水中微囊藻毒素高效液相色谱检测与前处理条件优化  

Optimization in analysis and sample preparation of microcystins in water with high-performance liquid chromatography

作　　者：张立将[1] 尹立红[1] 浦跃朴[1] 朱光灿[2] 李先宁[2] 吕锡武[2] 

机构地区：[1]东南大学公共卫生学院,南京210009 [2]东南大学土木工程学院,南京210096

出　　处：《东南大学学报（自然科学版）》2005年第3期446-451,共6页Journal of Southeast University：Natural Science Edition

基　　金：国家高技术研究发展计划(863计划)资助项目(2002AA601011);国家自然科学基金资助项目(50378014);江苏省自然科学基金资助项目(BK2004075).

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.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.

关 键 词：微囊藻毒素 高效液相色谱 前处理 优化 

分 类 号：X172[环境科学与工程—环境科学] O657.72[理学—分析化学]