Detection method for ofloxacin enantiomer in seawater

The technology of ofloxacin and enantiomer is applied in the field of rapid and efficient detection of ofloxacin enantiomer in seawater, and can solve the problems of high cost of ofloxacin enantiomer, long separation time, complicated operation and the like, Achieve the effect of optimized solid phase extraction conditions, good linear relationship and simple operation

Inactive Publication Date: 2016-08-03
ZHEJIANG OCEAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The purpose of the present invention is to provide a fast, high-precision, simple-to-operate, and low-precision defect in order to solve the existing crystallization method to detect ofloxacin enantiomers with high cost, long separation time, narrow applicability, complicated operation and low precision. Inexpensive method for detection of ofloxacin enantiomers in seawater

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  • Detection method for ofloxacin enantiomer in seawater

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Embodiment 1

[0024] A method for detecting ofloxacin enantiomers in seawater, comprising the following steps:

[0025] 1) Pretreatment: vacuum filter the seawater, then adjust the pH to 2, vacuum filter again, and store at 0-4°C to obtain pretreated seawater;

[0026] 2) Extraction: use methanol, L-(-)-p-methyldibenzoyl tartaric acid, HLB solid-phase extraction column activated by oxalic acid aqueous solution containing ammonium citrate in sequence, and take the seawater pretreated in step 1) to pass through the column, The flow rate of the column was 6mL / min. After the extraction was completed, it was rinsed with deionized water, sucked dry under negative pressure, and eluted twice with methanol solution containing 10% volume fraction. The flow rate of the eluent was 1.2mL / min. Remove the liquid in a nitrogen blowing apparatus in a water bath at 30°C, blow dry with nitrogen, redissolve the residue with ethanol, filter with 0.21 μm micropore nanofiltration, and use the filtrate for later u...

Embodiment 2

[0029] A method for detecting ofloxacin enantiomers in seawater, comprising the following steps:

[0030] 1) Pretreatment: vacuum filter the seawater, then adjust the pH to 3, vacuum filter again, and store at 0-4°C to obtain pretreated seawater;

[0031] 2) Extraction: use methanol, L-(-)-p-methyldibenzoyl tartaric acid, HLB solid-phase extraction column activated by oxalic acid aqueous solution containing ammonium citrate in sequence, and take the seawater pretreated in step 1) to pass through the column, The flow rate of the column was 7mL / min. After the extraction was completed, it was rinsed with deionized water, dried under negative pressure, and eluted with methanol solution containing 12% volume fraction in three times. The flow rate of the eluent was 1.3mL / min. Remove the liquid in a nitrogen blowing apparatus in a water bath at 33°C, blow dry with nitrogen, redissolve the residue with ethanol, filter with 0.22 μm micropore nanofiltration, and use the filtrate for lat...

Embodiment 3

[0034] A method for detecting ofloxacin enantiomers in seawater, comprising the following steps:

[0035] 1) Pretreatment: vacuum filter the seawater, then adjust the pH to 4, vacuum filter again, and store at 0-4°C to obtain pretreated seawater;

[0036] 2) Extraction: use methanol, L-(-)-p-methyldibenzoyl tartaric acid, HLB solid-phase extraction column activated by oxalic acid aqueous solution containing ammonium citrate in sequence, and take the seawater pretreated in step 1) to pass through the column, The flow rate of the column was 9mL / min. After the extraction was completed, it was rinsed with deionized water, dried under negative pressure, and eluted with methanol solution containing 13% volume fraction in 5 times. The flow rate of the eluent was 1.5mL / min. Remove the liquid in a nitrogen blowing apparatus in a water bath at 35°C, blow dry with nitrogen, redissolve the residue with ethanol, filter with 0.23 μm micropore nanofiltration, and use the filtrate for later u...

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Abstract

The invention relates to a method for detecting the enantiomer of ofloxacin in seawater, which comprises the following steps: vacuum filter the seawater, then adjust the pH to 2-4, and vacuum filter again to obtain pretreated seawater; Phase extraction column, seawater passes through the column, after the extraction is completed, rinse with deionized water, vacuum dry, and elute in 2-5 times, and the eluent is dried in a nitrogen blowing instrument in a water bath at 30-35°C , the residue was redissolved with ethanol, micropore nanofiltration, and the filtrate was used for later use; the concentration of the enantiomer of ofloxacin was detected by high performance liquid chromatography. The present invention optimizes the solid-phase extraction conditions, so that the time of solid-phase extraction is shortened and the efficiency becomes high, while the high-performance liquid chromatography method for analyzing the concentration of ofloxacin enantiomers has high precision, fast speed, simple operation and low cost. Low; the detection method has a good linear relationship to the target compound, high recovery rate, small relative deviation, low toxicity of the reagents used, less usage, and is environmentally friendly.

Description

technical field [0001] The invention relates to a method for rapidly and efficiently detecting the enantiomer of ofloxacin in seawater. Background technique [0002] Ofloxacin is a synthetic broad-spectrum antibacterial drug, which has a good inhibitory effect on Gram-positive bacteria, Gram-negative bacteria, mycoplasma, chlamydia and Legionella. In addition, ofloxacin also has It has the advantages of good absorption, low antibacterial concentration, high antibacterial activity, not easy to produce drug-resistant bacteria, and low toxicity. It has been widely used in aquaculture at present. Ofloxacin is a chiral drug containing two chiral enantiomers at one chiral center. Studies have shown that levofloxacin is the main active ingredient in the two enantiomers of ofloxacin, while the activity of dexofloxacin is very low; in addition, the antibacterial activity of levofloxacin is also higher than that of ofloxacin racemic It is more soluble in water, and its water solubil...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88G01N30/06
CPCG01N30/88G01N30/06
Inventor 欧阳小琨杨立业王艳飞王阳光高小峰
Owner ZHEJIANG OCEAN UNIV
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