沈菊芳, 房新宇, 戴艺, 卢大胜. 水中微囊藻毒素的氧化水解产物2-甲基-3-甲氧基-4-苯基丁酸的气相色谱-质谱检测研究[J]. 环境与职业医学, 2013, 30(11): 880-883.
引用本文: 沈菊芳, 房新宇, 戴艺, 卢大胜. 水中微囊藻毒素的氧化水解产物2-甲基-3-甲氧基-4-苯基丁酸的气相色谱-质谱检测研究[J]. 环境与职业医学, 2013, 30(11): 880-883.
SHEN Ju-fang , FANG Xin-yu , DAI Yi , LU Da-sheng . Determination of 2-Methyl-3-Methoxy-4-Phenylbutanoic Acid Derived from Oxidation and Hydrolyzation of Microcystin in Water by Gas Chromatograph Mass Spectrometry[J]. Journal of Environmental and Occupational Medicine, 2013, 30(11): 880-883.
Citation: SHEN Ju-fang , FANG Xin-yu , DAI Yi , LU Da-sheng . Determination of 2-Methyl-3-Methoxy-4-Phenylbutanoic Acid Derived from Oxidation and Hydrolyzation of Microcystin in Water by Gas Chromatograph Mass Spectrometry[J]. Journal of Environmental and Occupational Medicine, 2013, 30(11): 880-883.

水中微囊藻毒素的氧化水解产物2-甲基-3-甲氧基-4-苯基丁酸的气相色谱-质谱检测研究

Determination of 2-Methyl-3-Methoxy-4-Phenylbutanoic Acid Derived from Oxidation and Hydrolyzation of Microcystin in Water by Gas Chromatograph Mass Spectrometry

  • 摘要: 目的 采用衍生化建立一个便捷和高效的水中微囊藻毒素(MC)氧化产物2-甲基-3-甲氧基-4-苯基丁酸(MMPB)气相色谱-质谱仪联用(GC-MS)的检测方法。

    方法 高锰酸钾氧化水样,正己烷萃取,浓缩,六氟异丙醇-二乙胺N, N-二异丙基碳酰二亚胺(HFIP-DIC)衍生化, GC-MS检测,内标法定量。

    结果 通过对水样氧化水解和MMPB衍生化条件的优化,以GC-MS检测MMPB的方法检测限(MDL)为0.101μg/L(浓度均以总MC计),线性范围为0.2~10.0μg/L,具有良好的准确度(80%~120%)、精密度(RSD<15%)和重复性(RSD<15%),样品监测浓度水平为<0.101~3.090μg/L。

    结论 本方法对水中MC总量的分析提供了快速、简便、可靠的方法,能用于对日常水质中MC总量的监测分析研究。

     

    Abstract: Objective To develop a method for simple and rapid determination of 2-methyl-3-methoxy-4-phenylbutyric acid (MMPB), an oxidation and hydrolyzation product of microcystin (MC) in water using gas chromatography-mass spectrometry (GC-MS).

    Methods Samples were oxidized with potassium permanganate, extracted using n-hexane, then derivatized with hexafluoroisopropanol (HFIP)/N, N'-diisopropylcarbodiimide (DIC), and finally detected by GC-MS and quantified using internal standard method.

    Results The method was validated in terms of method detection limit (MDL) (0.101 μg/L), linearity range (0.2-10.0 μg/L), accuracy (80%-120%), precision (relative standard deviation, RSD<15%), and repeatability (RSD<15%). The representative samples were successfully detected with concentrations between < MDL and 3.090 μg/L.

    Conclusion The proposed method as an alternative method of HPLC-MS/MS is practicable for the routine analysis of total microcystins in water.

     

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