微囊藻毒素是一类由蓝藻产生的具有肝毒性的生物毒素。微囊藻毒素标准品是开展为微囊藻毒素相关研究的必需的实验材料,文章以滇池天然水华蓝藻为原料,建立了以5%乙酸和75%的甲醇溶液提取,通过优化提取、分离和制备条件,制备了一定量的微囊藻毒素高纯度样品,经HPLC鉴定分析,纯度可达90%以上。文章在相同的质谱条件下分别对MC—LR和[Dha7]MC-LR等毒素进行了质谱检测,一级质谱结果表明,MC-LR和[DhaT]MC-LR的一价电离离子峰分别为995和981,MC-RR的二价电离离子峰为520,并分析它们的二级质谱裂解特征,确定三种毒素化学结构MC—RR为环(Ala-Arg—MeAsp-Arg-Adda—Glu-Mdha)、MC-LR为环(Ala-Leu-MeAsp—Arg—Ldda—Glu—Mdha)、[Dha7]MC-LR为环(Ala-Leu—MeAsp-Arg—Adda-Glu-Dha)。改良后的检测方法同样应用于检测受微囊藻毒素污染的武汉东湖水样。
Microcystins are a kind of hepatotoxic cyanotoxin. Extraction of intracellular Microcystin variants is required to characterize and quantify all microcystins present in a sample. The method was established to isolate and purify Microcystins from natural cyanobacterial bloom dominated by Microcystis aeruginosa in Dianchi Lake, Yunnan Province, by the main steps of extraction with 75% aqueous methanol, 5% acetic acid solution through semi-prep-LC and ODS column with purity over 90%. The study was to develop an appropriate analytical procedure, based on solid phase extraction and liquid chromatography electrospray mass spectrometry for the determination of trace amounts of MCs in water samples. The developed method was applied to analyze the Microcystin-polluted surface water sampled from East Lake, Wuhan.