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

发布时间：2017-12-27 01:39

本文关键词：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　出处：《分析化学》2017年11期 　论文类型：期刊论文

【摘要】：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。
[Abstract]:A method for the direct determination of 10 kinds of alga toxin in water by full automatic on-line solid phase extraction - Ultra High Performance Liquid Chromatography - linear ion trap tandem mass spectrometry was established. Multiple injection was realized by program, and algae toxin was enriched by online solid-phase extraction. Then, the six way valve was switched to enrich the target and rinse it to the analytical column and then separated into linear ion trap mass spectrometry. The 10 algae toxins had good linear relationship in the corresponding concentration range, the correlation coefficients were all greater than 0.99, the detection limits were between 0.0015~0.0050 and g/L, and the spiked recoveries of 3 concentrations (0.02, 0.10 and 1 g/L) were 83.7%~98.5%. The results showed that online solid-phase extraction greatly simplifies the pretreatment process. Linear ion trap tandem mass spectrometry improves the sensitivity of the determination of trace algae toxins. The establishment of enhancer ion scanner (EPI) library provides a guarantee for the confirmation of algal toxins. This method is suitable for rapid identification and quantitative determination of various algal toxins in water.
【作者单位】：浙江省食品药品检验研究院;
【基金】：浙江省食品药品监管系统科技计划项目(No.SP201704)资助
【分类号】：O657.63;X832
【正文快照】： 1引言近年来,水体富营养化所导致的水华现象频频出现。水体出现富营养化现象时,藻类大量繁殖,同时代谢产生氰毒素类化合物,主要包括为肝毒素、神经毒素和脂多糖内毒素[1]。肝毒素包括微囊藻毒素(MCs)、节球藻毒素(NOD)和柱孢藻毒素(CYN)[2~4]。其中微囊藻毒素由一个环七肽和特

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