Abstract In this study I examined metabolic rates of Mytilus californianus located at the upper and lower extremes of the Mytilus distribution zone in an exposed rocky intertidal area at Hopkins Marine Station in Pacific Grove, CA. Mussels high in the zone spend less time exposed to normoxic conditions as a result of longer emersion periods. They also experience greater temperature fluctuations. Such abiotic stresses were expected to make metabolic rates among high and low mussels different. Respiration (O2 consumption) and malate dehydrogenase activities of gill tissue were used as indicators of metabolism. The design of this experiment led to mussel acclimation over a period of 25 days. When plotted against time, enzyme activities of low mussels showed a significant (p = 0.048 decrease in activity. Additionally, a significant (p = 0.014) decrease was observed in O, consumption of high mussels. The unexpectedly rapid physiological plasticity shown by M. californianus resulted in small sample sizes (enzyme n = 10, respiration n = 4) of freshly collected individuals, which may have contributed to the non-significant differences seen in high and low mussel MDH activities (p = 0.059) and respiration rates (p = 0.74). It was also concluded from this experiment that MDH activity is not a good predictor of respiration rate, possibly due to its role in both aerobic and anaerobic metabolism. 1. Introduction The rocky intertidal forms a variable environment where many specialized and diverse species thrive. Abiotic stresses such as tides, wave splash and impact, desiccation, food availability, and temperature establish steep gradients that affect how and where different organisms can survive in this highly variable macro-habitat (Denny 1988). As a result, intertidal species inhabit discrete vertical zones. Biochemical and physiological processes have been shown to vary between congeneric species and even between distinct conspecific populations residing at different heights (Pickens 1965, Hofmann & Somero 1995, Stillman & Somero 1996, Tomanek & Somero 2000). The purpose of this experiment was to further explore the relationship between physiology and vertical zonation in intertidal organisms. The experimental subject chosen was a sessile species, Mytilus californianus. It is a common prey for predatory animals (e.g. Pisaster ochraceous), making it a central species in community dynamics. Its range extends from the Aleutian Islands southward to Baja California and the species is usually found in the mid-intertidal zone of exposed coasts. Because of its mid-intertidal location, populations of M. californianus living at the lower extreme of the vertical zone are usually emersed only once a day during low tide. Conversely, individuals inhabiting the upper region experience long emersion periods, rarely being entirely submerged. Thus, upper mussels are more likely exposed to abiotic stresses such as desiccation, high temperature, and hypoxia. The physiology of high and low mussels was expected to differ as a result of the different environmental conditions in their microhabitats. One possible scenario was that high individuals, which have less time to feed and respire as a result of longer emersion periods, compensate by having bursts of aerobic metabolism when exposed to normoxic conditions (submerged). A second possibility is that low mussels are exposed to a richer source of nutrients and maintain a metabolic rate that is higher than that of mussels living higher in the distribution zone. Lack of literature and similar studies, however, made it difficult to give either scenario, or any other, more credibility. Consequently, the hypothesis here states only that metabolic rates of high and low mussels would be different. The indices of metabolic rate measured were respiration (O2 consumption) and activity of the enzyme malate dehydrogenase (MDH). 2. Materials & Methods 2.1. Animals Mussels (Mytilus californianus) were first collected on May 8", 2001 from a northwest facing rocky intertidal site at Hopkins Marine Station in Pacific Grove, CA. Approximately fifty mussels, 50 to 60 mm in length, were obtained from the upper and lower extreme at which M. californianus is found at that particular location. A second set of 8 samples of the same size was taken on the 26" of May from the same location. Shortly after sampling, the organisms were placed in large holding tanks with continuously flowing fresh seawater. 