金玉娥, 汪国权, 马佳鸣, 朱怡平, 温忆敏, 刘弘. 高效液相色谱-串联质谱法同时测定水产品中7种微囊藻毒素[J]. 环境与职业医学, 2012, 29(6): 343-346.
引用本文: 金玉娥, 汪国权, 马佳鸣, 朱怡平, 温忆敏, 刘弘. 高效液相色谱-串联质谱法同时测定水产品中7种微囊藻毒素[J]. 环境与职业医学, 2012, 29(6): 343-346.
JIN Yu-e , WANG Guo-quan , MA Jia-ming , ZHU Yi-ping , WEN Yi-min , LIU Hong . Determination of 7 Microcystin Variants in Aquatic Products by High Performance Liquid ChromatographyTandem Triple Quadrupole Mass Spectrometry[J]. Journal of Environmental and Occupational Medicine, 2012, 29(6): 343-346.
Citation: JIN Yu-e , WANG Guo-quan , MA Jia-ming , ZHU Yi-ping , WEN Yi-min , LIU Hong . Determination of 7 Microcystin Variants in Aquatic Products by High Performance Liquid ChromatographyTandem Triple Quadrupole Mass Spectrometry[J]. Journal of Environmental and Occupational Medicine, 2012, 29(6): 343-346.

高效液相色谱-串联质谱法同时测定水产品中7种微囊藻毒素

Determination of 7 Microcystin Variants in Aquatic Products by High Performance Liquid ChromatographyTandem Triple Quadrupole Mass Spectrometry

  • 摘要: 目的 建立用高效液相色谱-串联质谱法同时测定水产品中 7 种微囊藻毒素(microcystin, MC)的测定方法。

    方法 样品经 Tris-HC(l pH=7)缓冲液提取、HLB固相萃取柱(Oasis HLB)净化、C18柱分离、电喷雾电离质谱检测、内标法定量。

    结果 通过有效的提取和净化, 能同时完成水产品中 7种微囊藻毒素 MC-LR、MC-RR、MC-YR、MC-LA、MC-LW、MC-LY和 MC-LF的测定, 4种不同水产品基质中 10 μg/kg、40 μg/kg加标回收率为 51%~112%和 60%~117%, 相对标准偏差分别为 1.7%~12.7% 和 0.9%~8.0%(n=6); 检出限为 0.20~0.40 μg/kg。

    结论 本研究建立的液相色谱 -串联质谱同时测定水产品中 7种微囊藻毒素的测定方法是测定水产品中微囊藻毒素残留量快速、有效、实用的方法, 能为水产品中微囊藻毒素的监测提供有力的技术保障。

     

    Abstract: Objective To establish a high performance liquid chromatography-tandem triple quadrupole mass spectrometry method for simultaneous determination of 7 variants of microcystins in aquatic products.

    Methods All samples were subject to extraction in Tris-HCl buffer (pH=7), clean-up with Oasis HLB solid phase extraction, C18 separation, mass spectrometry detection and quantification with internal standards.

    Results After effective extraction and purification, 7 microcystins of LR, RR, YR, LA, LW, LY and LF were detected simultaneously. The mean recoveries spiked at levels of 10 μg/kg and 40 μg/kg in four matrices were 51%-112% and 60%-117%, with relative standard deviation of 1.7%-12.7% and 0.9%-8.0% (n=6), respectively. The limits of detection were 0.20-0.40 μg/kg.

    Conclusion A rapid and practical method with high efficiency is proposed and provides technical basis for standard determination protocol of microcystins.

     

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