Phosphorus in sediments — speciation and analysis

Characterization of sediment phosphorus is commonly based on sequential chemical extractions, in which phosphorus is supposed to be selectively removed from different compounds in the sediments. The first extraction schemes were designed to quantify discrete chemical or mineralogical compounds. As extraction schemes have been tested on different sediments, several systematic errors have been detected and the schemes have been modified and simplified accordingly. Other chemical extractions or treatments have attempted to determine phosphorus bound to particles with a certain strength or binding energy, the purpose being to determine the labile, loosely bound, exchangeable, mobile or algal-available fraction of sediment phosphorus. All extraction procedures yield operationally defined fractions and cannot be used for identification of discrete phosphorus compounds. The many methodological modifications make it necessary to be cautious when comparing results from the literature in this field.     

Phosphate fractionation in mud bank sediments from the southwest coast of India

Mud banks are unique, occurring along the southwest coast of India. They are known as ‘Zones of Bio-rhythm’, providing shelter to abundant aquatic life. The cyclic variation of nutrients in this region provides a clue to the continued and enriched presence of a variety of fish. This study reports on the different forms of phosphate in the resuspended sediments collected during the seasons with and without mud banks from the above mentioned coastal zones. Applying sequential and parallel chemical extractions using eight different schemes, the major forms of phosphate namely exchangeable P, anion exchangeable P, carbonate bound P, labile and resistant organic P, Fe-, Al- and Ca bound P and hydrolysable P have been determined. Quantitatively, these fractions vary and exhibit seasonal fluctuations. The concentration of potentially available anion exchange P, together with resistant organic and hydrolysable surplus P, provide an explanation to the existing organic food web supporting the aquatic life. Sediment phosphate fractionation reflects the role of chemical speciation of nutrients in the propagation of mud banks and is indicative of the biogenic processes controlling the pathways of phosphate in these coastal waters. Editorial note: Because of the sudden, regrettable death of the senior author, Dr P. N. K. Nambisan, editing remained unfinished. The guest editor remains responsible for errors left in the text.     

Available phosphorus in lake sediments in The Netherlands

The amount of phosphorus available to algae in the sediments of four lakes in the western part of the Netherlands has been assessed by means of chemical extraction and bioassay techniques. In addition to direct chemical sediment analyses, extractions were carried out with an NTA column method and a stepwise NH₄ Cl-NaOH-HCI shaking method, the latter supposedly separating the weakly bound, the Fe- and Al-bound and the Ca-bound phosphates in the sediments. Bioassays, with sediment as the sole source of P, were made withScenedesmus quadricauda in modified Skulberg's 28 medium to determine the amount of phosphates available to algae.The average total P concentration of the sediments varied from 0.8 to 3.6 mg P g^–1 dry wt and correlated well with the net external P loading of the lakes. Uptake of P by algae in the bioassays varied from 0.4 to 36% — while NTA extracted 36–69% of the total P. The ratio NH₄Cl extracted/ NaOH extracted/ HCI extracted phosphates is different from lake to lake, although in all lakes the highest extractions (27–62% of total P) are found in the NaOH fraction. However, in the peaty sediments of these lakes, the NaOH step extracted not only the Fe- and Al-bound phosphates but, also, large amounts of humus compounds. Hence, this fraction also contains non-available organic P.The results are related to soil type and chemical characteristics of the sediments, and compared with data from other authors. A positive correlation was found between phosphate available to algae and NTA- and NaOH-extractable P, but the correlation with total phosphorus was higher. Moreover, algal-extractable P proved to be positively correlated with total iron and clay content and negatively with the amount of organic matter.It is concluded that the sediments in the investigated lakes show great variability and that the chemical extraction techniques cannot replace the bioassays to assess the amount of phosphorus available to algae.     