2.2. Experimental procedure Oxygen consumption rate was chosen because it is a good indicator of metabolism and has been used in previous studies (Babarro et al. 2000). A modification in this study was that dissected gill tissue was used instead of the entire organism. This was done because mussel gills have been found to continue respiring after removal. It is also a quicker and more efficient method because one does not have to wait for mussels to gape. Respiration was measured in a sealed, water-jacketed respirometer at 15°C using excised gill tissue. An oxygen sensitive electrode was attached to a Powerlab unit that allowed for collection and analyses of data on a computer. Each respiration run was began by assembling the chamber, which consisted of a stirbar, platform, and mesh pieces (used to hold gill tissue in place). The chamber was rinsed with filtered seawater (FSW) containing 15 mg of Penicillin G and 15 mg Streptomyocin per liter and then filled to capacity with more FSW. The system was allowed to thermally equilibrate. Meanwhile, calibration of the electrode took place. Dissection of the mussel gill was done as follows: the bivalve was opened by cutting the anterior and posterior adductor muscles, followed by carefully cutting and removing the gills from both valves. These were then placed in a petri dish filled with FSW containing antibiotics and washed twice with FSW. One gill was transferred to a beaker of FSW and placed in a water bath at 15°C. The other gill was kept in FSW on ice for use later in the enzymatic analysis. Once the chamber had reached 15°C it was purged of any air bubbles present. The gill tissue was carefully placed inside the mesh attached to the platform, making sure that the gill was securely in place. Not doing so resulted in the gill floating up and touching the electrode tip, which interfered with the electrode's measuring capability. The chamber was filled to the point of overflow and any newly introduced bubbles were removed. The lid was then placed on the chamber and screwed in place. It was important to make sure no air bubbles were present because they could have oxygenated the water resulting in erred measurements. The electrode was secured in place and recording was begun. Each gill tissue was measured for 30 minutes and then the wet weight of the gill was determined. Äfter the gill was removed, the chamber was refilled with FSW and resealed to quantify background respiration by bacteria. Control run measurements were recorded for 20 minutes. Every day the chamber was cleaned with a 10% bleach solution for 10 minutes. Any remaining bleach was deactivated with a 1% sodium thiosulfate solution. All parts were rinsed with deionized water and laid out to dry overnight. 2.3. Analysis Activities of MDH were measured because it is a simple enzyme to assay. This was an important consideration due to time constraints. There are limitations, however, to the use of MDH because it is an indicator of aerobic and anaerobic ATP generating capacity. See Figures 1 and 2 for the specific role of MDH in both metabolic pathways Therefore, the results obtained from MDH were closely examined and plotted against respiration rates to see if indeed this enzyme was a good aerobic metabolic indicator. The reaction MDH catalyzes is: Oxaloacetatic acid + NADH + H — Malate + NAD Although the substrate is oxaloacetic acid (OAA), the conversion of NADH to NAD is actually what was measured over time. The reason for this is that these two compounds have very different absorbances at 340 nm. Therefore, they provide a good means by which to perform a colorimetric assay. Malate dehydrogenase activity was measured spectrophotometrically at 340 nm at 15°C. The first step involved preparing a cocktail containing 50 ml of 200 mM imidazole buffer (pH 7.0 % 20°C), 0.0054 g NADH (final conc. = 0.15 mM), and 0.0014 g OAA (final conc. = 0.2 mM). This cocktail was prepared daily and kept on ice throughout the experiment because NADH and OAA degrade over time. The gill tissue was then weighed wet, minced, and homogenized in a five-fold dilution of 200 mM imidazole buffer. Finally, the homogenate was transferred to an eppendorf tube and centrifuged at 14,000 RPM for 5 minutes at 4°C. Spectrophotometer readings were taken using cuvettes filled with 2 mL of cocktail. To initiate the reactions, homogenate samples were transferred into cuvettes with a 25 uL Lang-Levy pipette. Reaction data were recorded for 30 seconds. Five replicates were taken for each sample of tissue. 2.4. Calculations and statistics Respirometry readings were converted from slopes describing decreases in O2 concentration over time to umol O2s g" wet wt. However, only the set of data points from 10 to 30 minutes were used. The reason for using only these data was that the first 10 minutes usually gave high values that were inconsistent with the rest of the data. Control slopes (10 to 20 minute data points) were first subtracted from experimental slopes and then converted using the equation: (chamber volume) * (A O2 concentration/100) * (O2 solubility) = X umol O2;s This value was then divided by the wet weight of the gill tissue. MDH results were standardized from A Absorbance/min to umoles OAA converted to malate per minute per gram of wet tissue. The first step was to convert A Absorbance/min to units of activity, which equals (A Absorbance/min * 2.0)/6.22. The value of 2.0 represents the amount of cocktail placed in the cuvette and 6.22 is the micromolar extinction coefficient for NADH. This value was then divided by the wet weight of the gill tissue, which had been homogenized in a 5X dilution of buffer. This meant that in every mL of homogenate there was 0.2 g of tissue (it was assumed that a gram of tissue had a volume of 1 mL). Because 25 uL of homogenate were added to each cuvette, every reaction had a total of 0.005 g of tissue. Thus, activity values were divided by this value. To obtain final values for a given gill, the five replicate values were averaged. Respiration rates and enzymatic activities of freshly collected high and low mussels were compared using one-way ANÖVA tests. Values of mussels that had been placed in holding tanks for more than one day were graphed over time and the resulting slopes were tested to see if they were significantly different from a slope of O. All calculations were done using Microsoft Excel. 