水体中微囊藻毒素和节球藻毒素的UPLC-MS~n分析方法研究

[目的]针对水体中3种代表性的微囊藻毒素（microcystin-RR,MC-RR;microcystin-YR,MC-YR;microcystin-LR,MC-LR）和节球藻毒素（nodularin,NOD）,建立一种快速、准确、可靠的痕量分析方法。[方法]样品经C18固相萃取柱净化富集后,采用超高效液相色谱-电喷雾串联三重四级杆质谱法（ultra performance liquid chromatography/tande mmass spectrometry,UPLC-MS/MS）,在多反应监测（Multi reaction monitoring,MRM）模式下进行检测,采用基质匹配标准曲线法消除基质效应。[结果]该方法加标回收率为95.7%~115.0%,精密度（RSD）范围为2.43%~6.04%,检测限可达0.05~0.20ng/L。将该方法应用于实际水样分析,水体中3种微囊藻毒素和节球藻毒素含量低于检测限。[结论]建立了水体中3种痕量微囊藻毒素和节球藻毒素的UPLC-MS/MS分析方法,该方法可用于实际水样的检测。

Analysis of Microcystins and Nodularin in Water by Ultra Performance Liquid Chromatography/Tandem Mass Spectrometry

[Objective] To establish an analytical method for the determination of trace content of microcystins（MC-RR, MC-YR and MC-LR）and nodularin（NOD）in water sample.[Methods] After cleaned and enriched by solid phase extraction （SPE）using C18,the water sample was determined by ultra performance liquid chromatography/tandem mass spectrometry（UPLC- MS/MS）in multi-reaction-monitoring mode.Matrix-matched standard curves were used to compensate the matrix effect.[Results] The recoveries were in range of 95.7%-115.0%with relative standard deviation（RSD）2.43%-6.04%.The detection limits were 0.05-0.20ng/L.[Conclusion] An analytical method for the determination trace microcystins and nodularin in water sample was established by UPLC-MS/MS.This method could be used to analyze local water samples.