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Method for testing aminoglycoside drug residue in animal derived food

An aminoglycoside and animal-derived technology, which is applied in the field of determination of aminoglycoside drug residues in animal-derived foods, can solve problems such as low sensitivity, limited detection categories of aminoglycoside antibiotics, and inability to meet actual monitoring requirements. Strong, simple effect

Active Publication Date: 2019-03-29
厦门海关技术中心
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Invention patent CN106053638B discloses a detection method for aminoglycoside antibiotic residues in food of animal origin, which is suitable for neomycin, spectinomycin, dihydrostreptomycin, streptomycin, gentamicin, apramycin It is not suitable for the detection of more than 10 other aminoglycoside antibiotics such as paromomycin and ribomycin. This method has limited detection categories of aminoglycoside antibiotics in animal source foods and cannot accurately characterize or indicative of the true status of aminoglycoside antibiotics in food
In addition, the patented method uses a hydrophilic interaction chromatographic column to analyze six antibiotics, including neomycin, spectinomycin, dihydrostreptomycin, streptomycin, gentamicin, and apramycin. The lower detection limit of the method is 100ug / kg, low sensitivity, can not meet the actual monitoring requirements

Method used

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  • Method for testing aminoglycoside drug residue in animal derived food
  • Method for testing aminoglycoside drug residue in animal derived food
  • Method for testing aminoglycoside drug residue in animal derived food

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0061] Sample preparation

[0062] Take 500g of representative honey samples. For uncrystallized samples, stir vigorously evenly. For samples with crystallization, plug the cap of the sample bottle tightly and warm it in a water bath not exceeding 60°C. Stir evenly after the samples are completely melted. , rapidly cooled to room temperature. Care should be taken to prevent moisture evaporation during melting. The prepared samples were divided into two parts, put into sample bottles respectively, sealed, and marked with marks. One was used as a test sample, and the other was stored below -18°C.

[0063] Take 500g representative royal jelly sample, thaw it at room temperature, wait until the sample is completely melted, stir well, divide the sample into two parts, put them into sample bottles respectively, seal them, and mark them. One was used as a test sample, and the other was stored below -18°C.

[0064] During the operation of sample preparation, sample contamination o...

Embodiment 2

[0118] Embodiment 2 Linear Range and Linear Equation

[0119]Referring to the method in Example 1, take a blank honey matrix solution, add a known amount of aminoglycosides, so that: streptomycin, dihydrostreptomycin, tobramycin, hygromycin B, ribomycin, western Somicin is 5ng / mL, 10ng / mL, 20ng / mL, 50ng / mL, 100ng / mL, spectinomycin, neomycin, apramycin, gentamicin, kanamycin, small promise 20ng / mL, 50ng / mL, 100ng / mL, 250ng / mL, 500ng / mL of Amikacin, Etimicin, Netilmicin, Paromomycin, Amikacin, respectively, as matrix matching mixed standard solution , carry out the liquid chromatography-mass spectrometry measurement, plot the corresponding mass concentration (X axis, ng / mL) with the response peak area (Y axis) of the quantitative ion, and the results are shown in Table 5. The results show that there is a good linear relationship between the response peak area of ​​the quantitative ion and the sample concentration within the corresponding linear range of 16 kinds of aminoglycosi...

Embodiment 3

[0123] Embodiment 3 Determination of lower limit

[0124] Select a series of 16 aminoglycoside drug mixed matrix working standard solutions with lower mass concentrations, process and analyze and detect according to the method in Example 1 and chromatographic conditions, and calculate the lower limit of determination.

[0125] Measure and find that the method of the present invention is 5 μ g / kg to the assay low limit of streptomycin, dihydrostreptomycin, tobramycin, hygromycin B, ribomycin, sisomicin in honey; The lower limit of determination of amycin, neomycin, apramycin, gentamicin, kanamycin, micronomycin, paromomycin, amikacin, etimicin and netilmicin is 25 μg / kg. The lower limit of this method for determination of streptomycin, dihydrostreptomycin, tobramycin, hygromycin B, ribomycin and sisomicin in royal jelly is 10 μg / kg; spectinomycin, neomycin, The lower limit of determination of apramycin, gentamicin, kanamycin, micronomycin, paromomycin, amikacin, etilmicin and...

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Abstract

The invention relates to a method for testing aminoglycoside drug residue in animal derived food. The method comprises the steps of extracting the residual aminoglycoside in a sample by phosphate buffer solution, performing enrichment purification on SupelMIP SPE-Aminoglycosides solid-phase extraction column, separating an SIELC ObeliscR chromatographic column and Hypercarb chromatographic column,and performing measuring according to a high-efficiency liquid chromatograph-tandem mass spectrometry. The method for testing aminoglycoside drug residue in the animal derived food can simultaneouslydetect the residue condition of 16 aminoglycosides in the animal derived food. Compared with reversed phase chromatography for analyzing the drug, the method according to the invention has advantagesof no adding of ion pairing agent in a testing process, and no pollution of a mass spectrometer. Compared with hydrophilic interaction chromatography, the method according to the invention has advantages of high sensitivity, high peak form, high response speed and large number of kinds of analyzing drugs.

Description

technical field [0001] The invention relates to a detection technology of aminoglycoside antibiotics (AGs), in particular to a method for determining aminoglycoside drug residues in animal-derived foods. Background technique [0002] Aminoglycoside antibiotics (AGs) are a class of antibiotics containing aminoglycoside bonds. They have a broad antibacterial spectrum and have strong antibacterial activity against aerobic Gram-negative bacilli and Pseudomonas aeruginosa. At present, there are dozens of natural antibiotics or semi-synthetic varieties. . Natural aminoglycoside antibiotics produced by Streptomyces, Micromonospora, and bacteria include streptomycin, kanamycin, tobramycin, spectinomycin, neomycin, gentamicin, sisomicin , Asemicin, etc.; semi-synthetic aminoglycoside antibiotics include amikacin, netilmicin, etc. Aminoglycoside antibiotics are one of the most commonly used antibiotics in the world today due to their high efficiency and low price. They are widely us...

Claims

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Application Information

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IPC IPC(8): G01N30/88
CPCG01N30/88G01N2030/8818
Inventor 严丽娟徐敦明林立毅吴敏张洁赖国银林建忠张志刚张峰
Owner 厦门海关技术中心
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