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Solid phase extraction and HPLC-fluorescence detection method for fluoroquinolones antibiotics

A technology for fluoroquinolones and fluorescence detection, which is applied in solid-phase extraction and HPLC-fluorescence detection of fluoroquinolone antibiotics, and in the field of detection of fluoroquinolone antibiotics, which can solve the problems of increased test costs, expensive instrument analyzers, and unfavorable popularization of detection methods and other problems to achieve the effect of lowering the detection limit and reducing the cost of testing

Inactive Publication Date: 2010-04-21
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Although the above existing methods can meet the requirements of environmental sample detection, the required instruments such as ESI-MS / MS analyzers are very expensive, resulting in increased test costs, which is not conducive to the popularization of detection methods

Method used

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  • Solid phase extraction and HPLC-fluorescence detection method for fluoroquinolones antibiotics
  • Solid phase extraction and HPLC-fluorescence detection method for fluoroquinolones antibiotics
  • Solid phase extraction and HPLC-fluorescence detection method for fluoroquinolones antibiotics

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Water sample pretreatment: take 100mL water sample from the outlet of Hangzhou Sibao Sewage Treatment Plant and filter it with medium-speed qualitative filter paper and 0.45μm water film, add 5mL Na with a concentration of 0.2g / L to the filtrate 2 EDTA aqueous solution, the pH was adjusted to 4.0 with acetic acid to obtain the pretreated water sample.

[0039] Solid phase extraction: sequentially use 1mL methanol, 1mL methanol, 1mL methanol and 5mL Na with a concentration of 0.2g / L 2 EDTA aqueous solution activates the solid phase extraction column.

[0040] Pass the pretreated water sample through the activated solid-phase extraction column at a speed of 3mL / min, and then use 5mL Na with a concentration of 0.2g / L 2 EDTA aqueous solution rinses the solid-phase extraction column, then evacuates for 30min, takes the concentrated ammonia solution (volume percent concentration is 25%) and the volume ratio of methanol and is eluted three times with the concentrated ammonia-...

Embodiment 2

[0048] Water sample pretreatment: Take 1000mL Hangzhou Qiantang River water sample and filter it with medium-speed qualitative filter paper and 0.45μm water film, add 2mL Na with a concentration of 0.2g / L to the filtrate 2 EDTA aqueous solution, the pH was adjusted to 4.0 with phosphoric acid to obtain the pretreated water sample.

[0049] Solid phase extraction: sequentially use 1mL methanol, 1mL methanol, 1mL methanol and 5mL Na with a concentration of 0.2g / L 2 EDTA aqueous solution activates the solid phase extraction column.

[0050] Pass the pretreated water sample through the activated solid-phase extraction column at a speed of 3mL / min, and then use 5mL Na with a concentration of 0.2g / L 2 EDTA aqueous solution rinses the solid-phase extraction column, then evacuates for 30min, takes the concentrated ammonia solution (volume percent concentration is 25%) and the volume ratio of methanol and is eluted three times with the concentrated ammonia-methanol solution of 2: 38, ...

Embodiment 3

[0056] Embodiment 3 recovery test

[0057] Get 5 parts of pure water and 5 parts of river water, each part of 1L and add a certain amount of OFL standard substance, NOR standard substance, CPX standard substance, ENRX standard substance to carry out the recovery rate experiment, according to the solid phase extraction treatment step in the embodiment 1 to water Samples were enriched and extracted, and HPLC-fluorescence assay was performed, a working curve was drawn according to the relationship between the peak height of the chromatogram and the concentration of the standard substance, and the recovery rate was calculated using the peak height. The results are shown in Table 3.

[0058] Table 3 Recovery test result

[0059]

[0060]

[0061] Seen from Table 3: the recoveries are all between 83.6~95.2%, and the RSDs are also all within 4.3%, showing that the method of the present invention has strong anti-interference ability, and can more accurately measure...

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Abstract

The invention discloses a solid phase extraction and HPLC-fluorescence detection method for fluoroquinolones antibiotics. The method comprises the following steps of passing a pretreated water sample through an activated solid phase extraction column; eluting the solid phase extraction column with a Na2EDTA aqueous solution; then vacuumizing; and finally, eluting the water sample for three times by a concentrated ammonia methanol solution with a concentrated ammonia volume percent concentration of 6 percent by 0.5-2mL each time. An obtained eluent is blow-dried to 0.1-0.4mL in air flow, water is added to reach a constant column of 1.0mL so as to obtain a test sample, and then HPLC-fluorescence detection is carried out. By adopting the solid phase extraction-HPLC-fluorescence detection technology and utilizing a conventional analytical instrument, the method can simultaneously measure the contents of four typical fluoroquinolones antibiotics of ofloxacin, norfloxacin, ciprofloxacin and enrofloxacin in the water sample. The method has simple operation and low cost and can be applied to the measurement of the ultratrace of four typical fluoroquinolones antibiotics in waste water and surface water.

Description

technical field [0001] The invention relates to a detection method for fluoroquinolone antibiotics, in particular to a solid-phase extraction and HPLC-fluorescence detection method for fluoroquinolone antibiotics, and belongs to the technical field of environmental monitoring. Background technique [0002] Fluoroquinolone antibiotics are a class of antibacterial drugs that have developed rapidly in recent years. They are widely used in humans and livestock because of their advantages such as broad antibacterial spectrum, strong antibacterial activity, long half-life, high efficiency and low toxicity, convenient use, and many dosage forms. and fish disease treatment and prevention, also often used as a growth promoter for livestock and fish. After taking fluoroquinolone antibiotics, a large part of them is excreted from the body of humans and animals in their original form and enters the sewer. Some of the drugs (about 70-80%) are removed by sewage treatment plants, and some ...

Claims

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Application Information

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IPC IPC(8): G01N30/74G01N30/06B01D15/08
Inventor 童裳伦卓霞军
Owner ZHEJIANG UNIV
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