在线固相萃取-超高效液相色谱-质谱法检测水中8种微囊藻毒素

Determination of 8 microcystins in water by on-line solid phase extraction coupled with ultra performance liquid chromatography-mass spectrometry

建立了一种在线固相萃取-超高效液相色谱-质谱同时检测水中8种微囊藻毒素的方法。水样经在线富集、色谱柱分离后,梯度洗脱,采用电喷雾离子源正离子多反应监测模式,外标法定量。该方法分析时长为11.0 min,标准曲线的线性相关系数R2>0.98,地表水样品的回收率为83.8%~97.2%,相对标准偏差(RSD)为1.8%~4.9%,检出限为0.28~0.91 ng/L。该方法适用于水体中微囊藻毒素的快速检测。

An online solid-phase extraction-ultra performance liquid chromatography-mass spectrometry(UPLC-MS)method was developed for the simultaneous detection of eight microcystins in water.The water samples were enriched online,separated on a chromatographic column with gradient elution,and quantified by external standard method using electrospray ionization source in positive ions multiple reaction monitoring mode.The analytical time of the method was 11.0 min,the linear correlation coefficient(R2)was higher than 0.98,the recoveries of surface water samples were 83.8%-97.2%,the relative standard deviations(RSDs)were 1.8%-4.9%,and the detection limits were 0.28~0.91 ng/L.The method is suitable for the rapid determination of microcystins in water.