Factors Controlling the Geochemical Partitioning of Trace Metals in Estuarine Sediments

The geochemical partitioning of trace metals in sediments is of great importance in risk assessment and remedial investigation. Selected factors that may control the partitioning behavior of Cu, Pb and Zn in non-sulfidic, estuarine sediments were examined with the use of combined sorption curve—sequential extraction analysis. This approach, which has not been previously used to examine estuarine sediments, allowed determination of sorption parameters for Cu, Pb and Zn partitioning to individual geochemical fractions. Partitioning behavior in sulfidic sediments was also determined by sequentially extracting Cu, Pb, and Zn from synthetic sulfide minerals and from natural sediment and pure quartz sand after spiking with acid-volatile sulfide (AVS). Trace metal sorption to the “carbonate” fraction (pH 5, NaOAc extraction) increased with metal loading due to saturation of sorption sites associated with the “Fe-oxide” (NH₂OH·HCl extraction) and “organic” (H₂O₂ extraction) fractions in non-sulfidic sediments. Freundlich parameters describing sorption to the “Fe-oxide” and “organic” fractions were controlled by the sediment Fe-oxide and organic carbon content, respectively. Sequential extraction of Cu from pure CuS, AVS-spiked sediment and AVS-spiked quartz sand showed that AVS-bound Cu was quantitatively recovered in association with the “organic” fraction. However, some AVS-bound Pb and Zn were recovered by the NH₂OH·HCl step (which has been previously interpreted as “Fe-oxide” bound metals) in the sequential extraction procedure used in this study. This indicates that the sequential extraction of Pb and Zn in sulfidic sediments may lead to AVS-bound metals being mistaken as Fe-oxide bound species. Caution should therefore be exercised when interpreting sequential extraction results for Pb and Zn in anoxic sediments.     

Reactivity of Iron Minerals in the Seabed Toward Microbial Reduction – A Comparison of Different Extraction Techniques

Abstract

Dissimilatory iron reduction and sulfate reduction are the most important processes for anaerobic mineralization of organic carbon in marine sediments. The thermodynamics and kinetics of microbial Fe(III) reduction depend on the characteristics of the Fe(III) minerals, which influence the potential of Fe(III)-reducers to compete with sulfate-reducers for common organic substrates. In the present study, we tested different methods to quantify and characterize microbially reducible Fe(III) in sediments from a transect in Kongsfjorden, Svalbard, using different standard sequential endpoint extractions and time-course extractions with either ascorbate or a Fe(III)-reducing microbial culture. Similar trends of increasing ‘reactive Fe’ content of the sediment along the fjord transect were found using the different extraction methods. However, the total amount of ‘reactive Fe’ extracted differed between the methods, due to different Fe dissolution mechanisms and different targeted Fe fractions. Time-course extractions additionally provided information on the reactivity and heterogeneity of the extracted Fe(III) minerals, which also impact the favorability for microbial reduction. Our results show which fractions of the existing Fe extraction protocols should be considered ‘reactive’ in the sense of being favorable for microbial Fe(III) reduction, which is important in studies on early diagenesis in marine sediments.     

The evaluation of inorganic phosphate species in salt water lake sediments

Abstract

Surface sediments drawn from 10 shallow bays have been subjected to selective extraction in order to sub-divide the total P content into sub-categories such as water soluble P, Ca-P, Al-P and Fe-P. The reagents selected were similar to systems used in soil analysis, but evaluation of the procedures showed that the species values varied with time of extraction, weight of sediment taken, volume of extradant and chemical nature of the sediment. In water extractions, the P levels appeared to be determined by saturation with a sparingly soluble salt, while in acidic media P extract levels peaked (using different experimental conditions) due to loss of extracted P as a new phase (e.g. CaHPO₄) or through re-adsorption on other components.

The optimum conditions for P speciation in sediments must be determined from a series of preliminary studies because each of the five sediments studied in detail displayed individual characteristic behaviour.     

