【摘要】 通过对前处理过程中关键环节进行单因素不同水平比较,以及运用正交试验设计进行多因素综合分析,优选出洗脱剂、淋洗剂、固相萃取柱、浓缩定容方式等因素的最优试验方案,建立实用简便易行的一般水样前处理流程.微囊藻毒素高效液相色谱进样分析时,选用甲醇0.05%三氟乙酸水溶液作为流动相进行梯度洗脱,对于MC-RR和MC-LR取得较好分离效果,水样检出限可达0.02μg/L.优化后的前处理、检测方法,对MC-RR,MC-LR平均回收率分别为88.9%和92.1%.另外,对于总(胞内胞外)微囊藻毒素的检测前处理,冰乙酸处理法优于其他处理法.优化后的方法已成功应用于不同水域环境样本的藻毒素分析.更多还原

【Abstract】 Some key processes of high-performance liquid chromatography (HPLC) analysis for microcystins and its sample preparation were optimized. Single factor comparison and orthogonal design test were conducted. The result show that when methanol and water-0.05% trifluoroacetic acid (TFA) are applied to gradient mobile process, HPLC assay offeres a good potential for a sensitive and selective determination of MC-RR (microcystins-RR) and MC-LR (microcystins-LR), and the limit of detection for microcystins reaches 0.02 μg/L. The optimized protocols of water sample preparation include eluents, rinse solvents, solid phase extraction (SPE) cartridges, concentrating manner, et al. By using optimized method, the recoveries of MC-RR and MC-LR are around 88.9% and 92.1%, respectively. As for analysis of total microcystins (the sum of intra- and extracellular microcystins) treating with acetic acid is better than others. The optimized method has been successfully applied to the analysis of field samples from various kinds of water.更多还原