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[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。
[Objective] The research aimed to investigate the effects of microcystin-LR (MC-RR), microcystin-YR (MC-LR), microcystin-LR (MC-LR) and nodularin (NOD) , To establish a fast, accurate and reliable trace analysis method. [Method] The samples were purified by C18 solid phase extraction column and purified by ultra performance liquid chromatography / tandem mass spectrometry (UPLC-MS / MS) Measurements were performed in Multi-reaction monitoring (MRM) mode and the matrix effect was eliminated using a matrix matching standard curve. [Result] The recoveries were 95.7% ~ 115.0% with RSD ranging from 2.43% to 6.04%. The detection limit was 0.05 ~ 0.20ng / L. The method was applied to the actual water sample analysis. The contents of three microcystins and nodulated toxin in the water were below the limit of detection. [Conclusion] UPLC-MS / MS method was established for the determination of trace microcystin and nodularin in water samples. The method can be used for the detection of real water samples.