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建立了采用固相萃取法(SPE)富集、HPLC法检测微囊藻毒素(MC-LR)的分析方法,采用80%的甲醇溶液按1∶50的质量体积比,在室温下磁力搅拌抽提2 h,于8 000 r/min转速下离心20 min,取出上清液,利用旋转蒸发仪脱除提取液中的甲醇,采用蛋白质等电点沉淀法进一步去除色素,最后利用SPE富集纯化MC-LR。该方法具有较好的测定准确度、精密度和回收率,且提取率高、藻毒素中杂质含量低,检测限为0.1 mg/L,适用于分析水体中的痕量MC-LR。
A method for the determination of microcystin (MC-LR) by solid phase extraction (SPE) and mass spectrometry (HPLC) was established. The mass ratio of methanol to methanol was 1:50, After 2 h, centrifuged at 8 000 r / min for 20 min, the supernatant was removed, and the methanol in the extract was removed by rotary evaporator. The pigment was further removed by isoelectric point precipitation of protein and finally purified by SPE MC-LR. The method has good determination accuracy, precision and recovery, and high extraction rate, low impurity content of algal toxins, the detection limit of 0.1 mg / L, suitable for the analysis of trace MC-LR in water.