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水体中微囊藻毒素和节球藻毒素的UPLC-MSn分析方法研究

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

    摘要
  • 摘要:
    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;microcystinLR,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/tandemmass 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0.05~0.20 ng/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。

     

    Abstract:
    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 (UPLCMS/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 0.05-0.20 ng/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.

     

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