A solid-phase extraction column for trace analysis of tetracycline antibiotics and its application

A solid-phase extraction column and trace technology, which is applied in the direction of analyzing materials, measuring devices, and material separation, can solve the problems of unsatisfactory TCs recovery rate and insufficient specificity of tetracycline antibiotics, and achieve small relative deviation and high selectivity. Strong, easy-to-operate effects

Active Publication Date: 2020-05-05
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, most of the literature shows that these commonly used solid-phase extraction columns are not specific enough for tetracycline antibiotics, and the recovery rate of TCs (10%-86.2%) is not very ideal

Method used

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  • A solid-phase extraction column for trace analysis of tetracycline antibiotics and its application
  • A solid-phase extraction column for trace analysis of tetracycline antibiotics and its application
  • A solid-phase extraction column for trace analysis of tetracycline antibiotics and its application

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Experimental program
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Effect test

Embodiment 1

[0080] First, determine the standard working curve based on the detection method of the present invention, the specific steps are as follows:

[0081] (a) Prepare a mixed standard stock solution: use 50% methanol / water solution (v / v) to prepare 5 kinds of TCs into a 100 mg / L mixed standard stock solution, and place it in a brown reagent bottle; at the same time, prepare 100 mg of TC-D6 / L stock solution, placed in a brown reagent bottle for use.

[0082] (b) Dilute the mixed standard stock solution in step (a) with 50% methanol / water solution (v / v) to different concentration gradients: 1, 2, 4, 10, 20, 40, 100, 200 and 500 μg / L, At the same time, add TC-D6 solution to each concentration gradient sample, so that each concentration gradient contains an internal standard solution of equal concentration (100 μg / L);

[0083] (c) Use LC-MS / MS to analyze each concentration gradient sample, use the above-mentioned optimized liquid chromatography operating parameters and mass spectrom...

Embodiment 2

[0098] Continue to detect typical 5 kinds of tetracycline antibiotics in the water source according to the method of the present invention, comprise the following steps:

[0099] (1) Sample pretreatment:

[0100] Select a water sample from a water source in East China, use a 0.7 μm glass fiber membrane as a filter to remove suspended solids, adjust the pH to 5.0 and add complexing agent Na 2 EDTA, then add 100μg / L internal standard TC-D6 to complete the pretreatment;

[0101] (2) Concentration and enrichment of target TCs:

[0102] First use 5mL of equal volumes of methanol and ultrapure water to pass through the new solid-phase extraction column successively for activation, then take 1000mL of the water sample pretreated in step (1) for column extraction and enrichment, and then take 5% methanol / water solution ( v / v) was used as the eluent to rinse the small column, and dried in vacuum for 20min to remove moisture, then continued to use 10mL formic acid / methanol solution (7...

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Abstract

The invention relates to a novel solid-phase extraction column for trace analysis of tetracycline antibiotics and application of the novel solid-phase extraction column. An application method specifically comprises the steps: the adopted novel solid-phase extraction column achieves effective enrichment and separation of the tetracycline antibiotics through hydrogen bonds, pi-pi bonds and the electrostatic adsorption effect, selectivity is high, the anti-matrix effect is high, and meanwhile the five types of tetracycline antibiotics in water are quantitatively analyzed and detected through HPLC-MS / MS. Compared with the prior art, the detection result accuracy is reliable, the detection limit is low, and the novel solid-phase extraction column can be effectively applied to detection and quantitative analysis of the trace tetracycline antibiotics in faeces, soil, surface water and drinking water.

Description

technical field [0001] The invention belongs to the technical field of trace antibiotics, and relates to a novel solid-phase extraction column used for trace analysis of tetracycline antibiotics in water environment and its application. Background technique [0002] Tetracycline antibiotics (TCs) are a class of broad-spectrum antibiotics discovered in the 1940s, which can treat infections caused by Gram-positive and negative bacteria, intracellular mycoplasma, chlamydia and rickettsia, and are widely used Disease treatment and animal husbandry. However, because only a small part of TCs is bioabsorbed and degraded in the organism, most of them are excreted in the form of the parent body, and migrate into the water environment in nature through surface runoff, which directly affects human health. At the same time, long-term exposure of TCs in the environment will induce Production of resistant bacteria and transfer of resistance genes. Therefore, the residual situation of TC...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/60G01N30/06G01N30/02
CPCG01N30/02G01N30/06G01N30/60G01N2030/062
Inventor 崔长征胡军张天阳曹赞张申平姚诗杰胡亚茹任静冉雨灵薛佳佳张磊赵剑锋
Owner EAST CHINA UNIV OF SCI & TECH
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