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Method for rapidly detecting sulfonamide antibacterial medicines in milk by using in-tube solid-phase micro-extraction technology

An extraction technology and a detection method technology, applied in the detection field of sulfonamide antibacterial drugs, can solve the problems of long pretreatment time, limited application range, low sensitivity and accuracy, etc., to increase specific surface area and stability, and reduce material interference , Improve the effect of extraction capacity

Active Publication Date: 2015-04-22
BEIJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Among them, the detection speed of microbial detection method is fast, but the sensitivity and accuracy are not high, and it can only be used for qualitative detection. Solve the problem of non-specific adsorption; although thin-layer chromatography has good selectivity, but poor repeatability; high-performance liquid chromatography is more general, has the advantages of high sensitivity and low detection limit, but its sample pretreatment time is long and the operation is complicated , not suitable for rapid detection of drug residues; while chromatographic mass spectrometry combines the high separation ability of chromatography and the high qualitative ability of mass spectrometry, but mass spectrometry instruments are relatively expensive, and the requirements for operators are also high, which limits its application range

Method used

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  • Method for rapidly detecting sulfonamide antibacterial medicines in milk by using in-tube solid-phase micro-extraction technology
  • Method for rapidly detecting sulfonamide antibacterial medicines in milk by using in-tube solid-phase micro-extraction technology
  • Method for rapidly detecting sulfonamide antibacterial medicines in milk by using in-tube solid-phase micro-extraction technology

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] Embodiment 1 Preparation of solid-phase microextraction capillary monolithic column

[0043] The preparation method of the solid-phase microextraction capillary monolithic column of the present invention is specifically implemented according to the following steps:

[0044] S1. Silanization of capillaries,

[0045] Take a fused silica capillary with an inner diameter of 100 μm and a length of 30 cm, rinse the inner wall of the capillary with 1mol / L NaOH, ultrapure water, and 1mol / L HCl for 30 minutes, then rinse with ultrapure water and acetone for 20 minutes, and blow dry with nitrogen.

[0046]The treated capillary was injected with 50% (v / v) 3-(trimethoxysilyl)propyl methacrylate in acetone solution, and the silanization reaction was carried out at room temperature in the dark for 12 hours. After the reaction was completed, the capillary was rinsed with methanol for 30 min to remove unreacted silylating reagent, and dried with nitrogen to obtain a silanized capillar...

Embodiment 2

[0052] Example 2 Milk sample spiked recovery rate experiment

[0053] A graphene-containing n-butyl methacrylate-ethylene glycol dimethacrylate polymer extraction column was prepared according to the method described in Example 1.

[0054] Accurately measure 1 mL of milk, add 10 μL of 0.1 g / L sulfonamide antibacterial mixed solution, add 20 mmol / L, pH=5 phosphate solution to dilute to 10 mL, at this time the spiked concentration of each sulfonamide antibacterial Both were 100 μg / L, vortexed, centrifuged at 10,000 r / min for 20 min, and the supernatant was taken, and filtered through a 0.22 μm Nylon filter membrane for later use. Take 20 μL of supernatant in a small bottle, and under the action of 400 psi pressure, the sample solution to be tested flows through the extraction column. Take 10 μL of 80% methanol-water solution as the analysis solvent. Under the pressure of 400 psi, the analysis solvent flows through the extraction column, and the centrifuge tube at the outflow en...

Embodiment 3

[0063] The detection of sulfa antibiotics in embodiment 3 milk samples

[0064] A graphene-containing n-butyl methacrylate-ethylene glycol dimethacrylate polymer extraction column was prepared according to the method described in Example 1.

[0065] For fresh milk bought in supermarkets, take 1mL accurately, add 20mmol / L, pH=5 phosphate solution to dilute to 10mL, vortex and mix well, centrifuge at 10000r / min for 20min, take the supernatant, and filter it through 0.22μm Nylon Reserved after membrane filtration. Take 500 μL of supernatant in a small bottle, and under the action of 400 psi pressure, the sample solution to be tested flows through the extraction column. Take 5 μL of 80% methanol-water solution as the analysis solvent. Under the pressure of 400 psi, the analysis solvent flows through the extraction column, and the centrifuge tube at the outflow end collects the eluted target analyte.

[0066] Add 5 μL of acetate solution with pH=3.5 and 0.5 μL of fluorescamine de...

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Abstract

The invention discloses a method for rapidly detecting sulfonamide antibacterial medicines in milk by using an in-tube solid-phase micro-extraction technology, belonging to the technical field of analytic chemistry. The method comprises the following steps: firstly taking a graphene-embedded n-butyl methacrylate-ethylene glycol dimethacrylate porous polymer monolithic column as an extraction phase of in-tube solid-phase micro-extraction, extracting sulfonamide antibacterial medicines in milk, performing analysis, then reacting with fluorescamine to produce a derived material with strong fluorescence properties, and finally separating and detecting a derived sample by using a capillary electrophoresis-laser-induced fluorescence detector. The method disclosed by the invention is simple to operate, is environmentally friendly, is high in detection sensitivity and short in detection time, is a simple, convenient, rapid and accurate analysis method, and has wide application prospects in the fields of environmental analysis and food safety.

Description

technical field [0001] The invention relates to a detection method of sulfonamide antibacterial drugs, in particular to an analysis method for detecting sulfonamide antibacterial drugs using solid-phase microextraction-capillary electrophoresis-laser-induced fluorescence detection combined technology in a tube, which belongs to analytical chemistry-food safety detection technology field. Background technique [0002] Sulfonamide antibacterial drugs are a class of chemical drugs (SAs) with broad-spectrum antibacterial activity, which are widely used in the prevention and treatment of bacterial infectious diseases in animal husbandry, and low doses can also promote the growth of livestock and poultry. However, excessive use of such drugs will lead to drug residues in animal foods, and even cause allergic reactions and cancer, which will endanger human health. In order to ensure human food safety, many countries have established the maximum allowable amount of SAs residues in ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/64G01N1/28
Inventor 汪夏燕张婧王昱郭广生
Owner BEIJING UNIV OF TECH
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