Method for detecting residuals of sulfanilamides or fluoroquinolones drugs

A technology for fluoroquinolones and sulfonamides, which is applied in the field of analytical chemistry, can solve the problems of few types of sulfonamides in separation, cumbersome detection steps, etc., and achieves the effect of satisfying daily rapid quantitative detection, fast analysis speed, and reducing purification procedures.

Active Publication Date: 2012-07-11
西安血氧生物技术有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The invention provides a method for detecting residues of sulfonamides or fluoroquinolones, so as to solve the technical problems in the prior art that the types of sulfonamides are separated in one chromatographic analysis, or the detection steps are cumbersome, etc.

Method used

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  • Method for detecting residuals of sulfanilamides or fluoroquinolones drugs
  • Method for detecting residuals of sulfanilamides or fluoroquinolones drugs
  • Method for detecting residuals of sulfanilamides or fluoroquinolones drugs

Examples

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specific Embodiment 1

[0037] Specific Example 1: Separation and detection of sulfa antibiotic residues in pork

[0038] Take 5g of pork tissue, add 20mL of acetonitrile to homogenate, centrifuge at a centrifugal force of 10,000×g for 5min after homogenization, recover the supernatant, evaporate to dryness on a rotary evaporator, dissolve with 0.5mL of acetonitrile, wash repeatedly, and then purify the sample with nitrogen Blow dry, and finally dissolve the sample with 1 mL of acetonitrile (other well-known organic solvents can also be used to make up the volume), filter through a 0.45 μm filter membrane, and carry out chromatographic analysis and quantification.

[0039] Chromatographic separation conditions: high performance liquid chromatography; reversed-phase chromatographic column (4.6mm I.D.×250mm); flow rate: 0.8mL / min; temperature: room temperature; eluent: A: 0.1% formic acid solution; B: acetonitrile; C: 0.01mol / L ammonium acetate solution; detection wavelength is 270nm (adopted the maxim...

specific Embodiment 2

[0043] Specific Example 2: Separation and detection of sulfonamide antibiotic residues in milk

[0044] Take 0.45mL of milk, add 0.5mL of trichloroacetic acid (1g / mL) to precipitate the protein in it, then centrifuge at 10,000×g for 5min, recover the supernatant, and re-dilute to 5mL with acetonitrile (other known organic solvents can also be used to dilute to 5mL). Volume), 0.45μm membrane filtration, chromatographic analysis and quantification.

[0045] Chromatographic separation conditions: high performance liquid chromatography; reversed-phase chromatographic column (4.6mm I.D. × 250mm); flow rate: 0.8mL / min; temperature: room temperature; eluent: A: 0.06% acetic acid solution; B: acetonitrile; C: 0.015mol / L sodium acetate solution; the detection wavelength is 270nm, and the gradient ratio during separation is shown in the table below:

[0046] Chromatographic gradient ratio when table 2 separates sulfonamides

[0047]

[0048]

[0049] After the separation is comp...

specific Embodiment 3

[0050] Specific Example 3: Separation and detection of fluoroquinolone antibiotics in beef

[0051] Take 2g of beef tissue, add 10mL 50mmol / L phosphate for homogenization, centrifuge at 10,000×g for 5min after homogenization, recover the supernatant, evaporate to dryness on a rotary evaporator, and use 0.05mol / L phosphoric acid solution / triethylamine- Acetonitrile (82:18, volume ratio) was dissolved, and the volume was adjusted to 1 mL, and chromatographic analysis and quantification were carried out after filtration with a 0.45 μm filter membrane.

[0052] Chromatographic gradient ratio when table 3 separates sulfonamides

[0053]

[0054] After the separation is completed, the area of ​​the separated residual sulfonamide antibiotics is integrated, and quantitative calculation is performed based on the standard curve prepared by the standard to obtain the residual content. The standard curve made of the standard substance mentioned here should also adopt the same chromato...

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Abstract

The invention provides a method for detecting residuals of sulfanilamides medicines. An eluent adopted according to the method is composed of the following three solutions by volume percent: 55%-66% of 0.05-0.3vol% organic acid solution (A), 4%-15% of acetonitrile (B) and 25-35% of 0.005-0.03mol / L salt solution (C). A liquid chromatograph is used, and the proportion of the eluent during a process of separating an analyte is adjusted, namely, the proportion of acetonitrile in the eluent is gradually increased and the final proportion of acetonitrile in the eluent is not more than 50%. According to the method provided by the invention, the process of purifying a sample is reduced; various residuals of sulfanilamides drugs can be quickly separated and detected; and under a same condition, various fluoroquinolones drugs are separated.

Description

technical field [0001] The invention belongs to the technical field of analytical chemistry, and in particular relates to a method for separating residual antibiotics in samples by reverse-phase high-performance liquid chromatography. Background technique [0002] Sulfonamides and fluoroquinolones are a class of antibiotic compounds. They are widely used to treat diseases of livestock, poultry or fish. Excessive or uncontrolled use will lead to excessive antibiotic residues in meat products. At the same time, it will also bring antibiotic residues to the environment, which will cause food safety problems or environmental problems. Regular consumption of these foods with a large amount of antibiotic residues will lead to allergic reactions, antibiotic resistance and even cancer. Sensitive and rapid detection methods are therefore routinely required. [0003] At present, many methods have been developed, such as high performance liquid chromatography tandem mass spectrometry,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
Inventor 严坤平朱宏莉陈超
Owner 西安血氧生物技术有限公司
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