Significant correlation of Cd,Cu, Pb and Zn in sediments and oysters (Saccostrea cucullata) collected from Qeshm Island,Persian Gulf,Iran

Abstract

The relationships are evaluated between the heavy metal species in sediments and the accumulation by the soft tissues of Saccostrea cucullata collected from the northern and southern coasts of Qeshm Island, Persian Gulf. The sequential extraction technique was employed to fractionate the sediment into non resistant and resistant fractions. Data from sequential extractions indicated that the metals were mainly associated with the residual fraction at the north coast and with non residual fractions at the south coast. The results showed that the best correlations were observed between heavy metals concentrations in soft tissues and the fractions in the southern sediment. Note that the bioavailability of trace metals is influenced by the chemical characteristics and properties of the sediment. Therefore, the present results generally supported the use of soft tissues of S. cucullata as a more accurate biomonitoring organism for Cu, Pb and Cd in sediments from the southern coast of Qeshm Island, Persian Gulf.     

Predicting efficiency of different chemical extraction methods in risk assessment of trace metals in sediment of the Persian Gulf

Different chemical methods have been developed to evaluate the bioavailable fraction of the trace metals. Due to the lack of a universal method for analysis of the bioavailable metal fractions, due to the differences in sediment characteristics, it is necessary to validate an appropriate chemical method for assessing the available fraction of trace metals. For this propose, in this study, different chemical extraction methods including extraction with HCl and desorption test as a single reagent leaching test as well as geochemical fractions method have been evaluated. Bushehr coastal sediments in the Persian Gulf coasts have been selected for this purpose. To validate the efficacy of these methods, a gastropod species (Trochus erithreus), as a bioindicator, has been selected and monitored for trace metals of Fe²⁺, Pb²⁺, Cu²⁺, Zn²⁺, Mn²⁺, and Ni²⁺. According to the one-way ANOVA results, all partial extraction methods for all the trace metals (except for Mn²⁺) showed no significant variation, but linear correlation coefficients were between the results of the selective chemical extraction methods and concentrations of trace metals in organism tissues. It offered that selective extraction with HCl can be used as a simple method for measuring the bioavailable fraction of the metals in the sediments.     

Retention and mobility of atmospheric particle-associated organic pollutant PCDD/Fs and PAHs in maize leaves

The fate of polychlorinated dibenzo- p -dioxins and dibenzofurans and polycyclic aromatic hydrocarbons deposited to maize leaves under ambient conditions was investigated, with focus on those compounds that are primarily associated with particles in the atmosphere. Leaf samples collected from mature maize plants over an 8-wk period were subjected to four extraction procedures: (1) rinsing with distilled water; (2) shaking in aqueous EDTA solution; (3) immersion in chloroform/methanol; (4) soxhlet extraction with toluene. Of the compounds deposited primarily in association with particles, > 20% of the total leaf contamination was present in the first two aqueous extracts, indicating that only a small portion of these substances was subject to ready erosion from the leaf surfaces. Some 50–60% of the chemical was present in the third extract, while 20–40% was found in the final extract. The chemical in the final extract was no longer associated with particles, since these had been removed with the first three extractions. This chemical must have desorbed from the particles with which it was originally deposited, and migrated through the epicuticular waxes. Model calculations indicated that 15–35% of the chemical in the third extract had also desorbed from the particles, and there was evidence that polychlorinated dibenzo- p -dioxins and dibenzofurans desorb more readily than polycyclic aromatic hydrocarbons. It is concluded that desorption of chemical from particles and subsequent transport through the cuticle is an important process determining plant accumulation of organic contaminants associated with atmospheric particles.     

