Analysis of Selenium in Fish Tissue: An Interlaboratory Study on Weight Constraints.

Environmental monitoring programs that target fish tissues for selenium (Se) analysis present unique sampling and analytical challenges. Selenium monitoring programs ideally focus on egg/ovary sampling but frequently sample multiple tissues with varying lipid content, often target small-bodied fish species because of their small home ranges, and require reporting in units of dry weight. In addition, there is a growing impetus for nonlethal tissue sampling in fish monitoring. As a result, Se monitoring programs often generate low-weight tissue samples of varying lipid content, which challenges analytical laboratories to quantify tissue Se concentrations accurately, precisely, and at desired detection limits. The objective of the present study was to stress-test some conventional analytical techniques used by commercial laboratories in terms of their ability to maintain data quality objectives (DQOs) in the face of sample weight constraints. Four laboratories analyzed blind a suite of identical samples, and data were compared against a priori DQOs for accuracy, precision, and sensitivity. Data quality tended to decrease with decreasing sample weight, particularly when samples were less than the minimum weights requested by the participating laboratories; however, effects of sample weight on data quality were not consistent among laboratories or tissue types. The present study has implications for accurately describing regulatory compliance in Se monitoring programs, highlighting some important considerations for achieving high data quality from low-weight samples. Environ Toxicol Chem 2023;42:2119-2129. © 2023 SETAC.

Feeding response in marine copepods as a measure of acute toxicity of four anti-sea lice pesticides.

Anti-sea lice pesticides used in salmon aquaculture are released directly into the environment where non-target organisms, including zooplankton, may be exposed. The toxicity of four pesticides to field-collected copepods was examined in 1-h exposures with lethality and feeding endpoints determined 5-h post-exposure using staining techniques. Copepods were immobilized within 1 h, at aquaculture treatment concentrations of deltamethrin (AlphaMax), cypermethrin (Excis), and hydrogen peroxide (InteroxParamove50). All organisms showed vital staining, indicating immobilized organisms were still alive, thus LC50s were not determined. Feeding on carmine particles was inhibited and EC50s ranged from 0.017 to 0.067 µg deltamethrin/L, 0.098-0.36 µg cypermethrin/L, and 2.6-10 mg hydrogen peroxide/L, representing 30- to 117-fold, 13- to 51-fold, and 120- to 460-fold dilutions of the respective aquaculture treatments. No effects were observed in copepods exposed to azamethiphos (Salmosan) at 5-times the aquaculture treatment. Acute exposure to three of the four pesticides affected feeding and mobility of copepods at environmentally-realistic concentrations.

Accumulation and depuration of polychlorinated biphenyls from field-collected sediment in three freshwater organisms.

As laboratory-based bioaccumulation methods are standardized and expanded to include other test species, kinetic studies assessing the major classes of contaminants with these species are needed to adequately select the standard duration for bioaccumulation tests. In the present study we measured the uptake (28-d exposure) of polychlorinated biphenyls (PCBs; total and selected congeners) from field-contaminated sediment in the oligochaete Lumbriculus variegatus, mayfly nymph Hexagenia spp., and fathead minnow Pimephales promelas. Depuration (25 d) of PCBs was measured in organisms that had been transferred to clean sediment after the 28-d exposure. Uptake and elimination of PCBs was rapid in L. variegatus and Hexagenia spp. Tissue residues reached steady-state concentrations within 28 d; elimination rates and biota-sediment accumulation factors (BSAFs) of the PCB congeners were not correlated with K(OW). Uptake and elimination rates of PCBs were slower in P. promelas, and it is not clear whether steady-state was reached in fish tissues. Elimination rates of the PCB congeners significantly decreased with increasing K(OW) in fish. The appropriateness of a 28-d exposure for measuring steady-state concentrations in tissue of the invertebrates was confirmed, but further study is required for fish.

Validation of Ontario's new laboratory-based bioaccumulation methods with in situ field data.