3. Results 3.1. Respiration rate Freshly collected low M. californianus (n = 2) had oxygen consumption rates with an average of 0.00141 + 0.00027 umol O2 sec" g" wet wt. (mean + S.E.M.), while freshly collected high mussels (n = 2) had an average of 0.00126 + 0.00029 umol O2 sec gwet wt. These averages were not significantly different (p = 0.74). (Fig. 3) During the 25 days of the experiment, low and high mussels held in tanks with continuous flowing seawater exhibited a decrease in oxygen consumption, as can be seen in Fig. 4. The change observed in low M. californianus was significant (p = 0.014) whereas the change observed in high mussels was not (p = 0.126) 3.2. Malate dehydrogenase activity The activity average for freshly collected high mussels (n = 5) was 40.088 + 1.44 umoles OAA min" g wet wt. Average for fresh low mussels (n = 5) was 34.032 + 2.35 umol OAA min" g’ wet wt. Similar to respiration rate averages, these were not significantly different (p = 0.059). (Fig. 5) Over time, MDH activities also showed acclimatory changes. High mussels showed a significant (p = 0.048) decrease in activity during the 25 days they were held. An insignificant (p = 0.147) increase in activity, however, was noted in low mussels. See Fig. 6. 3.3. Respiration rates vs. MDH Activity When plotted against each other (Fig. 7) oxygen consumption rates and enzyme activity results showed that MDH was not a good predictor of aerobic metabolic rate. 4. Discussion The design of this experiment led to acclimation by Mytilus californianus, which confounded the results and did not allow me to conclusively answer the question of whether or not a metabolic difference exists between low and high intertidal mussel populations. Rather, this experiment strongly suggested that M. californianus is a plastic organism capable of modifying its physiology over a period of 25 days in response to environmental factors. This experimental design artifact resulted in small sample sizes of freshly collected organisms, which may explain the non-significant differences between low and high mussels. The results for fresh high (n = 5) and low (n = 5) mussel MDH activity were very close to being significant (p = 0.059). It is important to note, however, that because both indicators of metabolic activity showed significant convergences over time it is only logical that an initial difference exists between low and high M. californianus populations. The observed decrease in oxygen consumption rate of low mussels indicates a decline in metabolic rate. A speculative, yet logical, explanation for this observation is that low M. californianus were removed from their natural habitats, where they are normally submerged and exposed to a rich source of nutrients, and placed in holding tanks where food may have been less. This conjecture is supported by Dahlhoff and Menge’s (1996) finding that near shore food availability is strongly correlated to metabolic activity. Their results showed that mussels living at a wave-exposed site with relatively high phytoplankton concentrations had higher citrate synthase and MDH activities than organisms living at a wave-protected site with low phytoplankton concentrations. As explained in the introduction, MDH is involved in aerobic as well as anaerobic metabolism. The results attained in this experiment seem to be better explained by the enzyme's role in anaerobiosis. Because high mussels have longer emersion periods they also have longer time spans in which they must close their valves to prevent desiccation. This forces high organisms to switch over to anaerobic metabolism for extended periods of time, resulting in a reliance on MDH for producing ATP under oxygen-limited conditions. Thus, when high M. californianus are placed in an environment where they are continuously submerged, as it was in the holding tanks, one would expect to see a decrease in the enzyme’s activity because the need for generating ATP anaerobically is reduced. This is what was indeed observed. The preceding argument that MDH activities measured in this experiment were largely activities of anaerobic metabolism would also explain why such poor correlation was seen between respiration rates and enzyme activities. In the future I think it would be interesting to repeat this experiment using a larger number of freshly collected samples from more than one site to control for any possible location factors. It may also be interesting to use entire mussels for respiration measurements as opposed to only gill tissue. Perhaps doing a long-term study would reveal seasonal variation in these two M. californianus populations. Another possible experiment would be to use an enzyme involved only in aerobic metabolism, such as citrate synthase. Finally, I think it is worth designing an experiment in which mussels are exposed to abnormally long periods of emersion and heat stress and then tested for MDH activities. This would show whether or not MDH activity measurements in Mytilus californianus are actually from anaerobic metabolism. 