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Detection method of macrolide antibiotics in organic fertilizer and sample treatment method of macrolide antibiotics in organic fertilizer

A macrolide and sample processing technology, applied in measurement devices, instruments, scientific instruments, etc., can solve the problems of easy blockage of solid-phase extraction columns, failure to meet detection limit standards, and poor repeatability of test results. The effect of synergistic adsorption capacity, developed voids, and increased convenience

Active Publication Date: 2022-04-12
ZHEJIANG SHUREN COLLEGE ZHEJIANG SHUREN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Due to the complex components in organic fertilizers, the solid-phase extraction column of traditional adsorption materials is used for extraction. During the purification process, the solid-phase extraction column is easy to block, reducing the quality of the sample and failing to meet the detection limit standard; and the solid-phase extraction column has serious compound loss. , technical problems such as poor repeatability of test results, time-consuming, laborious and high cost

Method used

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  • Detection method of macrolide antibiotics in organic fertilizer and sample treatment method of macrolide antibiotics in organic fertilizer
  • Detection method of macrolide antibiotics in organic fertilizer and sample treatment method of macrolide antibiotics in organic fertilizer
  • Detection method of macrolide antibiotics in organic fertilizer and sample treatment method of macrolide antibiotics in organic fertilizer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Example 1Fe 3 o 4 Synthesis of @ZnO&MnO powder

[0042] Add manganese sulfate, thioacetamide, zinc sulfate, ethylene glycol and isopropanol into the three-necked flask, stir for 20 minutes and mix well, then add nano-Fe 3 o 4 (100nm), in which manganese sulfate, zinc sulfate, thioacetamide and Fe 3 o 4 The mass ratio of Fe is 1:1:2.5:0.16, Fe 3 o 4 The ratio of the number of milligrams of ethylene glycol to the number of milliliters of ethylene glycol and the number of milliliters of isopropanol is 1:0.4:0.4. Stir evenly and heat to 35°C ± 5°C. Stir and react at 35°C ± 5°C for 3 days (72h) ; Transfer the reaction solution to a hydrothermal kettle, and react at a constant temperature of 200° C. for 20 hours. After the reaction solution was cooled to room temperature, it was washed several times with pure water and ethanol, and the final product was vacuum-dried at 60°C for 6 hours, and the magnetic material Fe was obtained after grinding. 3 o 4 @ZnO & MnO powder...

Embodiment 2

[0045] Example 2 Fe 3 o 4 Synthesis of @ZnO&MnO powder

[0046] Add manganese sulfate, zinc sulfate, thioacetamide, ethylene glycol and isopropanol into the three-necked flask, stir for 20 minutes and mix well, then add nano-Fe 3 o 4 (100nm), of which manganese sulfate, zinc sulfate, thioacetamide, Fe 3 o 4 The mass ratio of Fe is 1:1:2.5:0.20, Fe 3 o 4 The ratio of the milligrams of ethylene glycol to the milliliters of ethylene glycol and the milliliters of isopropanol is 1:4:4, stir evenly and heat to 35°C±5°C, stir and react at 35°C±5°C for 60h; Transfer to a hydrothermal kettle, and react at a constant temperature of 220° C. for 25 hours. After the reaction solution was cooled to room temperature, it was washed several times with pure water and ethanol, and the final product was vacuum-dried at 60°C for 6 hours, and the magnetic material Fe was obtained after grinding. 3 o 4 @ZnO & MnO powder.

[0047] Magnetic material Fe 3 o 4 The XRD characteristic diagram ...

Embodiment 3

[0050] Fe 3 o 4 @ZnO&MnO Magnetic Solid Phase Extraction (MSPE) Macrolide Antibiotics in Organic Fertilizers:

[0051] Accurately weigh 1.0g of the organic fertilizer sample in a 25mL transparent glass sample bottle, add 100mg of the magnetic material Fe of Example 1 3 o 4 Add 10mL pH=7.0Na after @ZnO&MnO powder 2 EDTA-McIlvaine buffer solution, after vortex mixing, frequency 800rpm vibration extraction and adsorption for 20min. Then the magnetic material is adsorbed by an external magnet, and the solvent and the sample are poured and discarded, and the separated Fe 3 o 4 After @ZnO&MnO powder is washed with water, it is completely immersed in 5mL of eluent composed of acetonitrile and 25% mass percent ammonia water (wherein the volume of 25% mass percent ammonia water accounts for 5% of the eluent volume, denoted as 5 % ammonia acetonitrile) at a frequency of 800 rpm for desorption for 20 minutes, the magnetic material was adsorbed and separated by an external magnet, a...

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Abstract

The invention discloses a detection method of macrolide antibiotics in an organic fertilizer and a sample treatment method of the macrolide antibiotics. The sample treatment method comprises the following steps: synthesizing manganese sulfate, zinc sulfate, thioacetamide, ethylene glycol, isopropanol and ferroferric oxide to obtain Fe3O4 (at) ZnOamp; the method comprises the following steps of: performing magnetic solid-phase extraction and adsorption on an organic fertilizer in a buffer solution with the pH value of 4.0-7.0 by using MnO powder as an adsorption material, desorbing by using ammonia water acetonitrile eluent, and blow-drying the desorbed eluent to obtain a treated sample. According to the detection method for the macrolide antibiotics in the organic fertilizer, a treated sample obtained by the sample treatment method is adopted as a test sample, and one or more of existing detection methods for the macrolide antibiotics are directly adopted for detection. The method is simple and convenient to operate, time-saving and rapid, the adsorption material can be recycled, the detection result is accurate, and the method can be widely popularized and applied.

Description

technical field [0001] The invention relates to the technical field of antibiotic detection, in particular to a method for detecting macrolide antibiotics in organic fertilizers and a sample processing method thereof. Background technique [0002] Organic fertilizers are mainly derived from plants and (or) animals, and are applied to the soil to provide plant nutrition as a carbon-containing material whose main function is. It is processed from biomass, animal and plant waste, and plant residues. Artificially synthesized antibiotics added to animal feed will remain in manure, and antibiotics will remain in organic manure after manure processing. Studies have shown that compared with soil without organic manure, tetracyclines and large The content of cyclic lactone antibiotics will be increased ten to several tens of times. Antibiotics in organic fertilizers accumulate in the soil, which has a certain impact on crop growth, and can also spread to water bodies, causing surfa...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/72
CPCY02A50/30
Inventor 吴慧珍雷超孙娜波钱鸣蓉
Owner ZHEJIANG SHUREN COLLEGE ZHEJIANG SHUREN UNIV
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