Detection method of flumequine chiral enantiomer in seawater

A detection method, the technology of flumequine, which is applied in the field of detection of chiral enantiomers of flumequine, can solve the problems of no detection of flumequine enantiomer residues, etc.

Inactive Publication Date: 2014-12-17
ZHEJIANG OCEAN UNIV
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Problems solved by technology

At present, there are many studies on the residue detection of flumequine racemate in aqu

Method used

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  • Detection method of flumequine chiral enantiomer in seawater
  • Detection method of flumequine chiral enantiomer in seawater
  • Detection method of flumequine chiral enantiomer in seawater

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Embodiment Construction

[0018] The present invention will be further described in detail below in conjunction with the accompanying drawings and embodiments.

[0019] A method for detecting chiral enantiomers of flumequine in seawater, comprising the following steps:

[0020] (1) Take 100 mL of cultured seawater in a beaker, add 1 mg to 2 mg of flumequine standard substance, and ultrasonically dissolve it completely. Take 3 to 5 mL of HLB solid-phase extraction cartridge (activated by 5 mL of methanol + 5 mL of water), and pass through 5 mL of After rinsing with deionized water, elute with 5-10mL methanol, and collect the eluate in a 10mL volumetric flask;

[0021] (2) The eluent in step (1) was blown to almost dry with methanol nitrogen, the raffinate was dissolved in ethanol and fixed to 3 mL, and filtered with a 0.22 μm microporous membrane to obtain solution A;

[0022] (3) The above-mentioned solution A is detected by high performance liquid chromatography; CHIRALCEL OD-H chiral column is selec...

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Abstract

The invention discloses a detection method of a flumequine chiral enantiomer in seawater. The method is characterized by comprising the following steps: taking 80-110mL of aquaculture seawater and adding in a beaker, adding 1mg-2mg of flumequine standard substance, performing ultrasonic treatment to completely dissolve the flumequine standard substance, taking 3-5mL of the obtained solution, treating by an HLB solid-phase extraction column, leaching by using 4-6mL of deionized water, and then eluting by using 5-10mL of methanol; nitrogen-blowing the eluent to nearly dry, redissolving by using ethanol, metering volume to 3mL, filtering by a millipore filter membrane with size of 0.22-0.45 micron to obtain a solution A; using n-hexane and ethanol in volume ratio of (10-40): (60-90) as a mobile phase, and adding methanoic acid with volume content of 0.1%-0.3% and ammonium acetate aqueous solution (5mmol/L) in the mobile phase to separate the flumequine chiral enantiomer; detecting the solution A by using high performance liquid chromatograph, wherein a CHIRALCEL OD-H chiral column is adopted, the column temperature is the room temperature, the flow velocity is 0.5mL/min to 0.7mL/min, and the wavelength is 254nm. By adopting the method disclosed by the invention, the flumequine chiral enantiomer can be successfully separated so that the residual quantity of the flumequine chiral enantiomer in the seawater can be detected, and basis is provided for the residual risk assessment and reasonable and safe use of flumequine in the seawater aquaculture.

Description

technical field [0001] The invention relates to a method for detecting chiral enantiomers of flumequine in seawater. Background technique [0002] Flumequine (FLU) is a second-generation fluoroquinolone antibacterial drug, which is a special antibacterial drug for animals. And aquatic animal diseases have good curative effect. Its mechanism of action is mainly to inhibit the A subunit of DNA gyrase and destroy its activity. As a result, the synthesis of deoxyribonucleic acid, ribonucleic acid and protein is disturbed, so that cells can no longer divide, thus playing a bactericidal effect. Due to its high safety, tolerance and unique high permeability, flumequine has been widely used in the prevention and treatment of bacterial diseases in aquatic animals. The solubility of flumequine in fresh water is not high, but it can be dissolved in seawater with a higher pH value. Therefore, flumequine is often used for immersion disinfection of sea fish. However, wastewater with fl...

Claims

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Application Information

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IPC IPC(8): G01N30/06G01N30/02
Inventor 高小峰聂晶欧阳小琨王阳光杨立业吴伟建郁迪徐红萍李维曾浩杜军李玄
Owner ZHEJIANG OCEAN UNIV
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