High performance liquid chromatography determination method of tetracycline antibiotic in soil

A technology of high performance liquid chromatography and tetracyclines, which is applied in the field of high performance liquid chromatography determination of tetracycline antibiotics in soil, can solve the problems of incomplete separation of target analytes, poor peak shape of chromatographic peaks, and long detection time, etc. Purification and enrichment effect, good peak shape, and short operation time

Inactive Publication Date: 2012-04-04
SICHUAN AGRI UNIV
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Problems solved by technology

In recent years, new high-performance liquid chromatography methods for the detection of antibiotics in soil have been continuously established in China, but there are deficiencies such as low recovery rate, long detection time, poor chromatographic peak shape, and incomplete separation of target analytes. Find a more efficient method for the detection of tetracycline antibiotics in soil

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  • High performance liquid chromatography determination method of tetracycline antibiotic in soil
  • High performance liquid chromatography determination method of tetracycline antibiotic in soil
  • High performance liquid chromatography determination method of tetracycline antibiotic in soil

Examples

Experimental program
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Effect test

Embodiment 1

[0035] Taking the soil from the forest farm of Sichuan Agricultural University as the test soil, the contents of tetracycline, oxytetracycline and chlortetracycline were all below their detection limits. The soil samples to be tested were naturally air-dried and passed through a 60-mesh nylon sieve for later use.

[0036] Accurately weigh 0.1000g of each antibiotic standard (oxytetracycline, tetracycline, chlortetracycline) in a 200mL beaker, dissolve it with methanol, transfer it to a 1000mL brown volumetric flask, wash the beaker 3-5 times with methanol repeatedly, and wash the solution Transfer them together into a volumetric flask, then dilute to volume with methanol and shake well to obtain a 100 μg / mL standard stock solution, which should be stored in a refrigerator at 4°C.

[0037] Accurately pipette 5.00mL of each standard stock solution into a 500mL brown volumetric flask, dilute with methanol, shake well and make up to volume to obtain a 1μg / mL mixed standard solutio...

example 2

[0052] Example 2: On-the-spot collection of feces and biogas samples from 2-3 large farms in Zhihe Town, Jiuchi Town, Mengyang Town, Shengping Town, Lichun Town and Sanjie Town in Pengzhou City after harmless treatment liquid, the soil sample of the vegetable planting land applied with farm manure.

[0053] Soil sample collection and preparation: Collect the soil in the plow layer (0-20cm), avoiding the composting site and the edge of the field. Each mixed soil sample is obtained by mixing multiple single-point samples evenly and reducing them by the quartering method, weighing about 1kg, and putting them in a clean and sealed bag, keeping them away from light and bringing them back at low temperature. After the soil samples were air-dried indoors, they were finely ground and passed through a 60-mesh nylon sieve for later use.

[0054] Fecal sample collection and preparation: Collect fecal samples from representative large-scale farms after harmless treatment. Fecal samples ...

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Abstract

The invention relates to an environmental analysis detection method, and specifically, relates to a high performance liquid chromatography determination method of tetracycline antibiotic in soil. The high performance liquid chromatography determination method of tetracycline antibiotic in soil comprises the following steps of 1, a sample collecting and preparation process comprising collecting soil in a plough layer having thickness of 0 to 20 centimeters, wherein soil in a composting place and field edges is not adopted, uniformly mixing multiple single-point samples, carrying out quarteringreduction to obtain a mixed soil sample having weight of about 1kg, putting the mixed soil sample into a sealing bag, bringing the sealing bag with the mixed soil sample back with low-temperature preservation in the dark, putting the mixed soil sample into a room, drying in air, crushing, screening by a nylon sieve of 60 meshes, and weighing 2g of the mixed soil sample for next use, 2, an extractpreparation process, 3, an extraction, purification and enrichment process, and 4, an elution, volume metering and detection process. The high performance liquid chromatography determination method of tetracycline antibiotic in soil has normalized processes, reduces a vacuum drying process, produces low jamming, shortens operation time and improves operation accuracy. Through connection between astrong anion solid phase extraction column and a C18 inverted solid phase extraction column in series, purification and enrichment effects are greatly improved.

Description

technical field [0001] The invention relates to an environmental analysis and detection method, in particular to a high performance liquid chromatography detection method for tetracycline antibiotics in soil. Background technique [0002] Soil is one of the important components of the natural environment, an indispensable part of the biosphere, and the material basis for the survival of humans, animals and plants. Therefore, the quality of soil directly affects human production, life and development. When soil pesticide pollution has become a focus of attention and research, the problem of soil antibiotic pollution has emerged due to the abuse of antibiotics. Tetracyclines are acid-base amphoteric substances, easily soluble in acidic or alkaline solutions, relatively stable in weakly acidic solutions, and easily soluble in acidic solutions (pH<2), neutral or alkaline solutions (pH>7). The commonly used tetracycline antibiotics (TCs) are: tetracycline (Tetracycline...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
Inventor 伍钧张林杨刚沈飞张小洪张延宗王应军李黎漆辉
Owner SICHUAN AGRI UNIV
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