EPA-600/3-78-037 April 1978 Ecological Research Series ETHYLMERCURY: FORMATION IN PLANT TISSUES AND RELATION TO METHYLMERCURY FORMATION Environmental Monitoring and Support Laboratory Office of Research and Development U.S. Environmental Protection Agency Las Vegas. Nevada 89114 ------- RESEARCH REPORTING SERIES Research reports of the Office of Research and Development. U.S. Environmental Protection Agency, have been grouped into nine series. These nine broad categories were established to facilitate further development and application of environmental technology. Elimination of traditional grouping was consciously planned to foster technology transfer and a maximim interface in related fields. The nine sereies are: 1. Environmental Health Effects Research 2. Environmental Protection Technology 3. Ecological Research 4. Environmental Monitoring 5. Socioeconomic Environmental Studies 6. Scientific and Technical Assessment Reports (STAR) 7. Interagency Energy—Environment Research and Development 8. "Special" Reports 9. Miscellaneous Reports This report has been assigned to the ECOLOGICAL RESEARCH series. This series describes research on the effects of pollution on humans,plant and animal species, and materials. Problems are assessed for their long-and short-term influences. Investiga- tions include formations, transport, and pathway studies to determine the fate of pollutants and their effects. This work provided the technical basis for setting standards to minimize undesirable changes in living organisms in the aquatic, terrestrial, and atmospheric environments. This document is available to the public through the National Technical Information Service, Springfield, Virginia 22161 ------- EPA-600/3-78-037 April 1978 ETHYLMERCURY: FORMATION IN PLANT TISSUES AND RELATION TO METHYLMERCURY FORMATION By L. C. Fortmann, D. D. Gay, and K. 0. Wirtz Monitoring Systems Research and Development Division Environmental Monitoring and Support Laboratory P. 0. Box 15027 Las Vegas, Nevada 89114 U.S. ENVIRONMENTAL PROTECTION AGENCY OFFICE OF RESEARCH AND DEVELOPMENT ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY LAS VEGAS, NEVADA 89114 ------- DISCLAIMER This report has been reviewed by the Environmental Monitoring and Support Laboratory-Las Vegas, U.S. Environmental Protection Agency, and approved for publication. Mention of trade names or commercial products does not consti- tute endorsement or recommendation for use. ii ------- FOREWOKD Protection of the environment requires effective regulatory actions which are based on sound technical and scientific information. This information must include the quantitative description and linking of pollutant sources, transport mechanisms, interactions, and resulting effects on man and his environment. Because of the complexities involv- ed, assessment of specific pollutants in the environment requires a total systems approach which transcends the media of air, water, and land. The Environmental Monitoring and Support Laboratory-Las Vegas contributes to the formation and enhancement of a sound integrated monitoring data base through multidisciplinary, multimedia programs designed to: .develop and optimize systems and strategies for moni- toring pollutants and their impact on the environment .demonstrate new monitoring systems and technologies by applying them to fulfill special monitoring needs of the Agency's operating programs This report presents data demonstrating the biotransformation of elemental mercury in plants. The mercury, taken up as a vapor in its elemental state, is converted by the common garden pea to the toxic organomercurials, methylmercury and ethylmercury. The significance of this biotransformation will be considered by EPA and others in making decisions concerning regulations of activities known to generate mercury emissions. For additional information, please contact the Pollutant Pathways Branch, Environmental Monitoring and Support Laboratory-LV, P. 0. Box 15027. Las Vegas, Nevada 89114. George B. Morgan Director Environmental Monitoring and Support Laboratory Las Vegas, Nevada