5. Conclusions This experiment illustrated that Mytilus californianus is a physiologically plastic organism capable of altering its metabolic rate over a period of 25 days, as shown by a decreasing respiration rate in laboratory-acclimated mussels from low sites in the intertidal zone, and a decrease in MDH activity in laboratory-acclimated high organisms The results did not, however, indicate metabolic rate differences between freshly collected high and low populations of M. californianus. Additionally, the two indices used to measure metabolic rate, MDH activity and respiration, showed no correlation. 6. Acknowledgements 1 am grateful to Peter Fields for his help with the MDH assays and overall support and advice; Karen Braby and Eric Sanford for their help with the respirometry measurements; George Somero for all the guidance, advice, and the idea of this project; Jim Watanabe for help in analyzing data; and Jason Podrabsky for his help editing this manuscript. In closing I would like to thank the rest of the Somero lab for making this experience enjoyable and all the 175H Professors for the introduction into the world of research. 7. Literature Cited Babarro, J.M.F., Fernandez-Reiriz, M.J., and Labarta, U. 2000. Metabolism of the mussel Mytilus galloprovincialis from two origins in the Ria de Arousa (north-west Spain). Journal of the Marine Biological Association of the United Kingdom. 80: 865-872. Dahlhoff, E.P. and Menge, B.A. 1996. Influence of phytoplankton concentration and wave exposure on the ecophysiology of Mytilus californianus. Marine Ecology Progress Series. 144: 97-107. Denny, M.W. 1988. Biology and the Mechanics of the Wave-Swept Environment, Princeton University Press, Princeton, NJ Hofmann, G.E. and Somero, G.N. 1995. Evidence for protein damage at environmental temperatures: seasonal changes in levels of ubiquitin conjugates and hsp70 in the intertidal mussel Mytilus trossulus. The Journal of Experimental Biology. 198: 1509-1518. Pickens, P. E. 1965. Heart rate of mussels as a function of latitude, intertidal height, and acclimation temperature. Physiological Zoology. 38: 390-405. Stillman, J.H. and Somero, G.N. 1996. Adaptation to temperature stress and aerial exposure in congeneric species of intertidal porcelain crabs (genus Petrolisthes): correlation of physiology, biochemistry and morphology with vertical distribution. The Journal of Experimental Biology. 199: 1845-1855. Tomanek, L. and Somero, G.N. 2000. Time course and magnitude of synthesis of heat- shock proteins in congeneric marine snails (genus Tegula) from different tidal heights. Physiological and Biochemical Zoology. 73(2): 249-256. 8. Figure Legend Fig. 1. Aerobic metabolism, indicating role of MDH. Fig. 2. Anaerobic metabolism, indicating role of MDH. Fig. 3. Average respiration rates of high and low freshly collected mussels. Error bars are standard errors of the means. Fig. 4. Respiration rates of laboratory-acclimated mussels plotted against the number of the day the sample was tested. Fig. 5. Average enzyme activities of high and low freshly collected mussels. Error bars are standard errors of the means. Fig. 6. Enzyme activities of laboratory-acclimated mussels plotted against the number of the day the sample was tested. Fig. 7. Respiration rates of high and low mussels plotted against enzyme activities of high and low mussels. Fig. 1. GoP pyluvate ----. AcetylCoA oxoloocelote citrate cis-ôconitate malate isodit fumarate a-ketoglutarate, A 0 succingte succinylCoA 21 12 21 124 24 S NV NAD ADP-P;— LAIEI flovoprotein cytochrome b ADP-P,— cytochrome c cylochrome a ADP.PAT 2H++0, HO ELECTRON TRANSFER CHAIN C Fig. 2. GLYCOGEN P. GP GLUCOSEG6P ATP ADP ATP¬ ADP— FBP GAP -NAO+ 4----- ----- --- NA NADHA —NADH 3DPG — ADP — ATP 3964 2P6A PEF — ADP — ATP osportote pyruvote oetycoa NADH oxoloocetate aloniney NADH ethono alanopine NAD. strombine ocetote molote lysopine octopine fumorgte -ADP loctote succinoreATP — ADP — ATP propionote NAD Fig. 3. 0.0018 0.0016 0.0014 5 0.0012 0.001 0.0008 5 0.0006 O.0004 0.0002 Mean Respiration Rates of Fresh Mussels p=0.74 (2) (2) High Low Fig. 4. 0.0018 0.0016 0.0014 0.0012 0.001 0.0008 0.0006 0.0004 0.0002 Respiration vs. Day Äfter Collection Low R° = 0.7299 P=0.014 ... .. High Mussels High R“ = 0.403 Low Mussels p-0.126 Linear (Low Mussels) - - - Linear (High Mussels 10 20 30 Day Fig. 5. 45 40 o 35 5 30 20 01 Mean Fresh Mussel Enzyme Activity p=0.059 (5) Low High Fig. 6. 40 38 36 - 34 § 32 § 30 5 28 26 5 24 + 22 20 Enzyme Activity vs. Day after Collection High R“ = 0.574 p-0.048 High Mussels Low Mussels - - - Linear (High Mussels —Linear (Low Mussels) LOW R2 = 0.3704 p=0.147 20 30 Day Fig. 7. 0.0018 50.0016 3 0.0014 NO.0012 0 5 0.001 0.0008 50.0006 8 0.0002 Respiration vs. Enzyme Activity P2 5 00518 R?=0.4753 30 Activity (umol OAA min g*) High Mussels Low Mussels Linear (Low Mussels) - - - Linear (High Mussels) 20 40