[1]张立将,尹立红,浦跃朴,等.水中微囊藻毒素高效液相色谱检测与前处理条件优化[J].东南大学学报(自然科学版),2005,35(3):446-451.[doi:10.3969/j.issn.1001-0505.2005.03.026]
 Zhang Lijiang,Yin Lihong,Pu Yuepu,et al.Optimization in analysis and sample preparation of microcystins in water with high-performance liquid chromatography[J].Journal of Southeast University (Natural Science Edition),2005,35(3):446-451.[doi:10.3969/j.issn.1001-0505.2005.03.026]
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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()
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《东南大学学报(自然科学版)》[ISSN:1001-0505/CN:32-1178/N]

卷:
35
期数:
2005年第3期
页码:
446-451
栏目:
环境科学与工程
出版日期:
2005-05-20

文章信息/Info

Title:
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
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
Author(s):
Zhang Lijiang1 Yin Lihong1 Pu Yuepu1 Zhu Guangcan2 Li Xianning2 Lü Xiwu2
1 School of Public Health, Southeast University, Nanjing 210009,China
2 College of Civil Engineering, Southeast University, Nanjing 210096, China
关键词:
微囊藻毒素 高效液相色谱 前处理 优化
Keywords:
microcystins high-performance liquid chromatography sample preparation optimization
分类号:
X172;O657.72
DOI:
10.3969/j.issn.1001-0505.2005.03.026
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0.02 μg/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.

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备注/Memo

备注/Memo:
基金项目: 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).
作者简介: 张立将(1981—),男,硕士生; 尹立红(联系人),女,教授,博士生导师,lhyin@seu.edu.cn.
更新日期/Last Update: 2005-05-20