Abstract A method for determining seven microcystins and nodularin in surface water at nanogram per liter concentrations was developed based on on-line solid-phase extraction ultra-performance liquid chromatography – electrospray ionization tandem mass spectrometry (on-line SPE-UPLC-MS/MS). Aliquots of 5 mL water sample were directly injected into on-line SPE after passage through a membrane filter. The water sample was enriched and purified by a hydrophilic–liphophilic balance (HLB) polymeric column and eluted by mobile phase. The analytes were separated by Acquity BEH130 column, detected using tandem mass spectrometry, and quantified by external standardization. Under the optimized conditions, the method detection limits for all of the targets ranged from 1.4 to 3.3 ng/L with the recoveries from 85.5 to 121%. The precision of the method, indicated by the relative standard deviation, was 3.87 to 13.9%. The results of the analysis of surface water samples demonstrated that the proposed method has the ability to determine microcystins and nodularin without the need for complex manual pretreatment.

中文翻译：

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使用超高效液相色谱-串联质谱 (UPLC-MS/MS) 在线固相萃取 (SPE) 快速测定地表水中的微囊藻毒素和节球藻毒素

摘要 基于在线固相萃取超高效液相色谱-电喷雾电离串联质谱（在线 SPE-UPLC-MS/MS），建立了测定地表水中 7 种微囊藻毒素和节球藻毒素的方法）。通过膜过滤器后，将 5 mL 水样的等分试样直接注入在线 SPE。水样通过亲水亲油平衡（HLB）聚合物柱进行富集和纯化，并通过流动相洗脱。分析物通过 Acquity BEH130 色谱柱分离，使用串联质谱进行检测，并通过外部标准化进行定量。在优化条件下，所有目标的方法检出限范围为 1.4 至 3.3 ng/L，回收率为 85.5 至 121%。方法的精密度，由相对标准偏差表示，为 3.87 至 13.9%。地表水样品的分析结果表明，该方法无需复杂的手动预处理即可测定微囊藻毒素和节球藻毒素。