Selective chemical degradation of silica sinters of the Taupo Volcanic Zone (New Zealand). Implications for early Earth and Astrobiology

Most organic matter (OM) on Earth occurs as kerogen‐like materials, that is naturally formed macromolecules insoluble with standard organic solvents. The formation of this insoluble organic matter (IOM) is a topic of much interest, especially when it limits the detection of compounds of geomicrobiological interest. For example, studies that search for biomarker evidence of life on early Earth or other planets usually use solvent‐based extractions. This leaves behind a pool of OM as unexplored post‐extraction residues, potentially containing diagnostic biomarkers. Since the IOM has an enhanced potential for preservation compared to soluble OM, analysing IOM‐released biomarkers can also provide even deeper insights into the ecology of ancient settings, with implications for early Earth and Astrobiology investigations. Here, we analyse the prokaryotic lipid biosignature within soluble and IOM of the Taupo Volcanic Zone (TVZ) silica sinters, which are key analogues in the search for life. We apply sequential solvent extractions and a selective chemical degradation upon the post‐solvent extraction residue. Moreover, we compare the IOM from TVZ sinters to analogous studies on peat and marine sediments to assess patterns in OM insolubilisation across the geosphere. Consistent with previous work, we find significant but variable proportions—1%–45% of the total prokaryotic lipids recovered—associated with IOM fractions. This occurs even in recently formed silica sinters, likely indicating inherent cell insolubility. Moreover, archaeal lipids seem more prone to insolubilisation as compared to the bacterial analogues, which might enhance their preservation and also bias overall biomarkers interpretation. These observations are similar to those observed in other settings, confirming that even in a setting where the OM derives predominantly from prokaryotic sources, patterns of IOM formation/occurrence are conserved. Differences with other settings, however, such as the occurrence of archaeol in IOM fractions, could be indicative of different mechanisms for IOM formation that merit further exploration.     

Genotoxicity of fractionated organic material in airborne particles from São Paulo, Brazil

Particulate matter less than 10 microns aerodynamic diameter (PM10) is associated with adverse health effects including increased respiratory problems and mortality. PM10 is also associated with increases in cancer in some urban areas. Identification of toxic compounds in PM10 is a step toward estimating exposure to these compounds and evaluating their public health risk. However, the toxic compounds on PM10 are part of a highly complex mixture of compounds that makes chemical characterization difficult. Before this study, there has been little investigation of genotoxic compounds in particulate matter from Latin American cities. Here, both bioassay (mutagenicity) and chemical analyses were conducted with organic solvent extracts of PM10 collected from S?o Paulo, a major Brazilian city. Sequential extraction in dichloromethane (DCM) followed by acetone (ACE) yielded 20.3% and 10.2% of the total mass, respectively. Non-polar and moderately polar organic material solubilized in DCM. ACE extracted more polar organic species and some inorganic ions. Both extracts were fractionated separately using cyanopropyl-bonded silica chromatography with organic solvents of increasing polarity. The mass distribution among the fractions was measured. The mutagenic activity of the fractions was assayed using the microsuspension procedure with the Salmonella typhimurium tester strain TA98, with and without addition of metabolic enzymes (S9). The DCM extract had about four times higher mutagenic activity than the ACE extract. In general, addition of S9 resulted in an increase in mutagenicity of DCM fractions, but a decrease for the ACE extract. Most of the activity was concentrated in fractions in the mid-range of polarity within both the DCM and ACE extracts. The fractions were analyzed by gas chromatography with mass selective detection (GC/MS) without derivatization. The most mutagenic fractions in the DCM extract contained ketones, aldehydes, and quinolines. The most mutagenic ACE fraction had ketones, carboxylic acids, and aldehydes.     

The extraction of leukotrienes (LTC4, LTD4, and LTE4) from tissue fluids: the metabolism of these mediators during IgE-dependent hypersensitivity reactions in lung

