在线固相萃取-超高效液相色谱-线性离子阱串联质谱法直接测定水中10种藻类毒素

Simultaneous Determination of 10 Kinds of Algal Toxins in Water Samples by Online Solid Phase Extration Coupled with Ultra High Performance Liquid ChromatographyQuadrupole Linear Ion Trap Mass Spectrometry

建立了全自动在线固相萃取-超高效液相色谱-线性离子阱串联质谱法直接测定水中10种藻类毒素的方法。利用程序实现多次进样,通过在线固相萃取对藻类毒素进行富集,然后切换六通阀,将富集的目标物冲洗至分析柱进行分离后,进入线性离子阱质谱检测。10种藻类毒素在相应的浓度范围内线性关系良好,相关系数均大于0.99,检出限在0.0015~0.0050μg/L之间,3个浓度水平(0.02、0.10和1.00μg/L)的加标回收率为83.7%~98.5%。结果表明,在线固相萃取极大简化了前处理过程,线性离子阱串联质谱法提高了痕量藻类毒素测定的灵敏度,增强子离子扫描(EPI)谱库的建立为藻类毒素的确证提供保障。本方法适用于水体中多种藻类毒素的快速确证和定量测定。

An online solid phase extraction（ online-SPE） combined with ultra high performance liquid chromatography-quadrupole linear ion trap mass spectrometry（ UHPLC-MS/MS-Qtrap） was established for the simultaneous identification and determination of 10 kinds of algal toxins in water samples. Multiple injections of water samples were controlled by a preset program,and the target analytes were enriched by trap column. The six-way valve was switched subsequently,and the algal toxins in the trap column were back-flushed to the analytical column for separation and analysis. The results showed that the online SPE significantly simplified pretreatment process,and the linear ion trap tandem mass spectrometry improved the sensitivity of the determination. Moreover,the establishment of enhanced product ion（ EPI） scan library provided evidence for the confirmation of algal toxins. The 10 kinds of algal toxins showed a good linear relationship with correlation coefficient R20.99. The limits of detection（ LOD） were 0.0015-0.0050 μg/L. The mean recoveries at three spiked levels of 0. 02,0. 1,1. 0 μg/L were from 83. 7% to 98. 5%. The method was suitable for the rapid confirmation and quantitative determination of various algal toxins in water.