iii ------- INTRODUCTION Increased utilization of coal for energy production and continued industrial use of mercury may be expected to increase the levels of mercury pollutants in the environment in the future. Data are needed to define the effects of mercury pollutants on plants, the uptake and distribution of mercury within plants, and the species of mercury present and their bio- transformations within plants. Such data are essential to fully describe the impact of mercury on plants. The objective of this study was to examine the fate of one possible mercury pollutant, elemental mercury, in the tissues of Pisum sativum. CONCLUSION Both ethylmercury and methylinercury are formed in the pea following exposure to elemental mercury vapor. The pattern of change in concentration suggests both are metabolites of a single pathway. Methylmercury is identi- fied as an intermediate product of the pathway. The exact role of ethylmer- cury in this pathway cannot be defined at this time. MATERIALS AND METHODS Plant Material; Seeds of Pisum sativum, cv. Little Marvel were grown hydroponically in a greenhouse for 15 days before exposure. Exposure Conditions: Seventy seedlings were placed in a Plexiglas ® chamber of 58,000 cm3 volume, with 10 ml of elemental mercury in a tray placed on the floor of the chamber. The chambers were placed into a hood with constant air flow in order to maintain a temperature of 25 ±1 C, regardless of lighting conditions. Incandescent lighting at 110 uE m 2 sec 1 was used for a 12-hour daily light period. The concentration of elemental mercury vapor (Hg ) in the chamber was determined by gas chromato- graphy and calculated to be 1.71 ppb (Long, Scott and Thompson, 1973) with- in 30 minutes. A saturation level of 7.35 ppb was reached at 3 hours. Tissue Extraction; Tissue was ground by mortar and pestle with 2.21J HC1 (2 ml/g). The resultant brei was centrifuged at 10,000 rpm for 30 minutes. The supernatant fluid was then decanted and extracted with an equal volume of benzene (re-distilled nanograde) by vigorous shaking for 1 minute followed Registered Trademark ------- by centrifugation at 10,000 rpm for 10 minutes. This benzene fraction was passed through Whatman Phase Separating paper and then analyzed by gas chro- matography. The efficiency of the benzene extraction, as determined in our laboratory, agreed with the average of 76% reported by Talmi (1975). The efficiency of the extraction procedure for plant material was determined by extraction of 5-g plant samples to which known quantities of methylmercury (CH3HgCl) and ethyl- mercury (CaHsHgCl) had been added. Efficiency of the extraction was deter- mined to be 74% ± 2% for CH3HgCl and 69% ± 2% for C2H5HgCl. When a second benzene extraction of the aqueous phase was performed, an additional 21% of the original CH3HgCl and 20% of the added C2H5HgCl was obtained. For convenience and reduced handling of large numbers of samples during time-course experiments, the second benzene extraction was dropped. Having determined the benzene extracted to be 76% efficient, standards were pre- pared by a method similar to the plant extractions, i.e., known amounts of CH3HgCl and C2H5HgCl were added to 2.21J HC1, which was extracted with an equal volume of benzene. When this is used as the standard, reported values can be considered to be 95% ± 3% of actual concentration, without the neces- sity of using a correction factor. Sample Analysis: A Gas Chromatograph-Microwave Emission Spectrometer (GC-MES) system (Talmi, 1975) with a Gay-Frank optical system modification (Gay and Frank, 1977) was used for analysis of both air and benzene samples with the following operating conditions: Column: 3-foot by V-inch glass, packed with 4% FFAP (80/100 mesh) on Supelcoport® (Supelco Inc., Beliefonte, PA); Column temperature: 150 C for benzene samples, 30 C for air samples; Carrier gas: ultrapure argon at a flow rate of 11 ml/min; Temperature of injection port and detector; 225° C; Microwave generator output: 50 W incident, 3 W reflected power; Photomultiplier voltage: 500 V; Monochroma- tor