The metabolites of arachidonic acid known as the leukotrienes are a class of lipid mediators which have potent and diverse biological effects in pulmonary tissue. Leukotrienes C, D, and E (LTC4, LTD4, and LTE4) are known to be principal mediators of immunoglobulin E (IgE)-mediated hypersensitivity reactions in lung tissue. It is therefore important to develop reliable and quantitative isolation techniques for estimating levels of these mediators in tissue. In this study, LTC4, LTD4, and LTE4 were separated from other arachidonate metabolites by organic extraction procedures. 5-Hydroxyeicosatetraeonic acid and leukotriene B4 extract efficiently into the organic layer of aqueous:ether or aqueous:chloroform extractions, whereas arachidonate metabolites containing conjugated peptides (e.g., LTC4, LTD4, and LTE4) failed to extract into these organic solvents. An extraction step was therefore developed that affords quantitative extraction of LTC4, LTD4, and LTE4 into the organic phase of an isopropanol:ether:H2O mixture. This step is the key for a two-step extraction method that isolates histamine, LTC4, LTD4, and LTE4 with a recovery of 100, 85, 75, and 57%, respectively. One advantage of this separation procedure for obtaining these mediators by organic extraction is an ability to expediently process many samples. Furthermore, the leukotriene content of extracted samples can be analyzed using the guinea pig ileum bioassay without interference from vasoamines or platelet-activating factor. These later substances are eliminated from leukotriene-enriched fractions by this extraction process. When histamine and LTC4 were added to supernatant fluids recovered from isolated lung tissue, they were quantitatively recovered using this extraction method.(ABSTRACT TRUNCATED AT 250 WORDS)     

A comparison of fractionation methods for forms of phosphorus in soils

We used l6 soils to compare the Hedley method for soil phosphorus fractionation to an alternative method recently developed by Ruttenberg to differentiate among P fractions in marine sediments. For forms of labile and Fe-bound P in soils, these methods were poorly correlated, with the Hedley fractionation showing a greater ability to discriminate among variations in plant-available P. For Ca-bound P, total organic P, and total P, the methods were well correlated (r² = 0.93, 0.48, 0.74, respectively), although the sum of P measured in the Ruttenberg extractions is only 45% of the total P recovered by the Hedley fractionation. The Hedley fractionation seems superior when an index of plant-available phosphorus and a separation of organic and inorganic forms is needed, whereas the Ruttenberg method allows a separation of CaCO₃-bound P from apatite-P, which is potentially useful in calcareous soils.     

The chemical character and burial of phosphorus in shallow coastal sediments in the northeastern Baltic Sea

The chemical composition and vertical distribution of sediment phosphorus (P) in shallow coastal sediments of the northeastern Baltic Sea (BS) were characterized by sequential extraction. Different P forms were related to chemical and physical properties of the sediments and the chemistry of pore water and near-bottom water. Sediment P composition varied among the sampling sites located in the Archipelago Sea (AS) and along the northern coast of the Gulf of Finland (GoF): the organic rich sites were high in organic P (OP), while apatite-P dominated in the area affected by sediment transportation. Although the near-bottom water was oxic, the sediments released P. Release of P was most pronounced at the site with high sediment OP and reduced conditions in the sediment-water interface, indicating that P had its origins in organic sources as well as in reducible iron (Fe) oxyhydroxides. The results suggest that even though these coastal areas are shallow enough to lack salinity stratification typical for the brackish BS, they are vulnerable to seasonal oxygen (O₂) depletion and P release because of their patchy bottom topography, which restricts mixing of water. Furthermore, coastal basins accumulate organic matter (OM) and OP, degradation of which further diminishes O₂ and creates the potential for P release from the sediment. In these conditions, an abundance of labile OP may cause marked efflux of P from sediment reserves in the long-term.     

Biodegradation of pyrene in sand,silt and clay fractions of sediment

Microbial degradation is the dominant pathway for natural attenuation of PAHs in environmental compartments such as sediments, which in turn depends on the bioavailability of PAHs. The bioavailability of PAHs has seldom been studied at the sediment particle size scale. We evaluated biodegradation of pyrene by Mycobacterium vanbaalenii PYR-1 as a function of sediment particle sizes, and investigated the relationship between the rate of degradation on sand, silt and clay particles with their individual desorption kinetics measured with the Tenax extraction method. Regression analysis showed that the total organic carbon (TOC), black carbon (BC), and specific surface area (SSA) of the specific particle size fractions, instead of the particle size scale itself, were closely related (P < 0.01) with the mineralization rate. While the fraction in the rapid desorption pool (F _rapid) ranged from 0.11 to 0.38 for the whole sediments and different size groups, the fractions mineralized after 336-h incubation (0.52 to 0.72) greatly surpassed the F _rapid values, suggesting utilization of pyrene in the slow desorption pool (F _slow). A biodegradation model was modified by imbedding a two-phase desorption relationship describing sequential Tenax extractions. Model analysis showed that pyrene sorbed on silt and clay aggregates was directly utilized by the degrading bacteria. The enhanced bioavailability may be attributed to the higher chemical concentration, higher TOC or larger SSA in the silt and clay fractions, which appeared to overcome the reduced bioavailability of pyrene due to sorption, making pyrene on the silt and clay particles readily available to degrading microbes. This conjecture merits further investigation.     

