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Method for extracting and measuring sulfonamide antibiotics in plant

A technology for sulfonamides and antibiotics, applied in the environmental field, can solve problems such as low recovery rate, cumbersome test process, and low detection limit, and achieve high recovery efficiency, simple and fast operation steps, and effective separation

Active Publication Date: 2018-11-06
HUAIYIN TEACHERS COLLEGE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In order to overcome the problems of low recovery rate, cumbersome test process and low detection limit in the existing research on sulfonamide antibiotic residues in plants, the present invention provides a fast, accurate and efficient method for extracting and detecting sulfa antibiotics in plants method

Method used

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  • Method for extracting and measuring sulfonamide antibiotics in plant
  • Method for extracting and measuring sulfonamide antibiotics in plant
  • Method for extracting and measuring sulfonamide antibiotics in plant

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Embodiment 1: the linear range, detection limit, recovery rate and precision of this method

[0024] Dilute the standard stock solution of 5 kinds of sulfa antibiotics (sulfadiazine, sulfamethazine, sulfa-5-methoxine, sulfamethoxazole and sulfadimethoxine) with high-purity water to prepare concentrations of 0.05 and 0.1 , 0.2, 0.4, 0.8, 1.0 and 5.0 mg / L mixed standard series solutions, using Waters2695 high performance liquid chromatography to measure mixed standard series solutions, the chromatographic conditions are: the detector is an ultraviolet detector with a wavelength of 265nm; Symmetry C18 chromatographic Column (250mm×4.6mm, 5.0μm); mobile phase is methanol (A) and 0.5% acetic acid (B), column temperature is 35°C, flow rate is 1mL / min, injection volume is 20μL, gradient elution condition: 0min, methanol: The volume ratio of 0.5% acetic acid is 10:90, 15min, and the volume ratio of methanol:0.5% acetic acid is 30:70. Obtain the chromatographic separation figur...

Embodiment 2

[0033] Embodiment 2: contrast the recovery rate, precision and efficient that the present invention and other methods measure

[0034] The concrete process of this method is as follows:

[0035] Step 1. Collect radishes planted on artificial antibiotic-contaminated soil (adding the above-mentioned 5 kinds of sulfonamide antibiotics, the total concentration is 5mg / kg), and then grind them with liquid nitrogen to obtain powdery samples;

[0036] Weigh 1.0g of the above sample and the sample with 50μg / kg of antibiotics into a 30mL glass centrifuge tube, add 10mL of methanol / hydrochloric acid mixed extract (volume ratio 95:5), sonicate for 30min, vortex for 3min, and centrifuge (4000r / min) Collect the supernatant after 10 minutes; add 10 mL of acetone to the solid phase residue, sonicate for 30 minutes, vortex for 3 minutes, and centrifuge (4000r / min) for 10 minutes to collect the supernatant;

[0037] Step 2. After combining the supernatants, pass them through a Waters OasisHLB ...

Embodiment 3

[0052] Embodiment 3: The influence of different extracting solutions on the residual state of sulfadiazine and the recovery rate

[0053] Step 1. Collect radishes planted on artificial antibiotic-contaminated soil (add the above-mentioned 5 kinds of sulfonamide antibiotics, the total concentration is 5mg / kg), and then grind them with liquid nitrogen to obtain powdery samples; weigh 1.0g of the above-mentioned samples and add Add 50 μg / kg antibiotic sample to a 30mL glass centrifuge tube, add 10mL methanol / hydrochloric acid mixed extract (volume ratio 95:5), sonicate for 30min, vortex for 3min, and centrifuge (4000r / min) for 10min to collect the supernatant; Add 10 mL of acetone to the phase residue, sonicate for 30 min, vortex for 3 min, and centrifuge (4000r / min) for 10 min to collect the supernatant;

[0054] Step 2. After combining the supernatants, pass them through a Waters OasisHLB (6 mL, 500 mg) solid-phase extraction column activated with 5 mL of methanol and 5 mL of u...

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Abstract

The invention discloses a method for extracting and measuring sulfonamide antibiotics in plant. The method comprises the following specific steps: adding a pretreated plant sample into a methanol / hydrochloric acid mixed extracting solution, sequentially performing ultrasonic, vibration and centrifugation processes, then collecting supernate to be stand-by; continuously adding acetone into a residual, sequentially performing ultrasonic, vibration and vortexprocesses, and collecting supernate; separating the supernate through a solid phase extraction column, ensuring that eluant is methanol, drying the eluant through nitrogen, and dissolving the nitrogen through the methanol; measuring the content of sulfonamide antibiotics in a methanol solving liquid through high performance liquid chromatography. The method overcomes the problems of low recovery rate, complicated test processes and low detection limit in the research of sulfonamide antibiotic residues in the existing plant, and is convenient, accurate and efficient.

Description

technical field [0001] The invention belongs to the field of environmental technology, and in particular relates to a method for extracting and measuring sulfonamide antibiotics in plants. Background technique [0002] Sulfonamide drugs refer to the general term of a class of drugs with p-aminobenzenesulfonamide structure, which is a class of chemotherapeutic drugs for the prevention and treatment of bacterial infectious diseases. For a long time, sulfonamide antibiotics have been widely used in the prevention and treatment of human and animal diseases, and at the same time added to animal feed to improve feed utilization and promote animal growth. Most of the antibiotics used in large quantities are excreted with feces and urine in the form of drugs, and continue to enter the ecological environment, becoming new important environmental pollutants, posing a serious threat to the ecological environment and human health. When the livestock and poultry manure containing these ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/062
Inventor 徐永刚白天霞赵祥祥罗玉明徐建明
Owner HUAIYIN TEACHERS COLLEGE
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