动物源性食品蜂蜜中六种氟喹诺酮药物残留检测方法研究-药物分析专业论文.docxVIP

Study on detection methods of six kinds of animal origin fluoroquinolone residues in honey product Major: Pharmaceutical analysis Postgraduate:Yang Wei-Wei Supervisor:Hao Xiao Yan Xu Qian LI [Abstract] Objective: To establish a method for determining six kinds of fluoroquinolones norfloxacin, ciprofloxacin, danofloxacin, enrofloxacin, sarafioxacin, and difloxacin in honey. Methods: 1.The detection method of six kinds of fluoroquinolone residues above in honey product has been researched by using thin layer chromatography (TLC). Vortex extract the sample by the solution of 5% acetic acid in acetonitrile, centrifugal extract the supernatant and purify with dispersive- solid phase extraction (QuEChERS). Using the lower solution of trichloromethane- methyl alcohol-ethyl acetate-ammonia-water(15∶10∶4∶2∶1) as a solvent to extract and dry, and be sprained with chromogenic agent 3%Terbium(III) chloride hexahydrate. 2. We use high performance liquid chromatography with fluorescence (HPLC- FLD) to study the detection method of six fluoroquinolone residues in honey products. Solutions are obtained by pretreatment of samples.We use the Ultimate XB-C18 (250×4.6 mm, 5 μm) chromatographic column, with isocratic elution using acetonitrile and 0.2% formic acid solution (13∶87) as mobile phase at a flow rate of 1.0 mL/min.The column temperature is 30℃. High performance liquid chromatography-fluorescence detection, excitation wavelength 280 nm, emission wavelength 450 nm. 3. We used ultra performance liquid chromatography combined with mass spectrometry (UPLC/MS/MS) to study the qualitative methods of six fluoroquinolones that residue in honey products. Sample solution was tested in sequence by UPLC/MS/MS analysis, chromatographic column, agilent ZORBAX SB-C18(2.1 mm×50 mm, 1.8 μm).The acetonitrile as the mobile phase A, ammonium formate solution with 0.1% methanoic acid for B using the gradient elution mode with column flow rate 0.5 mL/min. Temperature 45℃.