色谱 ›› 2011, Vol. 29 ›› Issue (03): 212-216.DOI: 10.3724/SP.J.1123.2011.00212

• 研究论文 • 上一篇    下一篇

液相色谱-二极管阵列检测器/离子阱质谱法检测水中的5种微囊藻毒素

王超*, 吕怡兵, 许人骥, 陈烨, 阴琨, 滕恩江   

  1. 中国环境监测总站, 北京 100012
  • 收稿日期:2010-11-22 修回日期:2011-01-10 出版日期:2011-03-28 发布日期:2011-03-28
  • 通讯作者: 王超,硕士,助理工程师,主要从事环境监测技术及分析方法研究.
  • 基金资助:

    国家水体污染控制与治理科技重大专项子课题(No. 2009ZX07527-001).

Qualitative and quantitative analysis of five microcystins in water by liquid chromatography-diode array detector/ion trap mass spectrometry

WANG Chao*, L Yibing, XU Renji, CHEN Ye, YIN Kun, TENG Enjiang   

  1. Determination of five microcystins in water using liquid chromatography-diode array detection/ion trap mass spectrometry
  • Received:2010-11-22 Revised:2011-01-10 Online:2011-03-28 Published:2011-03-28
  • Contact: Chao Wang

摘要: 建立了一种液相色谱-二极管阵列检测器(LC-DAD)/离子阱质谱(IT MS)对水中5种微囊藻毒素(microcystins)的分析方法。水中的微囊藻毒素经固相萃取富集和净化,经LC分离后,采用DAD和IT MS定性分析,DAD定量分析。在优化的条件下,水中5种微囊藻毒素的检出限为0.1 μg/L; 3个质量浓度加标水平(0.2、0.8和5 μg/L)的平均回收率为52.2%~115.2%,相对标准偏差为1.2%~10.0%。该方法从紫外吸收光谱和质谱角度同时进行定性定量分析,可用于地表水和饮用水中多种微囊藻毒素的检测。

关键词: 二极管阵列检测器, 固相萃取, 离子阱质谱, 水, 微囊藻毒素, 液相色谱

Abstract: A method for the determination of five microcystins (MCs) in water was established using liquid chromatography (LC)-diode array detection (DAD)/ion trap mass spectrometry (IT MS). The five MCs in water were enriched and purified by solid phase extraction, and determined by LC-DAD/IT MS. DAD was used for both qualitative and quantitative analysis, and IT MS was used for qualitative analysis only. Under the optimized conditions, the detection limits of 5 MCs in water were 0.1 μg/L. The average recoveries of the three spiked levels (0.2, 0.8 and 5 μg/L) were 52.2%~115.2% with the relative standard deviations (RSDs) of 1.2%~10.0%. This method uses UV absorption spectrum and MS spectrum in the qualitative and quantitative analysis, and can be applied in the determination of various MCs in both surface water and drinking water.

Key words: diode array detection (DAD), ion trap mass spectrometry (IT MS), liquid chromatography (LC), microcystin, water, solid phase extraction

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