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A method for the detection of aminoglycoside antibiotic residues in food of animal origin

A technology for aminoglycosides and detection methods, which is applied in the field of detection of residues of 6 aminoglycoside antibiotics in animal source foods, can solve the problems of cumbersome steps, contamination of mass spectrometers, long sample processing time, etc., and achieve simple processing, The detection method is simple and avoids the effect of ion suppression

Active Publication Date: 2018-10-09
潍坊海润华辰检测技术有限公司
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Problems solved by technology

[0005] The technical problem to be solved by the present invention is to adopt reverse ion chromatography in the prior art, and the ion-pairing reagent heptafluorobutyric acid used in it can cause ion suppression, contaminate the mass spectrometer, and the pre-sample processing time of the existing detection technology is long, and the steps cumbersome technical issues

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  • A method for the detection of aminoglycoside antibiotic residues in food of animal origin
  • A method for the detection of aminoglycoside antibiotic residues in food of animal origin
  • A method for the detection of aminoglycoside antibiotic residues in food of animal origin

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Embodiment

[0032] 1. The experimental equipment and reagents are as follows:

[0033] Reagents: ammonium formate, ammonium acetate, disodium edetate, sodium chloride, trichloroacetic acid, sodium hydroxide, hydrochloric acid, Cleanert PWCX solid phase extraction SPE column.

[0034] Instruments: Shimadzu LC-MSMS 8050 chromatography-mass spectrometer, Xiangyi L550 centrifuge, EYEL 4 separating funnel shaker.

[0035] 2. The test plan is as follows:

[0036] Standard curves were established with gentamicin, apramycin, neomycin, streptomycin, dihydrostreptomycin, and spectinomycin, and the optimal conditions for chromatography-mass spectrometry were determined based on the standards.

[0037] A blank duck liver was selected for the authenticity detection test, and a blank duck meat was selected for the sample addition recovery test, and the lower limit of detection was obtained.

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Abstract

The invention discloses a method for detecting the aminoglycoside antibiotic residue amount in an animal-derived food and particularly relates to a method for detecting the aminoglycoside antibiotic residue amount in the animal-derived food based on HILIC chromatographic column tandem triple quadrupole mass spectrometry. The method is characterized in that a sample is subjected to extraction, solid phase extraction and ZIC-HILIC chromatographic column separation and then is determined through quadrupole mass spectrometry. The detected neomycin, spectinomycin, dihydrostreptomycin, streptomycin and gentamicin concentrations have good liner relation within the range of 10-500 micro-g / kg, a response value S / N under the concentration of 20 micro-g / kg is good and is greater than 10, the sample truth degree has no obvious matrix effect, and the detection limit of the concentration in the sample can be reduced to be 100 micro-g / kg. Compared with the prior art, the method has the advantages of being short in sample earlier-stage treatment time, low in cost, simple, convenient, comprehensive in matrix coverage, high in accuracy and the like.

Description

technical field [0001] The invention relates to a method for detecting residues of aminoglycoside antibiotics, in particular to a method for detecting residues of six aminoglycoside antibiotics in animal source foods by using a ZIC-HILIC chromatographic column in series with a triple quadrupole mass spectrometer. Background technique [0002] Aminoglycoside antibiotics (Aminoglyeosides) are a kind of glycoside antibiotic drug composed of aminosugar and aminocyclic alcohol linked by oxygen bridge. It has significant antibacterial effect on a variety of Gram-positive bacteria and Gram-negative bacteria, can effectively inhibit the growth and reproduction of bacteria, and is often added to feed to promote animal growth and development. It is currently a commonly used veterinary drug in animal husbandry in my country . Such drugs have side effects such as ototoxicity and nephrotoxicity, and long-term consumption of animal products with excessive residues will directly cause harm...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/027G01N2030/062
Inventor 刘刚
Owner 潍坊海润华辰检测技术有限公司
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