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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

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【作者】 张立将尹立红浦跃朴朱光灿李先宁吕锡武

【Author】 Zhang Lijiang~1 Yin Lihong~1 Pu Yuepu~1 Zhu Guangcan~2 Li Xianning~2 Lü Xiwu~2 (~1School of Public Health, Southeast University, Nanjing 210009,China) (~2College of Civil Engineering, Southeast University, Nanjing 210096, China)

【机构】 东南大学公共卫生学院东南大学土木工程学院东南大学土木工程学院 南京210009南京210009南京210096南京210096

【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.

【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.

【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).
  • 【文献出处】 东南大学学报(自然科学版) ,Journal of Southeast University (Natural Science Edition) , 编辑部邮箱 ,2005年03期
  • 【分类号】X832
  • 【被引频次】58
  • 【下载频次】1142
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