高效液相色谱-串联质谱法同时分析水中9种典型藻毒素

Simultaneous determination of nine cyanotoxins in water by high performance liquid chromatography-tandem mass spectrometry

应用两种水样预处理方法和高效液相色谱-串联质谱检测,建立了同时分析水中微囊藻毒素、柱孢藻毒素和节球藻毒素等共9种典型藻毒素的方法,并用于实际样品分析。采用水样直接分析方式,水样经0.22μm聚偏氟乙烯(PVDF)滤膜过滤后直接进样检测,回收率为39.8%～102.2%,方法检测限和定量限分别为0.004～0.108μg/L和0.012～0.360μg/L,该方法为环境监测中大量样本的藻毒素检测提供了简便快速的方法。采用固相萃取富集预处理方式,水样经HLB小柱富集浓缩后进样检测,地表水加标回收率为72.3%～91.7%,方法检测限和定量限分别为0.021～0.382ng/L和0.069～1.275ng/L,该方法能够对痕量水平的藻毒素进行准确定量。南方某大型水库采样分析显示,检测到9种藻毒素,浓度为5.9～329.6ng/L,无健康风险。

A method of simultaneous determination of nine cyanotoxins in water,including seven microcystins,cylindrospermopsin and noduralin was developed using two sample pretreatment methods and high performance liquid chromatography-tandem mass spectrometry detection analysis.By direct injection,0.22 μm Polyvinylidene Fluoride(PVDF) filters were used to remove insoluble matters.Its recovery was between 37.0% and 102.2%;its limit of detection(LOD) was 0.004 to 0.108 μg/L;in addition,its limit of quantification(LOQ) was 0.012 to 0.360 μg/L.It provided a convenient and rapid analysis for cyanotoxin determination of mass water samples.By solid phase extraction,HLB cartridges were used to extract cyanotoxins.The recovery of this method ranged from 72.3% to 91.7% for surface water;its LOD was from 0.021 to 0.382 ng/L;and its LOQ was from 0.069 to 1.275 ng/L.Nine cyanotoxins were detected in water samples which were collected from a reservoir located in south China,and the total concentration was from 5.9 to 329.6 ng/L.There was no healthy risk in the reservoir water.