Optimal strategies for determination of free/extractable and total microcystins in lake sediment

[Display omitted] ► An optimized solvent extraction for analysis of free MCs in sediments was proposed. ► Best recovery of free MCs in sediments was found via sequential solvent extraction. ► We further optimized the Lemieux oxidation for analysis of total MCs in sediments. ► The yield of MMPB decre...

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Bibliographic Details
Published in:Analytica chimica acta 2012-01, Vol.709, p.66-72
Main Authors: Wu, Xingqiang, Wang, Chunbo, Xiao, Bangding, Wang, Yang, Zheng, Na, Liu, Jingshuang
Format: Article
Language:English
Subjects:
2-Methyl-3-methoxy-4-phenylbutyric acid (MMPB)
Analytical chemistry
Chemistry
Chromatographic methods and physical methods associated with chromatography
Chromatography, High Pressure Liquid
Diphosphates - chemistry
Edetic Acid - chemistry
Exact sciences and technology
Freshwater
Geologic Sediments - chemistry
Lakes
Lemieux oxidation
Liquid-Liquid Extraction
Mathematical analysis
Methanol - chemistry
Methyl alcohol
Microcystin
Microcystins - analysis
Microcystins - isolation & purification
Optimization
Other chromatographic methods
Oxidation
Oxidation-Reduction
Phenylbutyrates - analysis
Phenylbutyrates - isolation & purification
Sediment
Sediments
Soil Pollutants - analysis
Soil Pollutants - isolation & purification
Solvent extraction
Strategy
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Summary:[Display omitted] ► An optimized solvent extraction for analysis of free MCs in sediments was proposed. ► Best recovery of free MCs in sediments was found via sequential solvent extraction. ► We further optimized the Lemieux oxidation for analysis of total MCs in sediments. ► The yield of MMPB decreased as the content of sediment organic matter increased. ► Seven of thirty sediment samples showed positive results of MCs in Lake Dianchi. 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.
ISSN:0003-2670
1873-4324
DOI:10.1016/j.aca.2011.10.027