环境水体中磺胺类抗生素分析方法的建立与应用

Establishment and Application of Analysis Method for Sulfonamide Antibiotics in Environmental Waters

应用高效液相色谱-串联质谱(HPLC-MS/MS)联用的技术,建立了水体中磺胺类抗生素的检测方法。选用电喷雾离子源(ESI),在正离子模式下对目标化合物进行选择性反应检测(SRM)扫描。采用固相萃取法对样品进行前处理,通过HLB小柱对样品进行富集和净化。液相色谱选用C18柱,以甲醇和0.1%甲酸作为流动相对样品进行梯度洗脱分离。方法的回收率为53.6%~96.2%。方法的最低检出限除磺胺噻唑(STZ)为0.3ng/L外,其余均为0.1ng/L,本方法的RSD为4.7%~9.3%,该方法适用于水体中磺胺类抗生素的残留检测。

An analysis method for sulfonamide antibiotics in water bodies was established using high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) technology.Electrospray ion sources (ESI) were used to scan the target compound in positive ion mode for selective reaction monitoring (SRM).The samples were pretreated by solid phase extraction and enriched and purified by HLB column.C18 column was selected for liquid chromatography,and samples were subject to gradient elution separation using methanol and 0.1% formic acid as moving phases.The recovery rate of the method is 53.6%~96.2%.The lowest detection limit of the method is 0.1ng/L except that it is 0.3 ng/L for sulfathiazole (STZ),and RSD of the method is 4.7%~ 9.3%.This method is suitable for the residual detection of sulfonamide antibiotics in water bodies.