HPLC-MS/MS法测定水产品中14种磺胺类药物

Determination of 14 Kinds of Sulfonamide Residue in Aquatic Products by HPLC-MS/MS

采用高效液相色谱质谱法（HPLC-MS/MS）建立了一种能够同时测定水产品中14种磺胺类药物残留的检测方法。样品匀浆后用乙腈提取，离心后上清液用旋转蒸发器蒸干，残渣用乙腈-0.01 mol/L乙酸铵（2∶3）溶解，过滤后定容。以甲醇和0.1%甲酸-2 mmol/L甲酸铵水溶液作为流动相，选择反应监测正离子模式测定。该方法检测磺胺类药物的检出限（RSN=3）为0.5μg/kg，定量限为1.0μg/kg，平均回收率为74%～105%。

An high performance liquid chromatography-tandem mass spectrometric （HPLC-MS/MS） method has been developed for the simultaneous determination of 14 sulfonamide residues in aquatic products. Samples were extracted with acetonitrile, dried with the rotary evaporator after centrifuging, and the residues were then dissolved in acetonitrile-0.01 mol/L ammonium acetate （2 ∶ 3）. The 14 sulfonamides were separated with a mobile phase composed of methanol and 2 mmol/L ammonium formate solution （containing 0.1%formic acid）, and the mass spectrometer was operated in the positive ion mode using select reaction monitoring for qualitative and quantitative analysis. The limits of detection and the limit of quantitative were 0.5 μg/kg and 1.0 μg/kg, respectively. The average recoveries ranged 74%-105%.