Key Laboratory of Wetland Ecology and Environment, Northeast Institute of Geography and Agroecology, Chinese Academy of Sciences, Changchun, China.
Anal Chim Acta. 2012 Jan 4;709:66-72. doi: 10.1016/j.aca.2011.10.027. Epub 2011 Oct 21.
The optimization of analytical procedures for the quantification of free and total microcystins (MCs) in natural sediments was systematically examined based on solvent extraction and Lemieux oxidation. In this optimized analytical procedure, a sequential solvent extraction using 50% (v/v) methanol and EDTA-sodium pyrophosphate was selected as the optimal extraction solvent for free MCs analysis, after which the purified extracts and sediment residuals were applied to the optimized Lemieux oxidation for determination of total MCs in lake sediments. The optimized procedures were shown to be efficient and reliable for the routine analysis of both free and total MCs in lake sediment samples, as indicated by the minimal adverse impact of sediment organic matter on the recovery of free MCs and yield of MMPB (2-methyl-3-methoxy-4-phenylbutyric acid). Finally, the developed procedures were applied to field sediment samples collected from Lake Dianchi during a bloom season and seven of thirty samples showed positive results.
基于溶剂萃取和莱米厄氧化，系统地研究了定量分析天然沉积物中游离态和总微囊藻毒素（MCs）的分析方法的优化。在这个优化的分析程序中，选择 50%（v/v）甲醇和 EDTA-焦磷酸钠的连续溶剂萃取作为游离态 MCs 分析的最佳萃取溶剂，然后将净化后的提取物和沉积物残留物应用于优化的莱米厄氧化，以测定湖泊沉积物中的总 MCs。优化的程序对于湖泊沉积物样品中游离态和总 MCs 的常规分析是有效和可靠的，这表明沉积物有机质对游离态 MCs 的回收率和 MMPB（2-甲基-3-甲氧基-4-苯基丁酸）的产率的负面影响最小。最后，将开发的程序应用于滇池在水华季节采集的现场沉积物样品，其中 30 个样品中有 7 个呈阳性。
