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Analysis method for simultaneously measuring residues of sulfonamide, quinolone and benzimidazole medicaments and metabolites thereof in chicken liver

A technology for benzimidazoles and quinolones, which is applied to the analysis field of simultaneous determination of sulfonamides, quinolones, benzimidazoles and their metabolite residues in chicken liver, and can solve the problems of unreported detection methods

Inactive Publication Date: 2011-07-20
新疆出入境检验检疫局检验检疫技术中心
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Problems solved by technology

The detection method for the simultaneous determination of sulfonamides, quinolones, benzimidazoles and their metabolite residues in chicken liver has not been reported

Method used

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  • Analysis method for simultaneously measuring residues of sulfonamide, quinolone and benzimidazole medicaments and metabolites thereof in chicken liver
  • Analysis method for simultaneously measuring residues of sulfonamide, quinolone and benzimidazole medicaments and metabolites thereof in chicken liver
  • Analysis method for simultaneously measuring residues of sulfonamide, quinolone and benzimidazole medicaments and metabolites thereof in chicken liver

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Embodiment Construction

[0065] The present invention will be described in detail below in conjunction with the accompanying drawings and specific embodiments.

[0066] 1 Experimental part

[0067] 1.1 Instruments and reagents

[0068] ACQUITY UPLC-Quattro premier XE TM Mass spectrometer (Waters, USA); high-speed refrigerated centrifuge (Kontron, Italy); wrist oscillator (Burrell, USA); nitrogen blowing instrument (Organomation, USA); knife-type grinding homogenizer (Retsch, Germany) ; MS3 vortex mixer (IKA company); small centrifuge; 1.5mL screw mouth full recovery sample bottle (U.S. Waters company).

[0069] Amino (NH 2 ) Adsorbent (40~63μm), Beijing Zhenxiang Company; filter membrane: regenerated cellulose, 0.2μm, 13mm (Agilent, USA); methanol, acetonitrile, formic acid, n-hexane (chromatographically pure); dimethyl sulfoxide ( Superior grade pure); glacial acetic acid, anhydrous sodium sulfate (analytical pure); water is ultrapure water.

[0070] Standard: Sulfadiazine (Sulfadiazine, SDZ), S...

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Abstract

The invention discloses an analysis method for simultaneously measuring residues of 12 sulfonamide medicaments, 19 quinolone medicaments and 8 benzimidazole medicaments and metabolites thereof in chicken liver by quick, easy, cheap, effective, rugged and safe (QuEChERS) extraction and purification-ultrahigh performance liquid chromatography-tandem mass spectrometry (QuEChERS-UPLC-MS / MS). The method comprises the following steps of: extracting a sample by using 1 percent acetic acid-acetonitrile solution, purifying the sample by using NH2 adsorbent, and degreasing the sample by using n-hexane;and then performing separation by using a Kromasil Eternity C18 chromatographic column (100mm*2.1mm, 2.5mum), performing gradient elution by using 0.1 percent formic acid and methanol as mobile phases, performing ionization in an electron spray positive ion (ESI<+>) mode, performing detection in a multi-reaction monitoring (MRM) mode, and performing quantification by an internal standard method. The 39 medicaments have good linearity (r is more than 0.98) in a blank adding concentration range of 5 to 100mug / kg, the average recovery rate of the medicaments in the adding level range of 10 to 50mug / kg, the relative standard deviation (RSD) is 1.5 to 23.4 percent, the limit of detection (LOD) of the 39 medicaments is 5mug / kg, and the low limit of quantification (LOQ) is 10mug / kg. The method is simple, convenient, quick, sensitive, accurate and rugged, and is suitable for confirmation and quantitative determination of the residues of the residues of the sulfonamide, quinolone and benzimidazole medicaments in the chicken liver.

Description

technical field [0001] The invention relates to an analysis method for simultaneous determination of sulfonamides, quinolones, benzimidazoles and their metabolite residues in chicken liver by QuEChERS-UPLC-MS / MS. Background technique [0002] Sulfonamides (SAs) and quinolones (quinolones, QNs) are broad-spectrum antibacterial drugs, which are widely used in animal husbandry, aquaculture and other aquaculture production because of their broad antibacterial spectrum, high efficiency, low toxicity, and low price. . However, excessive use may accumulate in the human body, and when the accumulated concentration exceeds a certain value, it will be harmful to the human body and lead to drug resistance of pathogens. In particular, sulfa drugs such as sulfamethazine may cause cancer, teratogenicity, and mutagenesis; nelidixic acid has been proven to interfere with the reproductive system, affect photosensitivity, carcinogenicity, and mutagenesis. Therefore, the International Codex ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/14G01N30/72
Inventor 李锋格苏敏李晓岩张红霞姚伟琴窦辉张万权
Owner 新疆出入境检验检疫局检验检疫技术中心
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