UHPLC-MS/MS法快速测定水产品中17种磺胺和喹诺酮类药物

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

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 10 sulfonamide and 7 floxacins residue in seafood products by high performance liquid chromatography-tandem mass spectrometry （UPLCMS/MS） has been developed. The sampleswere 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.