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A method for simultaneous enrichment and detection of quinolone antibiotics in drinking water based on SPE column

A quinolone and antibiotic technology, which is applied in the field of new SPE column for simultaneous enrichment and detection of quinolone antibiotics in drinking water, can solve the problem of few detection types, and achieve the effects of saving sample testing time, high sensitivity and small relative deviation.

Active Publication Date: 2020-03-31
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Compared with the previous method, this method is simple to operate, low in cost, and highly specific to quinolone antibiotics. However, as far as the quinolone substances that may remain in the water environment are concerned, it only targets 4 kinds of quinolone antibiotics, and there are few types of detection.

Method used

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  • A method for simultaneous enrichment and detection of quinolone antibiotics in drinking water based on SPE column
  • A method for simultaneous enrichment and detection of quinolone antibiotics in drinking water based on SPE column
  • A method for simultaneous enrichment and detection of quinolone antibiotics in drinking water based on SPE column

Examples

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Embodiment 1

[0103] A method for the simultaneous enrichment and detection of typical quinolone antibiotics in drinking water based on a novel SPE column of reversed-phase / ion-exchange mixed-mode chromatographic packing. The specific steps for making a standard working curve are as follows:

[0104] (a) Prepare mixed standard stock solution: use 40%-80% methanol / water solution (v / v) to mix 9 kinds of QNs of known concentration to prepare a mixed standard stock solution with the same concentration of single QNs, and place in brown reagent in the bottle;

[0105] (b) Dilute the mixed standard stock solution in step (a) with 40%-80% methanol / water solution (v / v) to different concentration gradients: 1, 2, 5, 10, 20, 50, 80, 100 and 200 μg / L, add CIP-D to each concentration gradient sample at the same time 8 Prepare 100μg / L internal standard working solution;

[0106] (c) Use LC-MS / MS to analyze each concentration gradient sample, and use the above-mentioned optimized liquid chromatography ...

Embodiment 2

[0112] A method for the simultaneous enrichment and detection of nine typical quinolone-like antibiotics in drinking water based on a novel SPE column of reversed-phase / ion-exchange mixed-mode chromatographic packing materials, comprising the following steps:

[0113] (1) Sample pretreatment:

[0114] Select a water sample from a water source in East China, use a 0.45 μm glass fiber membrane as a filter to remove suspended solids, adjust the pH to 5.0-9.5 and add complexing agent Na 2 EDTA, then add a known amount of 100μg / L internal standard to complete the pretreatment;

[0115] (2) Concentration and enrichment of target QNs:

[0116] First use 5-10mL of equal volumes of methanol and ultrapure water to pass through the SPE cartridge (reversed-phase / ion-exchange mixed mode chromatographic packing solid-phase extraction cartridge is used in this example) for activation, and then take 500mL of step (1) for pretreatment The final water sample was enriched by column extraction,...

Embodiment 3

[0125] A method for the simultaneous enrichment and detection of nine typical quinolone-like antibiotics in drinking water based on a novel SPE column of reversed-phase / ion-exchange mixed-mode chromatographic packing materials, comprising the following steps:

[0126] (1) Sample pretreatment:

[0127] Select a water sample from a water source in East China, use a 0.45 μm glass fiber membrane as a filter to remove suspended solids, adjust the pH to 5.0-9.5 and add complexing agent Na 2 EDTA, then add a known amount of 100μg / L internal standard to complete the pretreatment;

[0128] (2) Concentration and enrichment of target QNs:

[0129] First use 5-10mL of equal volumes of methanol and ultrapure water to pass through the SPE cartridge (reversed-phase / ion-exchange mixed mode chromatographic packing solid-phase extraction cartridge is used in this example) for activation, and then take 500mL of step (1) for pretreatment The final water sample was enriched by column extraction,...

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Abstract

The invention relates to a method for simultaneously detecting and enriching quinolone antibiotics in drinking water based on an SPE column. The method comprises the following steps: concentrating andenriching a pre-treated water sample by a solid phase extraction column with a reverse phase / ion exchange mixed mode chromatographic packing, analyzing and detecting the concentrated water sample through high performance liquid chromatography-tandem mass spectrometry (HPLC-MS / MS), and detecting the concentrations of the quinolone antibiotics in the water sample according to the analytical chromatogram of the sample and the standard working curve of each antibiotic. Compared with the prior art, the method adopting the SPE-HPLC-MS / MS to realize the simultaneous enrichment and detection of trace(tiny) amounts of typical quinolone antibiotics in drinking water has the advantages of reliable detection result precision, low detection limit and small relative standard deviation, and can be effectively applied to the detection and the quantitative analysis of a trace (tiny) amount of quantalone in feces, soil, surface water and drinking water.

Description

technical field [0001] The invention relates to a detection and analysis technology for trace (micro) organic pollutants in water environment, in particular to a method for simultaneously enriching and detecting quinolone antibiotics in drinking water using a novel SPE column based on reversed-phase / ion-exchange mixed-mode chromatographic packing. Background technique [0002] Quinolones (QNs) antibiotics are a class of artificially synthesized antibiotics with broad-spectrum resistance, strong antibacterial power, strong penetrating power, high efficiency, low toxicity, and long half-life. They are widely used in humans, animal husbandry, etc. Prevention and treatment of existing bacterial diseases. However, because only a small part of QNs antibiotics is bioabsorbed and degraded in the organism, most of them are excreted in the form of the mother, and migrate into the drinking water environment in nature through surface runoff, directly affecting human health. At the same ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/08G01N30/86
CPCG01N30/08G01N30/8631
Inventor 崔长征张天阳金郁韩琪胡亚茹曹赞雷丹丹姚诗杰奚桢浩王漫莉任静徐晓庆
Owner EAST CHINA UNIV OF SCI & TECH
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