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Method for determining residual quantity of 10 aminoglycoside antibiotics in eggs

An aminoglycoside and determination method technology, applied in the field of trace veterinary drug residue detection, can solve problems such as contamination of a mass spectrometer detector, and achieve the effects of improving sensitivity, improving efficiency and good purification effect

Inactive Publication Date: 2021-05-28
SHANDONG INST FOR FOOD & DRUG CONTROL
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Problems solved by technology

[0005] Aiming at the problems existing in the prior art of using ion-pair chromatography-mass spectrometry detection, contaminating the mass spectrometer detector and the vacancy of the pretreatment technology of aminoglycoside drugs in eggs, the present invention provides a method for measuring the residues of 10 aminoglycoside drugs in eggs. Determination method, through the establishment of a new pretreatment method and hydrophilic interaction chromatography-tandem mass spectrometry detection instrument method to achieve fast, simple, high-sensitivity quantitative detection

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  • Method for determining residual quantity of 10 aminoglycoside antibiotics in eggs
  • Method for determining residual quantity of 10 aminoglycoside antibiotics in eggs
  • Method for determining residual quantity of 10 aminoglycoside antibiotics in eggs

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Embodiment

[0031] 1. Instruments and materials

[0032] Shimadzu LC / MS-8050 ultra-high performance liquid chromatography-tandem mass spectrometer (with electrospray ionization source); 3-18K desktop high-speed centrifuge; BT 125D electronic balance; MS3 vortex mixer; SB-800DTD ultrasonic cleaner; Milli-Q ultrapure water system.

[0033] Streptomycin, dihydrostreptomycin, hygromycin B, kanamycin, amikacin, tobramycin, apramycin, spectinomycin, neomycin, gentamicin standard Methanol; Acetonitrile; Formic acid; Ammonium formate; Trichloroacetic acid; Disodium EDTA; Hydrochloric acid; Sodium hydroxide; Ammonia; Ammonium acetate; Prime HLB solid-phase extraction cartridge (200 mg, 6 mL); Chromatography column (150×2.1mm, 5 μm).

[0034] 2. Pretreatment

[0035] 2.1 Standard stock solution and mixed standard intermediate solution

[0036] Accurately weigh and convert to 10 mg (accurate to 0.01 mg) streptomycin, dihydrostreptomycin, hygromycin B, kanamycin, amikacin, tobramycin, apramycin ...

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Abstract

The invention relates to a method for determining the residual quantity of 10 aminoglycoside antibiotics in eggs, and belongs to the technical field of trace veterinary drug residue detection. The determination method specifically comprises the following steps of: pre-treating a sample, preparing a standard stock solution, a mixed standard intermediate solution and a matrix matching working solution, performing determination by utilizing the matrix matching standard working solution and adopting hydrophilic interaction chromatography-triple quadrupole mass spectrometry, drawing a standard curve, and detecting the to-be-detected solution according to the same instrument parameters, thus obtaining mass chromatograms of the 10 aminoglycosides in the sample, and then carrying out qualitative and quantitative analysis. According to the invention, pollution of ion pair reagents to chromatography and mass spectrometry is avoided, according to the detection method provided by the invention, pollution of heptafluorobutyric acid, sodium heptanesulfonate and other ions to a chromatographic column and a mass spectrometry detector is avoided; the pretreatment operation is simple, the purification effect is good, the sensitivity is higher, the detection limit and the quantitation limit are greatly reduced, and the limit requirement of the national standard on aminoglycoside in eggs is completely met.

Description

technical field [0001] The invention relates to a method for determining the residues of 10 aminoglycoside antibiotics in eggs, and belongs to the technical field of detection of trace veterinary drug residues. Background technique [0002] Aminoglycosides are broad-spectrum antibiotics, which have significant antibacterial effects on Gram-positive and Gram-negative bacteria, can effectively inhibit the growth and reproduction of bacteria, and are widely used in animal husbandry and aquaculture. Aminoglycosides not only treat animal diseases, but also can be used as feed additives to promote the growth and development of animals. Studies have shown that aminoglycosides have certain ototoxicity, nephrotoxicity and neuromuscular blockade. [0003] In order to ensure food safety, my country's GB 31650-2019 "National Food Safety Standard Maximum Residue Limits of Veterinary Drugs in Food" stipulates that the maximum residue limits of spectinomycin, neomycin and hygromycin in eg...

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/72G01N30/06G01N30/14G01N30/34G01N30/86G01N30/88
CPCG01N30/02G01N30/06G01N30/14G01N30/34G01N30/72G01N30/8634G01N30/8679G01N30/88G01N2030/062G01N2030/146G01N2030/884
Inventor 魏莉莉薛霞刘艳明卢兰香武传香丁一
Owner SHANDONG INST FOR FOOD & DRUG CONTROL
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