Determination of 13 Aminoglycoside Residues in Milk by Weak Cation Exchange Solid Phase Extraction Coupled with Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry
In this study,a method based on weak cation exchange(WCX)solid phase extraction(SPE)coupled with ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)was developed for the simultaneous determination of 13 aminoglycoside(apramycin,amikacin,paromomycin,hygromycin B,ribostamycin,kanamycin,streptomycin,gentamicin C1,dihydrostreptomycin,tobramycin,spectinomycin,neomycin and micronomicin)residues in milk.Samples were extracted using a mixture of ammonium acetate buffer solution and acetonitrile,and purified using a WCX SPE column.Chromatographic separation was achieved using a SILICA SG80 column with gradient elution using a mobile phase made up of 0.1%formic acid aqueous solution and acetonitrile.Detection was accomplished using an electrospray ionization source(EIS)in the positive ion mode,and quantification was carried out using a matrix-matched external standard method.Excellent linear relationships were observed for the 13 aminoglycosides in the concentration range of 5.0-500.0 ng/mL(R2≥0.998 3).The limit of detection(LOD)for hygromycin B,ribostamycin,streptomycin,tobramycin,and dihydrostreptomycin were 3 μg/kg,and the limit of quantification(LOQ)were all 10 μg/kg for these aminoglycosides.For apramycin,amikacin,paromomycin,kanamycin,gentamicin C1,micronomicin,neomycin and spectinomycin,the LODs and LOQs were 15 and 50 μg/kg,respectively.The recovery rates of milk spiked at 1×,2×and 5×LOQ levels were 73.8%-107.4%,with relative standard deviation(RSD)of 1.0%-9.8%.This developed method is sensitive,simple,stable,and suitable for the determination of these 13 aminoglycoside residues in milk.
万方数据
维普