slit width: 70 ym; and Spectral wavelength: 253.7 nm. The concentra- tion of mercury compounds, expressed as nanograms per gram (ng/g) in this report, represents nanograms Hg+ per gram fresh weight of identical tissues of control plants. This convention was necessary since the effect of Hg° toxicity is dessication of the leaf. RESULTS Initially, plants were exposed to elemental mercury for 24 hours to determine whether any organomercury compounds would be formed. As indicated in Table 1, C2H5Hg+ and CH3Hg+ were detected in all parts of the plant. There was no definite pattern of distribution of either metabolite within the plant with the exception of consistently high levels of both mercury species in the oldest lateral branch (stem and leaf). This lateral was the first to show visible signs of mercury toxicity. The pea, having a single growing point, was an ideal plant for study of a gas known to effect plant senescence (Speitel and Siegel, 1975). Damage to the plant occurred in a gradient from the first lateral to the top of the plant. The effects of mercury vapor ® Registered Trademark ------- toxicity consisted of wilting, followed by severe dessication of the leaf. An exposure duration was lengthened, each successive lateral up the stem wilted, then became severely dessicated, although no abscission occurred during the 48-hour period. TABLE 1. THE FORMATION OF ETHYLMERCURY AND METHYLMERCURY IN THE PEA AFTER EXPOSURE TO ELEMENTAL MERCURY VAPOR FOR 24 HOURS (Values reported are the average of triplicate samples and represent ng Hg+/gram fresh weight of identical tissue of control plants.) Plant Part 1st Lateral* 2nd Lateral* 3rd Lateral* 4th Lateral* 5th Lateral* Apex Stem Root Control C2H5Hg+ (ng/g) 12.82 ± 0.60 9.93 ± 0.35 5.40 ± 0.05 8.05 ± 1.81 6.99 ± 3.59 11.00 ± 1.67 5.22 ± 3.33 4.85 ± 1.34 N.D.** CH3Hg+ (ng/g) 19.21 ± 8.07 ± 4.21 ± 9.95 ± 6.49 ± 17.26 ± 10.77 ± 11.55 ± N.D.** 12.82 1.77 0.79 7.05 0.47 5.66 7.59 6.35 *Includes both leaf and stem, the 1st lateral branch being the lowest and oldest branch off the central axis. **None detectable in any plant part. In an attempt to define the relationship between the two mercury com- pounds, a time-course of exposure was performed. Concentrations of both CHsHg"1" and C2HsHg+ varied considerably over the 48 hours of exposure (Figure 1) In the aerial portion of the plant CaHsHg"*" concentration rose during the 48- hour period from 2.20, 4.05, and 4.25 ng/g to 25.92, 19.48, and 24.07 ng/g for the stem, apex, and laterals, respectively. A similar rise in concentra- tion was not observed for CH3Hg . Concentrations ranged from 1.79 ng/g to 17.28 ng/g in the aerial portion of the plant, with an average concentration of 4.66 ng/g. It is significant that in all aerial parts the CH3Hg+ concen- tration after 48 hours of exposure was nearly the same as that recorded at the first extraction (4 hours). Comparison of graphs a, b, and c of Figure 1 indicates a distinct pat- tern of concentration change in the aerial portion of the plant. Periods of ------- 8 12 16 20 24 28 32 36 40 44 48 HOURS OF EXPOSURE 8 I? 16 20 24 ?8 32 36 40 44 4B HOURS OF EXPOSURE 38- 32- 28- 24- .20- :16- 12- |B) APEX 8 12 16 20 24 28 32 HOURS OF EXPOSURE i-'"r CONTROL f""i 36 40 44 48 12 16 20 24 28 32 HOURS OF EXPOSURE 36 40 44 Figure 1. Changes in the concentration of ethylmercury and methylmercury in various plant parts of peas exposed to elemental mercury vapor for 48 hours. ------- high CgHsHg"^ concentration are periods of low CH3Hg+ concentration, and vice versa, so that the two curves are similar but are out of phase. To elaborate this relationship more fully, peas were exposed to elemental mercury vapor for a period of either 24 hours light or 24 hours continual darkness. The results indicate nearly twice as much CaHsHg"*" formed in the laterals and apex during the light period than in the dark (Figure 2). No C2HsHg+ could be detected in the stem or root under conditions of continuous darkness, despite concentrations of CHaHg comparable to those recorded for the plants exposed in the light. levels of CHsHg"1" in the plant. Light had no significant effect on the 32- 28- 24' 20- i 16- 12- i fc 8- 4- ^ P :•? 