The chemical character and behaviour of phosphorus in poorly oxygenated sediments from open sea to organic-rich inner bay in the Baltic Sea

The chemical composition and vertical distribution of phosphorus (P) in poorly oxygenated sediments in a continuum extending from the open Baltic Sea towards an organic-rich inner bay were characterized by sequential extraction to examine the potential for release of sediment P. The chemical composition of P was related to chemical and physical characteristics of the sediments and the chemistry of pore water and near-bottom water to better understand the behaviour of P. Sediment P increased towards the inner bay, and the concentration of organic matter appeared to dictate its composition: the dominance of apatite-P turned to dominance of organic P (OP). Sediment P burial and, thus, release from sediment P reserves varied depending on the chemical composition of P. Dissolved species at the sediment–water interface suggested fluctuating redox conditions that affect P binding at short time scale. Redox-sensitive, iron (Fe)-bound P was usually relatively low because of poor oxygen (O₂) conditions, which emphasized the role of OP in P release. The results indicate that, over the long term, the abundant organic P reserve may support a significant continuing P release from hypoxic sediments in the severely eutrophied Gulf of Finland (GoF) because capture of P into Fe oxyhydroxides at the sediment surface is restricted. The average long-term minimum annual rate of P release from poorly oxygenated sediments below about 60 m depth in the GoF was approximated on the basis of the vertical distribution of sedimentary P forms and estimates of sedimentation rate.     

Determination of Distributions of Cd, Cu, and Pb Concentrations in Sediments of a Mexican Reservoir to Infer Their Environmental Risk

The José Antonio Alzate Dam in the State of Mexico, Mexico, receives wastewaters from domestic, industrial, and agricultural activities through the Lerma River. Chemical and physicochemical characteristics of the water were determined. Sediment has been studied in order to define the importance of its influence on the reservoir's state as a whole. The quantification of the metals, Cd, Cu, and Pb in total forms and the geochemical distribution and the chemical mobility of these metals in sediment have been established using a chemical sequential extraction scheme. The three metals showed a common characteristic, being more abundant in fraction F6 (residual), but the other fractions of the geochemical distribution were variable depending on the metal. First, the contamination level was evaluated with the results of the total metals, using the criteria of EPA, Thomas and Murdoch, and the Ontario Ministry of Environment for sediment in water bodies. Subsequently, the risk was assessed using the same criteria but considering the results of sequential extractions, where the geochemical distribution of each metal allowed a better understanding of metal portions with more influence on the risk, in which Cu and Pb presented low risk, but not Cd.     

The selectivity of a sequential extraction procedure for the determination of iron oxyhydroxides andiron sulfides in lake sediments

