycline (CTC) and anhydro...

Embodiment 2

[0039] Embodiment 2, sample pretreatment

[0040] 100mL water sample was passed through a 0.45μm filter membrane to remove suspended solids, and about 1.5mg of magnetic material was added, heated and stirred in a 40°C constant temperature water bath for 15min for magnetic solid-phase extraction, and the magnetic material after extraction was collected using a magnet, and the extracted magnetic material was discarded. watery. Then use 10 mL ammonia water (pH=11) to sonicate for 10 min for elution, collect the eluate under the action of a magnet, filter through a 0.45 μm filter membrane, and obtain the filtrate for use.

Embodiment 3

[0041] Embodiment 3, linear dependence and sensitivity of the method

[0042] According to the method described in Example 1, an appropriate amount of six tetracycline mixed standard solutions (1000 μg L -1 ), diluted with methanol to obtain mass concentrations of 1, 5, 10, 20, 50 and 100 μg L -1 The series of standard solutions, experiments show that six tetracyclines in 1 ~ 100μg L -1 The linear relationship between the peak area (y) and the mass concentration (x) of the quantitative ion within the mass concentration range is good, and the correlation coefficient r 2 ≥0.995, the limit of detection (LOD, S / N=3) and limit of quantification (LOQ, S / N=10) ranges are 2.44~25.21ng·L, respectively -1 and 8.14~84.03ng·L -1 . (See Table 2)

[0043] Table 2 Linear regression equation, correlation coefficient, detection limit and quantification limit of six tetracyclines

[0044] tetracycline antibiotics linear regression equation Correlation coefficient (r 2 )

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Abstract

The invention discloses a detection method of tetracycline antibiotics in a water sample, wherein the method comprises the steps: firstly, pretreating a water sample with a magnetic material, and then determining the content of the tetracycline antibiotics in a filtrate by high performance liquid chromatography and tandem mass spectrometry. The method provided by the invention can detect trace or ultra trace tetracycline antibiotics in water bodies, and has the advantages of simple and fast operation, green environmental protection, reliable results, low detection limit and good reproducibility.

Description

technical field [0001] The invention relates to a method for determining antibiotics, in particular to a method for detecting tetracycline antibiotics in water samples. Background technique [0002] Tetracycline antibiotics (Tetracycline antibiotics, TCs) are a class of broad-spectrum antibiotics produced by actinomycetes, including tetracycline, oxytetracycline, aureomycin, etc., and are widely used in the treatment of human diseases and in livestock and poultry breeding. Due to the extensive use of tetracycline antibiotics and their incomplete metabolism in living organisms and excretion into the water environment, the gradual accumulation of tetracycline antibiotics in the water environment may stimulate the selective genetic variation of microorganisms and lead to the emergence of antibiotics. Drug-resistant pathogens cause harm to environmental microbial populations and cause irreversible damage to water systems. [0003] In the prior art, methods for detecting tetracy...

Claims

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Application Information

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IPC IPC(8): G01N30/02
CPCG01N30/02G01N2030/027
Inventor 于峰国明贾科玲李姣
Owner ZHEJIANG RES INST OF CHEM IND CO LTD
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