1 I g ^ LIGHT P II _b J I T P i| fe m I L # •f; *•* A | >;• •:•: 1 s r S' " • ^ETHYLMERCURY [^METHYLMERCURY [] TOTAL MERCURY -X- NONE DETECTABLE 1. S.E. OF THE MEAN .n L V I P p I f-; •.< Jl i; **. .*, ';. ;v p.;. Jn •M- •) •' •• DARK LIGHT DARK LIGHT DARK LIGHT DARK LATERALS STEM APEX ROOT Figure 2. The effect of light on ethylnxercury and methylniercury concen- tration in Pisuax sativua after a 24-hour escposure to mercury vapor. Both C2H5Hg+ and CH3Hg+ were detected in the root, although appreciable concentrations of CaHsHg+ were not observed until after 12 hours of exposure to Hg . The presence of these compounds can be explained by two possible mechanisms. Either they were formed in the root from mercury taken up from the water in which plants were grown, or they were transported from the aerial portion of the plant to the root. A less likely possibility is that all mercury detected in the aerial portion of the plant originated in the root. To determine the source of the organic mercury, the roots were "isolated" from the mercury vapor by placing the roots of seedlings grown in 5-ml micro- beakers into a 50-ml test tube, care being taken to form a tight seal between the beaker and test tube. A layer of activated charcoal was placed across the bottom of the microbeaker and was covered by a layer of vermiculite. As is indicated in Table 2, no C2H5Hg+ or CH3Hg+ was detected in the "isolated" ------- roots after a 24-hour exposure, despite formation of appreciable concentra- tions of both organomercury compounds in the aerial portions of the plant. TABLE 2. THE EFFECT OF ISOLATING THE ROOT MEDIUM FROM ELEMENTAL MERCURY VAPOR. (Exposure time, was 24 hours.) Root Medium Isolated Root Medium Exposed C2H5Hg+ (ng/g) CH3Hg+ (ng/g) C2H5Hg+ (ng/g) CH3Hg+ (ng/g) Apex Lat Stem Root 15.99 15.6 15.88 N.D.* 15.45 14.35 N.D.* N.D.* 12.67 6.73 8.04 4.25 11.62 4.99 3.18 6.43 *None Detectable. DISCUSSION The formation of both C2H5Hg+ and CH3Hg+ in peas exposed to Hg offers some fresh insight into the nature of the mercury pathway of the pea. Methyl- mercury formation in the pea has been reported previously by Gay (1975). +In both in vivo and in vitro experiments with inorganic mercury salts, CH3Hg was identified as an intermediate product. The data reported hereQsuggest that it may also be an intermediate in the biotransformation of Hg . This is supported by the following observations. (a) Although the level of C2H5Hg+ increased during the 48-hour exposure period, no corresponding rise in CH3Hg+ was observed. A baseline average of 4.66 nanograms CH3Hg+ per gram was maintained in the aerial portion of the plant with concentrations at 48 hours being nearly the same as those recorded at 4 hours. (b) Fluctuations in CH3Hg concentrations between replicate samples (Table 1 and Figure 2) suggest an intermediary role. The release of volatile mercury products from plants has been reported by Siegel (1974). His work resulted from the observation of analytical inconsistencies in data from re- plicate leaf samples. In this study, we observed similar inconsistencies in the CH3Hg+ data. However, standard error for C2H5Hg+ data was small. The efficiency of the extraction and analytical procedures being similar for both CH3Hg+ and C2H5Hg+, inconsistencies should have been observed for both, but were not. The apparent inconsistencies appear to be artifacts of the time intervals between extractions and the inability to detect other inter- ------- mediates or final mercury products, possibly because of their volatile nature. (c) Further verification of this role as intermediate is indicated by the failure of light to have any significant effect on CH3Hg"1" concentration despite a two-fold increase of CaHsHg"1" in the same tissue (Figure 2). Following the report that Hg vapor induces ethylene formation and abscission in Coleus and Citrus explants (Goren and Siegel, 1976), was considered a likely metabolite in the mercury pathway. The accumulation of