A popular sequential extraction procedure (Tessier et al. 1979) designed t o extract metals partitioned in various sediment phases, was evaluated for its selectivity. Amorphous FeOOH, FeS, and FeS₂ were added separately to natural lake sediments and sequentially extracted. The selectivity of the sequential procedure for the added solid phases was evaluated by determining the difference in the mass of Fe extracted from treated and control sediments. In the experiments where sulfide minerals were added, total S was measured in the residual solids in order to confirm selectivity of the method. Concentrations of total carbon remaining in the solid phase after each extraction step were also measured to determine the selectivity of the sequential procedure for carbon. The procedure was moderately selective for Fe added as FeOOH; a mean of 77 ± 12% (p < 0.05) of the Fe added was extracted in the step designed to reduce Fe-Mn oxyhydroxides. In experiments where FeS was added, a mean of 69 ± 11% (p < 0.05) of the Fe added as FeS was extracted in the fraction designed to oxidize sulfides and organic matter. Approximately 25% of the Fe added as FeS may have been extracted prematurely. Although less precise, total S analyses confirmed that much of the FeS was extracted in the oxidation step, yielding 104 ± 87% (p < 0.05) of the S added as FeS. The procedure was highly selective for FeS₂; 92 ± 14% (p < 0.05) of the Fe added as pyrite was extracted in the sulfide extraction step. Extraction of 80 ± 54% (p < 0.05) of S added as pyrite confirmed that FeS₂ were selectively extracted in the sulfide extraction step. Carbon in the sediments was also selectively extracted in the oxidation step (77 ± 2.4% of total C; p < 0.05). The applications and limitations of sequential extraction procedures as limnological research tools are discussed in light of our results. Request for offprints     

The effect of solvent extraction on antioxidant properties of apricot fruit

Two solvent extraction procedures were used to investigate the extraction efficiency in terms of total antioxidant capacity and total phenols in apricot fruit. Samples were either sequentially extracted with aqueous ethanol (ethanol/water 80% v/v) and tetrahydrofuran or directly extracted with tetrahydrofuran. Each extract was analyzed for total antioxidant capacity by the Trolox Equivalent Antioxidant Capacity (TEAC) assay and total phenols by the Folin-Ciocalteu assay. The results showed that using sequential solvent extraction, the majority (85%) of the total antioxidant capacity and total phenols was due to hydrophilic compounds. In tetrahydrofuran direct extractions, the total antioxidant capacity and total phenols were higher than values obtained with aqueous ethanol and the sum of results obtained from sequential extracts for either total antioxidant capacity or total phenols was similar to the tetrahydrofuran-extract antioxidant values. A linear correlation between total antioxidant capacity and total phenols was found and was independent of the solvent extraction method. In conclusion, the choice of solvent is related to the antioxidant potential of fruit and depends on the food hydrophilic/lipophilic composition.     

Analytical methods in bioassay-directed investigations of mutagenicity of air particulate material

The combination of short-term bioassays and analytical chemical techniques has been successfully used in the identification of a variety of mutagenic compounds in complex mixtures. Much of the early work in the field of bioassay-directed fractionation resulted from the development of a short-term bacterial assay employing Salmonella typhimurium; this assay is commonly known as the Ames assay. Ideally, analytical methods for assessment of mutagenicity of any environmental matrix should exhibit characteristics including high capacity, good selectivity, good analytical resolution, non-destructiveness, and reproducibility. A variety of extraction solvents have been employed in investigations of mutagenicity of air particulate; sequential combination of dichloromethane followed by methanol is most popular. Soxhlet extraction has been the most common extraction method, followed by sonication. Attempts at initial fractionation using different extraction solvents have met with limited success and highlight the need for fractionation schemes applicable to moderately polar and polar mutagenic compounds. Fractionation methods reported in the literature are reviewed according to three general schemas: (i) acid/base/neutral partitioning followed by fractionation using open-column chromatography and/or HPLC; (ii) fractionation based on normal-phase (NP) HPLC using a cyanopropyl or chemically similar stationary phase; and (iii) fractionation by open-column chromatography followed by NP-HPLC. The HPLC methods may be preparative, semi-preparative, or analytical scale. Variations based on acid/base/neutral partitioning followed by a chromatographic separation have also been employed. Other lesser-used approaches involve fractionation based on ion-exchange and thin-layer chromatographies. Although some of the methodologies used in contemporary studies of mutagenicity of air particulate do not represent significant advances in technology over the past 30 years, their simplicity, low cost, effectiveness, and robustness combine to result in their continued application in modern laboratories.