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Aminoglycoside antibiotics (such as neomycin, gentamicin, kanamycin, apramycin) with broad-spectrum bactericidal effect, common application in animal husbandry, but due to its own side effects in animal tissue residues can give a great deal of harm to the human. People began to more and more attention to the aminoglycoside antibiotic residues in food of animal origin, some developed countries and the Codex Alimentarius Commission limited aminoglycoside made very strict rules, so aminoglycoside antibiotics detection method research become a hot spot. The established aquatic neomycin, gentamicin pre-column derivatization HPLC method, preliminary exploration of the aminoglycoside antibiotic residue column derivatization high performance liquid detection method. An aquatic neomycin HPLC after derivatization detection method. Adopted with 10% trichloroacetic acid and 2? TA-Na2 potassium dihydrogen phosphate extraction aquatic neomycin, samples were centrifuged, n-hexane to remove fat, C18 solid phase extraction (SPE), FMOC chloride ( FMOC-Cl) as derivatization reagent, acetonitrile and water (90:10) as the mobile phase and fluorescence detector excitation wavelength 260nm, emission wavelength of 315nm results neomycin peak area and concentration 0.04μg/mL ~~ the range of 4.0μg/mL a good linear relationship, the correlation coefficient of 0.9999, detection limit of 0.04μg/mL, limit of quantification was 0.2mg/kg. Eel muscle samples at three levels 0.2mg/kg, 1.0mg/kg, 10mg/kg average recoveries of between 55% -81%, the relative standard deviations between 3.8% -38%. Japanese flounder muscle samples at three levels 0.5mg/kg, 1.0mg/kg, 10mg/kg average recoveries of between 47% -79% relative standard deviation in the range of 6% -27%. Gentamicin HPLC after derivatization detection method. Using the PBS extraction aquatic gentamicin, TCA precipitated protein samples were centrifuged, n-hexane to remove fat, C18 solid phase extraction (SPE), FMOC chloride (FMOC-Cl) as derivatization reagent, acetonitrile and water ( 85:15) as mobile phase and fluorescence detector, excitation wavelength is 260 nm, emission wavelength of 315nm. In peak area and concentration the range of 0.04μg/mL ~ 4.0μg/mL gentamicin showed a good linear relationship, the correlation coefficient r = 0.9994, the detection limit of 0.04μg/mL limit of quantification for the 0.1mg/kg. Eel muscle samples at three levels 0.1mg/kg, 1.0mg/kg, 10mg/kg average recoveries of between 75% -83%, the relative standard deviation in the range of 2% -12%. Japanese flounder muscle samples at three levels 0.1mg/kg, 1.0mg/kg, 10mg/kg average recoveries of between 63% -85%, the relative standard deviation between 5% -18%. The use of o-phthalaldehyde (OPA) as derivatization reagent, post-column derivatization method, discover aquatic aminoglycoside antibiotics by high performance liquid multi-residue detection method. C18 reverse phase analytical column and potassium cation exchange column as high performance liquid analytical column, select the potassium cation exchange column flow of the mobile phase proportion, on the Japanese flounder kanamycin, apramycin, gentamicin, neomycin were tested. Extracted with 8 mL of potassium dihydrogen phosphate solution containing 10% trichloroacetic acid and 2% EDTA-Na2 the Japanese flounder kanamycin, apramycin, gentamicin and neomycin, samples were centrifuged, n-hexane and chloroform at the same time remove the fat, C18 solid phase extraction (SPE), the use of potassium cation column separation, post-column OPA derivative fluorescence detector excitation wavelength is 330 nm, emission wavelength of 465 nm, four aminoglycoside antibiotics have been effectively Isolation.
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