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[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。
[Objective] The aim of the study was to establish a convenient and efficient method for the determination of 2-methyl-3-methoxy-4-phenylbutyric acid (MMPB), an oxidative product of microcystin (MC) GC-MS) detection method. [Method] Potassium permanganate was used to oxidize water samples, n-hexane extraction and concentration, derivatization with hexafluoroisopropanol-diethylamine N, N- diisopropylcarbodiimide (HFIP-DIC) Detection, internal standard method. [Result] The detection limit (MDL) of MMPB by GC-MS was 0.101μg / L (total concentration was total MC) by optimizing the conditions of oxidative hydrolysis of water sample and derivatization of MMPB. The linear range was 0.2-10.0 μg / L with good accuracy (80% -120%), precision (RSD <15%) and reproducibility (RSD <15%). [Conclusion] The method provided a quick, simple and reliable method for the analysis of total amount of MC in water, which could be used to monitor and analyze the total amount of MC in daily water quality.