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固相萃取高效液相色谱法测定水中微囊藻毒素

Determination of Microcystin-LR in Water by SPE and HPLC
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摘要 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。 The enrichment and detection of microcystin-LR were performed by the solid phase ex- traction (SPE) and high performance liquid chromatography (HPLC). The mierocystin-LR was extracted with 80% aqueous methanol (re^V) stirring for 2 h at room temperature when the fluid solid ratio was 1 : 50. The supernatant was obtained after centrifugation (20 rain, 8 000 r/rain). The methanol in the extract was removed by the rotary evaporator, and the color was removed by the protein isoelectrie point precipitation process. SPE was used for the microcystin-LR concentration and partial purification. The microcystin-LR was identified and quantified by HPLC. The method has good accuracy, precision, recov- ery rate, high extraction rate and low impurity content. The minimum detection limit was 0.1 mg/L. The method is suitable for analyzing the trace microcystin-LR in water.
出处 《中国给水排水》 CAS CSCD 北大核心 2012年第20期142-145,共4页 China Water & Wastewater
基金 山西省科技基础条件平台建设项目(2009091015) 山西省软科学研究项目(2008041033-03)
关键词 微囊藻毒素 高效液相色谱法 固相萃取 microcystin HPLC SPE
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