Method for simultaneous detection of ofloxacin and sarafloxacin in water body

A technology of ofloxacin and sarafloxacin, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems that the influence of impurities cannot be ruled out, and the separation time is long, so as to achieve short detection time, strong selectivity, and high usage little effect

Inactive Publication Date: 2013-10-09
CHINESE RES ACAD OF ENVIRONMENTAL SCI
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Problems solved by technology

High-performance liquid chromatography has high automation and good reproducibility, but for environmental samples with complex components, the sep

Method used

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  • Method for simultaneous detection of ofloxacin and sarafloxacin in water body
  • Method for simultaneous detection of ofloxacin and sarafloxacin in water body
  • Method for simultaneous detection of ofloxacin and sarafloxacin in water body

Examples

Experimental program
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Example Embodiment

[0048] Example 1: Recovery experiment

[0049] Take 1000ml ultrapure water and 1000ml actual water sample in a brown glass bottle, add 1ml100μg / L two trace fluoroquinolone antibiotics mixed standard stock solution to each bottle of water sample, and adjust the pH of the water sample to about 3.0 with acid after mixing. , Use GF / F (Whatman, 0.7μm) glass fiber filter membrane to filter to obtain the pretreated water sample. Use 6mL chromatographic pure acetone, 6mL chromatographic pure methanol, 6mL 5mM 0.1% formic acid aqueous solution to activate the HLB (Waters, 500mg, 6cc) solid phase extraction column, and finally add 5mL ultrapure water to keep the resin in the cartridge in an activated state, take 500~ 1000mL water sample is passed through the column, and the flow rate is controlled to be 3.0-5.0mL / min; after the enrichment is completed, the HLB solid phase extraction column is dried under nitrogen protection for 20 minutes, and then 10mL of eluent is used to elute the HLB c...

Example Embodiment

[0054] Example 2: The results of standard addition and recovery of water samples in Beijing Olympic Park.

[0055] A sample of 1000 ml of Beijing Olympic Park river water was placed in a brown glass bottle, and a standard addition experiment was carried out according to the method in Example 1. At the same time, a sample of 1000 ml of river water was taken without adding standard as a blank control.

[0056] The result of the spiked water sample is brought into the standard curve equation, and the concentration of the three sulfonamide antibiotics in the water sample to be tested is finally obtained by calculation. Calculate the recovery rate, and the results are shown in Table 2.

Example Embodiment

[0057] Example 3: Measurement results of actual water samples from Wangyanggou, Shijiazhuang, Hebei.

[0058] Take 1000ml of Shijiazhuang Wangyanggou River water sample in a brown glass bottle, and perform the standard addition experiment according to the method in Example 1.

[0059] The concentration of two FQs in the sample was determined by high performance liquid chromatography-tandem mass spectrometry. The calculation results show that two FQs, namely ofloxacin and sarafloxacin, were detected in the water samples of the Wangyanggou River in Shijiazhuang: 4.36 and 3.916 ng / L.

[0060] Table 1

[0061]

[0062] Table 2

[0063]

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Abstract

The invention relates to a method for simultaneous detection of ofloxacin and sarafloxacin in water body. The method mainly comprises the following steps of adjusting a pH value of a water sample to 2-4 by an acid; filtering the water sample to obtain a pretreated water sample; activating an HLB solid-phase extraction column by acetone, methanol and a formic acid aqueous solution containing ammonium acetate successively; adding ultrapure water to keep a resin in the HLB solid phase extraction column in an activated state; passing the water sample through the column; drying the HLB solid-phase extraction column under the protection of nitrogen after enrichment is finished; eluting with an eluent; collecting the eluent; drying under a nitrogen flow; adding acetonitrile to dissolve residual materials for detection; and detecting the concentrations of ofloxacin and sarafloxacin quantitatively. The method is advantageous in that the pretreatment of the water sample is environment-friendly; and the method can be operated easily, has high enrichment coefficient, and can analyze the content of two trace fluoroquinolone antibiotics in a water environment rapidly and accurately.

Description

technical field [0001] The invention belongs to the technical field of detection of water environmental pollutants, in particular to a method for detecting the content of two trace fluoroquinolone antibiotics in water, more specifically for trace amounts of ofloxacin and sarafloxacin in surface water detection method. Background technique [0002] Fluoroquinolones (FQs) antibiotic drugs are a class of artificially synthesized antibacterial drugs, which have good antibacterial effects on Gram-negative bacteria and Gram-positive bacteria, because of their strong tissue penetration, low toxicity, and more It is widely used because of high drug tolerance and longer half-life. Fluoroquinolone antibiotics include norfloxacin (NOR), ciprofloxacin (CIP), ofloxacin (OFL), lomefloxacin (LOM), difloxacin (DIF), sarafloxacin (SAR) etc. Although some of these compounds can be absorbed by humans and livestock, and removed in sewage treatment processes, a large number of compounds are st...

Claims

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Application Information

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IPC IPC(8): G01N30/88
Inventor 席北斗卢义许其功丁京涛高如泰张慧梁琼张媛
Owner CHINESE RES ACAD OF ENVIRONMENTAL SCI
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