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Method for detecting residuals of sulfanilamides or fluoroquinolones drugs

A sulfonamide drug and a technology to be detected, applied in the field of analytical chemistry, can solve the problems of few types of sulfa drug separation and cumbersome detection steps, etc., and achieve the effect of daily rapid quantitative detection, fast analysis speed, and reduced purification procedures

Active Publication Date: 2013-09-11
西安血氧生物技术有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The invention provides a method for detecting residues of sulfonamides to solve technical problems such as fewer types of sulfonamides or cumbersome detection steps in the prior art in one chromatographic analysis

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

Experimental program
Comparison scheme
Effect test

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 known organic solvents can also be used to make up the volume), filter through a 0.45 μm filter membrane, and perform chromatographic analysis and quantification.

[0039] Chromatographic separation conditions: high performance liquid chromatography; reversed phase column (4.6 mm 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; the detection wavelength is 270nm (using the maximum absorption wavele...

specific Embodiment 2

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

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

[0045] Chromatographic separation conditions: high performance liquid chromatography; reversed phase column (4.6 mm 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] Table 2 Chromatographic gradient ratios for the separation of sulfonamides

[0047]

[0048] After the separation is completed, the area of ​...

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Abstract

The invention provides a method for detecting residuals of sulfanilamides or fluoroquinolones drugs. 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 Patents(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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