Comparison of Extraction and HPLC Methods for Marine Sedimentary Chloropigment Determinations

Szymczak‐Żyła, Małgorzata; Louda, J. William; Kowalewska, Grażyna

doi:10.1080/10826070802000699

Cited by 15 publications

(10 citation statements)

References 32 publications

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“…This extraction method is used in our Marine Pollution Laboratory (MPL-IO) for chloropigments and has been intercalibrated with other traditional methods of pigment extraction. 9 Acetone has been shown to be an effective extraction solvent for wet sediment samples. 30 In many methods a small volume of solvent was used (up to 10 ml), after which the extract was analysed by HPLC.…”

Section: Resultsmentioning

confidence: 99%

“…[4][5][6] The extraction efficiency depends on the type of solvent, its volume and time of extraction. 4,[7][8][9][10] Pigments are extracted with different solvents, i.e. acetone, methanol, ethanol or their mixtures (see Table 1).…”

Section: Introductionmentioning

confidence: 99%

“…To increase extraction efficiency, liquid-liquid extraction of pigments from an acetone extract to another solvent has sometimes been used. 9 There are a number of publications on HPLC methods for determining carotenoids in sediments. 5,16,[20][21][22] RP-HPLC (C18) has mostly been used for this purpose (see Table 2).…”

Section: Introductionmentioning

confidence: 99%

“…Some authors calculated pigment concentrations from a calibration curve using HPLC analyses of standards, 6,24,27 others used a method based on additional spectrophotometric measurements of the same but diluted solution as that analysed by HPLC and literature extinction coefficients of particular pigments. 9,11,28 The aim of this paper was to develop an analytical procedure (sample preparation, HPLC analysis and quantification method) for determining carotenoids that could be applied to organic-rich sediments, and to indicate the problems to be overcome during the development of this method. The influence of liquid-liquid extraction from an acetone extract to benzene on carotenoid extraction efficiencies was checked.…”

Section: Introductionmentioning

confidence: 99%

“…Some authors have based their calculations on HPLC standard calibration curves, 6,14,27 others have used a method based on an additional spectrophotometric measurement of the same solution as that analysed by HPLC and literature extinction coefficients of particular pigments. 9,11,28 The different calculation methods are compared in Fig. 5.…”

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Carotenoid determination in recent marine sediments - practical problems during sample preparation and HPLC analysis

Krajewska¹,

Szymczak‐Żyła²,

Kowalewska³

2017

10.5267/j.ccl

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An analytical procedure for the analysis of carotenoids in marine sediments rich in organic matter has been developed. Analysis of these compounds is difficult; the application of methods used by other authors required optimization for the samples studied here. The analytical procedure involved multiple ultrasound-assisted extraction with acetone followed by liquid-liquid extraction (acetone extract:benzene:water -15:1:10 v/v/v) and HPLC analysis. The influence of column temperature on pigment separation and the quantification method were investigated -a temperature of 5 °C was selected for the Lichrospher 100 RP-18e column. The pigments in the sediment extract were quantified using a method based on HPLC analysis (at 450 nm) and spectrophotometric measurements (at 450 nm), and extinction coefficients were determined for standard solutions at this wavelength. It is very important to use the value of the extinction coefficient appropriate to the wavelength at which the detection of carotenoids was carried out.

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Section: Resultsmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

mentioning

confidence: 99%

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Carotenoid determination in recent marine sediments - practical problems during sample preparation and HPLC analysis

Krajewska¹,

Szymczak‐Żyła²,

Kowalewska³

2017

10.5267/j.ccl

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Analysis of chloropigments in marine sediments using accelerated solvent extraction (ASE)

Szymczak‐Żyła

2016

Limnology & Ocean Methods

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The application of accelerated solvent extraction (ASE) for the analysis of chloropigments in marine sediment samples was studied. Chloropigments (chlorophyll a, b, c and their derivatives) are a group of natural compounds providing valuable data on the state of the aquatic environment. As these compounds are rather unstable and given the considerable risk that alteration products will form, their analysis is difficult. The new extraction method was optimized by testing both solvents and ASE operating conditions (static time, rinse volume, number of static cycles). The results obtained using an ASE technique were compared with those using an ultrasound‐assisted extraction method. The results presented in this article indicate that the application of ASE gives high chloropigment recoveries, comparable with conventional methods, but in less time, without the use of elevated temperature during extraction. The type of solvent used has the greatest influence on the extraction efficiency while the effects of the other parameters tested are important in the case of organic‐rich sediments. In addition, the influence of freeze‐drying of sediment samples on chloropigments composition and target compound stability in freeze‐dried sediments during storage under different conditions was examined. The results indicate that freeze‐drying does not affect the composition of pigments in the sediment samples and improves reproducibility of results, although extraction of freeze‐dried sediments does require the use of a more polar solvent (95% acetone). Freeze‐dried sediment samples could be stored in a freezer (−20°C) for up to 6 months, without the risk of degradation of the target compounds.

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Orthogonal design for optimization of pigment extraction from surface sediments of the Changjiang River Estuary

Zhao

Yao

et al. 2011

Acta Oceanol. Sin.

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Using a suitable solvent for extracting pigments from sediment for high performance liquid chromatography (HPLC) analysis is critical for obtaining qualitative and quantitative estimates of phytoplanktonic and benthic algal biomass, as well as community composition. Five methodological factors (sample dehydration, extraction solvent, extraction duration, number of extractions, and ratio of solvent volume: sample weight) were studied using an L 9 (3 4 ) orthogonal design in a sedimentary pigment extraction experiment on samples collected from the Changjiang large-river delta-front estuary (LDE), using HPLC analysis. The results show that the optimal extraction method for sedimentary pigments should include freeze-drying samples prior to extraction. The effects of different factors on sedimentary pigment extraction were separated by the L 9 (3 4 ) orthogonal design experiments and showed that the extraction solvent was the most important, with extraction duration the second most important, and numbers of extraction and ratio of solvent volume: sample weight was the least important. The mixed solvent treatment comprised of acetone, methanol and water (80:15:5, by volume) was best for polar pigment extraction, with 100% acetone better for apolar pigments. For most pigments employed in this study (i.e., peridinin, fucoxanthin, alloxanthin, diatoxanthin, zeaxanthin, pheophytin-a and β-carotene), 3 h was found to be enough time for extraction from these deltaic sediments. However, for chlorophyll-a, the most important pigment used for estimating algal biomass, 12 h was needed. A small amount of solvent (3 ml) with duplicate extractions obtained the greatest amount and diversity of pigments. Unfortunately, no extraction method was found to be suitable for all pigments in sediments. The choice of extraction procedure should be made in accordance with the objective of each study, taking into consideration the properties of sediments and pigments in question.

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Comparison of Extraction and HPLC Methods for Marine Sedimentary Chloropigment Determinations

Cited by 15 publications

References 32 publications

Carotenoid determination in recent marine sediments - practical problems during sample preparation and HPLC analysis

Carotenoid determination in recent marine sediments - practical problems during sample preparation and HPLC analysis

Analysis of chloropigments in marine sediments using accelerated solvent extraction (ASE)

Orthogonal design for optimization of pigment extraction from surface sediments of the Changjiang River Estuary

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