Synchronous separation/enriched pretreatment method used for detecting trace fluoroquinolones in environmental water sample

A technology for fluoroquinolones and environment detection, which is applied in measurement devices, material separation, and analysis of materials, etc., can solve the problems of long processing time, secondary pollution of the environment, and large amount of organic solvents used, and achieves easy operation, saving raw materials, Separation-friendly effect

Inactive Publication Date: 2015-11-11
JILIN NORMAL UNIV
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0004] In order to solve the shortcomings of the existing separation / enrichment pretreatment methods, such as large amount of organic solvent used, long processing time, and secondary pollution to the environment, the present invention provides a method for detecting trace fluoroquinolones in environmental water samples. Synchronous separation / enrichment pretreatment method, the specific steps are as follows:

Method used

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  • Synchronous separation/enriched pretreatment method used for detecting trace fluoroquinolones in environmental water sample
  • Synchronous separation/enriched pretreatment method used for detecting trace fluoroquinolones in environmental water sample
  • Synchronous separation/enriched pretreatment method used for detecting trace fluoroquinolones in environmental water sample

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] (1) Mix the aqueous solution containing ciprofloxacin (CIP) and lomefloxacin (LOM) with (NH 4 ) 2 SO 4 Mix and make the phase-forming salt concentration be the (NH 4 ) 2 SO 4 solution;

[0041] (2) (NH) containing ciprofloxacin (CIP) and lomefloxacin (LOM) 4 ) 2 SO 4 After the solution is mixed with the EOPO solution with a concentration of 80% (w / w) according to the volume ratio of 47:3, shake it fully to dissolve it;

[0042] (3) above-mentioned mixed solution is left standstill in flotation cell to make it phase separation;

[0043] (4) Nitrogen is introduced from the bottom of the flotation cell for air flotation solvent flotation, and the nitrogen flow rate is 10-30mL min -1 , the flotation time is more than 30min;

[0044] (5) After the flotation is finished, take out the upper phase (EOPO phase) and transfer it to a container and add distilled water with 10% volume of the upper phase;

[0045] (6) Place the container with the upper phase at a temperatu...

Embodiment 2

[0051] Embodiment 2 (selection of phase forming salt)

[0052] Selection of a suitable phase-forming salt is an important factor in aqueous two-phase extraction. Therefore, the experiment discussed the CIP and LOM in different EOPO-((NH 4 ) 2 SO 4 ,NaH 2 PO 4 ,KCl,Na 2 SO 4 , K 2 HPO 4 or K 2 CO 3 ) distribution behavior in SPATPF, and the flotation rates of each system studied for CIP and LOM are listed in Table 1. As can be seen from the table, EOPO-(NH 4 ) 2 SO 4 The flotation rates of SPATPF to CIP and LOM were significantly higher than other systems, therefore, the selection of (NH 4 ) 2 SO 4 Construct SPATPF as a phase-forming salt to separate and enrich CIP and LOM by flotation.

[0053] Table 1

[0054]

Embodiment 3

[0055] Embodiment 3 ((NH 4 ) 2 SO 4 Effect of concentration on separation / enrichment)

[0056] Experiments discussed for EOPO-(NH 4 ) 2 SO 4 SPATPF at the same temperature, (NH 4 ) 2 SO 4 The influence of the concentration of CIP and LOM on the distribution of CIP and LOM in the system, and the change trend of its flotation rate with the concentration is plotted in figure 2 middle. From figure 2 It can be seen that, in general, the flotation rates of CIP and LOM vary with (NH 4 ) 2 SO 4 The concentration increases, this is because the system (NH 4 ) 2 SO 4 The increase of , will enhance the salting-out ability of the system, promote EOPO to drive CIP and LOM to precipitate from the salt phase, and phase transfer upward; when (NH 4 ) 2 SO 4 After the concentration exceeds 45%, continue to increase (NH 4 ) 2 SO 4 , the flotation rate did not increase significantly, which may be due to (NH 4 ) 2 SO 4 The salting-out effect has reached the maximum value a...

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Abstract

The invention relates to a pretreatment method for synchronously separating/enriching/detecting trace fluoroquinolones in an environmental water sample. According to the pretreatment method disclosed by the invention, by taking the establishment of an intelligent polymer aqueous two-phase gas solvent sublation method and combining the pretreatment method with high performance liquid detection, the trace fluoroquinolones in the environmental water sample are synchronously separated/enriched/detected. According to the pretreatment method, an intelligent polymer ethylene oxide propylene oxide (EOPO) copolymer is introduced into an aqueous two phase system, and two problems that the polymer cannot be recycled and target objects and the polymer cannot be separated in the aqueous two phase system are solved simultaneously; according to the pretreatment method, the intelligent aqueous two phase system is coupled with a gas solvent sublation technology, therefore not only is the defect that the enrichment multiple of the aqueous two phase system is low solved but also the problem of the environmental pollution of the gas solvent sublation technology is solved. The result shows that the pretreatment method disclosed by the invention has a very good separation, enrichment and detection effect on the fluoroquinolones in the practical sample under the optimum sublation condition, and EOPO can be recycled.

Description

technical field [0001] The invention belongs to the technical field of organic matter detection and analysis. Background technique [0002] Fluoroquinolone antibiotics use bacterial DNA (deoxyribonucleic acid) as the target point, and inhibit the replication process of bacterial DNA so that it cannot spread, thereby achieving antibacterial effects. Due to their broad antibacterial spectrum and strong antibacterial effect, fluoroquinolone antibiotics are widely used in aquaculture, resulting in high concentrations of these antibiotics in their adjacent waters. Although all countries have realized the serious threat of fluoroquinolone antibiotics to human health, fluoroquinolone antibiotics are still widely used in the aquaculture industry because of their good curative effect on some infectious diseases, low price and stable antibacterial effect. Therefore, in order to prohibit and eliminate the abuse of fluoroquinolone antibiotics in the aquaculture industry, it is very imp...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/08
Inventor 逯洋闫永胜丛飚陈波谭振江
Owner JILIN NORMAL UNIV
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