CaHsHg"1" observed in this investigation verifies this initial assumption, but does not enable definition of its role as initial product, intermediary, or final product in this biochemical pathway. The pattern of concentration changes observed (Figure 1) does indicate that CH3Hg+ and C2H5Hg+ are both metabolites of a single pathway of mercury in the pea. In the aerial portion of the plant, a high concentration of either metabolite is followed by a high concentration of the other metabolite, with a simultaneous decrease in the concentration (or rate of increase) of the former. The net result of this would be to prevent accumulation of high concentrations of any single mercury metabolite, presumably by conversion to other, presently unidentified, mercury products. REFERENCES Gay, D. D. 1976. Methylmercury: Formation in plant tissues. Ecological Research Series. U.S. Environmental Protection Agency report. EPA-600/3- 76-049, Las Vegas, Nevada, May 1976. Gay, D. D. 1976. Biotransformation and chemical form of mercury in plants. Ecological Research Series. U.S. Environmental Protection Agency report. EPA-600/3-76-082, Las Vegas, Nevada, July 1976. Gay, D. D. and C. W. Frank. Personal Communication, July 1976. Goren, R. and S. M. Siegel. 1976. Mercury induced ethylene formation and abscission in Citrus and Coleus explants. Plant Physiology 57, 628-631. Long, S. J. , D. R. Scott, and R. J. Thompson. 1973. Atomic absorption of elemental mercury collected from ambient air on silver wool. Analytical Chemistry 45_: 22-27. Siegel, S. M., N. J. Puerner, and T. W. Speitel. 1974. Release of volatile mercury from vascular plants. Physiologia Plantarum 32:174-176. Speitel, T. W. and S. M. Siegel. 1975. Auxin and carbon dioxide sensitive effects of mercury and iodine vapors in plant senescence. Plant and Cell Physiology 16_: 383-386. Talmi, Yair. 1975. The rapid sub-picogram determination of volatile organo-mercury compounds by gas chromatography with a microwave emission spectrometric detector system. Analytica Chimica Acta 74:107-117. ------- TECHNICAL REPORT DATA (Please read Instructions on the reverse before completing) 1. REPORT NO. EPA-600/3-78-037 3. RECIPIENT'S ACCESSION-NO. 4. TITLE AND SUBTITLE ETHYLMERCURY: FORMATION IN PLANT TISSUES AND RELATION TO METHYLMERCURY FORMATION 5. REPORT DATE April 1978 6. PERFORMING ORGANIZATION CODE 7. AUTHOR(S) L. C. Fortmann. D. D. Gay, and K. 0. Wirtz 8. PERFORMING ORGANIZATION REPORT NO. 9. PERFORMING ORGANIZATION NAME AND ADDRESS Environmental Monitoring and Support Laboratory Office of Research and Development U.S. Environmental Protection Agency Las Vegas, Nevada 39114 10. PROGRAM ELEMENT NO. 1AA601 11. CONTRACT/GRANT NO. 12. SPONSORING AGENCY NAME AND ADDRESS U.S. Environmental Protection Agency-Las Vegas, NV Office of Research and Development Environmental Monitoring and Support Laboratory Las Vegas. Nevada 89114 13. TYPE OF REPORT AND PERIOD COVERED Final 14. SPONSORING AGENCY CODE EPA/600/07 15. SUPPLEMENTARY NOTES 16. ABSTRACT Seedlings of the common dwarf garden pea, Pisum sativum, cv. Little Marvel, exposed to elemental mercury vapor formed both methylmercury and ethylmercury in all parts of the plant. Concentrations of both organomercury compounds fluctuated considerably over a 48-hour exposure period, but the total of detectable forms of mercury continued to rise due to increased ethylmercury formation. Ethylmercury formation was greater in the light than in the dark, but methylmercury concentration did not differ significantly. The pattern of change in the concentrations of methylmercury and ethylmercury suggests both are metabolites of a single mercury pathway in peas. 17. KEY WORDS AND DOCUMENT ANALYSIS DESCRIPTORS b.lDENTIFIERS/OPEN ENDED TERMS c. COSATI Field/Group Plant physiology Plant chemistry Mercury Trace elements Leguminous plants 06A,CrF 07B,C 18. DISTRIBUTION STATEMENT RELEASE TO PUBLIC 19. SECURITY CLASS (ThisReport) UNCLASSIFIED 21. NO. OF PAGES 12 20. SECURITY CLASS (Thispage) UNCLASSIFIED 22. PRICE EPA Form 2220-1 (9-73) «U. S. 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