UHPLC-MS/MS法快速测定水产品中17种磺胺和喹诺酮类药物

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。

Rapid determination of sulfonamides and fluoroquinolone residues in aquatic products by high performance liquid chromatography-tandem mass spectrometry

A method for the determination of 10 sulfonamide and 7 floxacins residue in seafood products by high performance liquid chromatography-tandem mass spectrometry(UPLCMS/MS) has been developed.The samples were extracted with 200 g/L hydroxylamine hydrochloride-acetonitrile solution.The identification and quantification were achieved by using electrospray ionization in positive ion mode(ESI+) with multiple reaction monitoring(MRM) at the same time.The linearities of two kinds of drugs in the range from 0.25 to 4.0 μg/L and from 0.10 to 2.0 μg/L had good correlation coefficients(r2>0.99).The average recoveries and relative standard deviations were 80%～128% and 7.4%～14% respectively.The limits of detection were 5.0 μg/kg for the 10 SAs and 2.0 μg/kg for the 7 QNs.The method is simple,rapid,sensitive and accurate.It is suitable for the quantitative determination and confirmation of two kinds of drugs.