高效液相色谱-串联质谱法同时测定水产养殖水体中17种超痕量特征抗生素残留OA

To accurately investigate characteristic antibiotic residues in aquaculture water,an ultra performance liquid chromatography mass spectrometry(UPLC-MS/MS)method was developed for the simultaneous determina-tion of 17 typical antibiotics including macrolides,chloramphenicols,quinolones and sulfonamides in water from farming ponds.The water samples filtered by 0.45 μm mixed cellulose ester millipore were extracted with HLB Solid phase extraction column at pH=4.0,then separated on Hypersil GOLDTM C18 chromatographic column(100×2.1 mm,3 μm)by gradient solution with methanol and 0.1%formic acid as the mobile phase.The anal-ysis was performed in positive and negative ion mode and multiple reaction monitoring(MRM).The results showed good linearity for 17 typical antibiotic residues within the range of 0.05～400.0 ng/L,the correlation coef-ficients(r2)was higher than 0.993,and the limits of detection and quantification were 0.02～0.2 ng/L and 0.05～0.5 ng/L,respectively.At three spiked levels of 5,10,50 ng/L,the average recovery rate ranged from 70.8%to 113.9%,and the relative standard deviations(RSD)were 1.2%～9.5%.Totally 11 kinds of 17 anti-biotics were detected in the 18 water samples collected from the aquaculture ponds in Shanghai.The method is convenient,sensitive and accurate,and can provide technical support for the qualitative and quantitative analysis of antibiotics in aquaculture water.