To validate the standardization of a laboratory protocol for measuring bioaccumulation, laboratory-derived tissue residues and biota-sediment accumulation factors (BSAFs) were compared with historical field data from nine sites in Ontario, Canada. As a result of temporal discontinuity between the field and the laboratory studies, a priori considerations, such as changes in site conditions or concentrations of contaminants in sediment, were necessary to assess whether to compare absolute or relative measures of bioaccumulation. For the majority of sites, BSAFs for field-collected and laboratory-exposed fish were within a factor of 2. Biota-sediment accumulation factors for laboratory-exposed oligochaetes were typically greater than those for mussels caged in the field, by a factor of 2 to 9. Overall, the laboratory methods for all species generally overestimated the relative bioavailability of contaminants compared with field conditions by a factor of 1.1 to 9.2. Other than the great disparity observed for polychlorinated dibenzo-p-dioxins and dibenzofurans (PCDD/Fs) between field and laboratory studies, on average the laboratory-derived BSAFs with Pimephales promelas and Lumbriculus variegatus overestimated those from field-collected fish and field-exposed mussels by factors of 1.6 and 3.6, respectively. The laboratory method reflects a potentially worst-case exposure scenario and provides an appropriately conservative estimate of bioaccumulation. Laboratory-based estimates can be comparable to bioaccumulation data from the field but may be confounded by species-specific differences in routes of exposure and bioaccumulation of certain compounds or other environmental and biological factors that should be considered in these comparisons.

A comparison of the bioaccumulation potential of three freshwater organisms exposed to sediment-associated contaminants under laboratory conditions.

In the field of sediment quality assessment, increased support has been expressed for using multiple species that represent different taxa, trophic levels, and potential routes of exposure. However, few studies have compared the bioaccumulation potential of various test species over a range of sediment contaminants (hydrophobic organics and metals). As part of the development and standardization of a laboratory bioaccumulation method for the Ontario Ministry of the Environment, the oligochaete Lumbriculus variegatus, mayfly nymph Hexagenia spp., and juvenile fathead minnow Pimephales promelas were exposed to a variety of field-contaminated sediments (n = 10) to evaluate their relative effectiveness for accumulating different contaminants (e.g., dichlorodiphenyltrichloroethane [DDT] and metabolites, polychlorinated biphenyls [PCBs), polycyclic aromatic hydrocarbons [PAHs), polychlorinated dibenzo-p-dioxins and dibenzofurans [PCDD/Fs), and heavy metals). Bioaccumulation was usually highest in L. variegatus but also most variable within and (relative measures) between sediments. Bioaccumulation was similar between L. variegatus and Hexagenia spp. in most of the sediments tested. Significant differences in bioaccumulation between species were observed for DDT, dichlorodiphenyldichloroethane (DDD), PAHs, and PCDD/Fs. The present study indicates that species-specific differences in bioaccumulation may, but do not always, exist and can vary with contaminant and sediment type. The choice of test species or combination to use in a standard test method may depend on the objectives of the sediment quality assessment and data requirements of an ecological risk assessment. The results of the present study provide insight for selection of test species and validation of laboratory methods for assessing bioaccumulation with these species, as well as valuable information for interpreting results of bioaccumulation tests.

Measuring bioaccumulation of contaminants from field-collected sediment in freshwater organisms: a critical review of laboratory methods.

To be effective, decision-making frameworks require data from robust and reliable test methods. Using standard methods allows for more effective comparison between studies and application of data, and it reduces unnecessary duplication of efforts. Laboratory methods to assess the toxicity of sediment have been standardized and extensively used; however, procedures for measuring the bioaccumulation of contaminants from sediment into aquatic organisms need further standardization. Bioaccumulation methods using freshwater invertebrates and fish exposed to field-contaminated sediment were reviewed to identify important similarities and differences in method protocols, test conditions that need to be controlled, and data gaps. Although guidance documents are available, great variation still exists in exposure techniques used in tests, which may potentially affect the estimation of bioaccumulation. The techniques most consistent across studies include the use of Lumbriculus variegatus as a test species, test temperatures between 20 and 25°C, and a 28-d exposure with no addition of food, followed by purging of organisms. Issues that were inconsistent between studies or remained unspecified, which should be addressed, include the bioaccumulation potential of other test species, loading density of organisms, and sediment-to-water ratio. In addition to proper evaluation of the various exposure techniques and conditions, a need exists for more consistent inclusion of quality control procedures during testing.