关键词: 氨基糖苷, 超高效液相色谱-串联质谱法, 牛奶, 弱阳离子交换固相萃取, 残留

Abstract: The weak cation exchange solid phase extraction-ultra performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS) was developed for the simultaneous determination of 13 aminoglycosides (apramycin, amikacin, paromomycin, hygromycin B, ribostamycin, kanamycin, streptomycin, gentamicin, dihydrostreptomycin, tobramycin, spectinomycin, neomycin and micronomicin) in milk. The milk samples were extracted with ammonium acetate buffer solution and acetonitrile, purified by weak cation exchange(WCX) solid phase extraction column, separated by SILICA SG80 liquid chromatography column. The gradient elution program using 0.1% formic acid aqueous solution and acetonitrile as the mobile phases, detected by ultra performance liquid chromatography-tandem mass spectrometry in Electrospray ionization positive ion mode, and quantified by matrix matching standard external standard method . The linear relationships of the 13 aminoglycosides were good in the range of 5.0?500.0 μg/kg (r2≥0.9983). The limits of detection of hygromycin B, ribostamycin, streptomycin, tobramycin, and dihydrostreptomycin were 3 μg/kg, and the limits of quantification were 10 μg/kg. The limits of detection of apramycin, amikacin, paromomycin, kanamycin, gentamicin, micronomicin, neomycin and spectinomycin were 15 μg/kg, and the limits of quantification were 50 μg/kg. The recoveries from milk spiked at LOQ, 2 LOQ and 5 LOQ levels were73.8% ~ 107.4%, and the relative standard deviations (RSDs) were 1.0%–9.8%. This method is sensitive, simple, stable, and can be used for detectmination of 13 aminoglycosides residues in milk.

Key words: aminoglycosides, ultra performance liquid chromatography-tandem mass spectrometry, milk, weak cation exchange solid phase extraction, residues