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建立了UHPLC-MS/MS法测定水产品中10种磺胺类(SAs)和7种喹诺酮类(QNs)药物残留的分析方法。样品用200 g/L盐酸羟胺-乙腈溶液提取,以乙酸铵溶液和乙腈为流动相进行梯度洗脱,电喷雾正离子(ESI+)模式电离,多反应监测模式检测,同时对水产品中10种SAs和7种QNs进行定量和定性。在0.25～4.0μg/kg和0.10～2.0μg/kg范围内两类药物的线性良好(r2>0.99);平均回收率为均为80%～120%,RSD为7.4%～14%;10种磺胺药物的检测限(LOD)均为5.0μg/kg,7种喹诺酮药物检测限(LOD)均为2.0μg/kg。该方法适合水产品中这两类药物残留的确证和定量测定。
A method for the determination of ten sulfonamides (SAs) and seven quinolones (QNs) residues in aquatic products by UHPLC-MS / MS was established. The samples were extracted with 200 g / L hydroxylamine-acetonitrile solution, gradient elution was carried out with ammonium acetate solution and acetonitrile as mobile phase, electrospray ionization (ESI +) mode ionization and multi-reaction monitoring mode. At the same time, 10 SAs and seven QNs for quantification and characterization. The linearity was good (r2> 0.99) in the range of 0.25 ~ 4.0μg / kg and 0.10 ~ 2.0μg / kg. The average recovery was 80% ~ 120% and RSD was 7.4% ~ 14% The limit of detection (LOD) of sulfanilamide was 5.0 μg / kg, and the limit of detection (LOD) of 7 quinolones was 2.0 μg / kg. This method is suitable for the confirmation and quantitation of these two types of drug residues in aquatic products.