Abstract Heat shock proteins are one type of molecular chaperone. Their primary responsibility is to help refold proteins that are denatured due to high temperatures These proteins are essential for organisms living at the edges of their thermal ranges, for example, many intertidal organisms which may be exposed to potentially lethal temperatures during low tide periods. An example of such an intertidal organism is the mussel Mytilus californianus, which is found in both subtidal and intertidal locations, and can often experience temperatures of 30° C and higher. Such temperatures were seen in the two artificial tide pools, one subtidal and one intertidal, which were created for this study. Equal numbers of M. californianus ranging in size were placed in the two pools and samples were collected over five weeks. Subsequent analysis showed that Heat shock protein-70 (Hsp 70) is expressed in response to extreme temperatures. The expressed Hsp 70 was visualized on the gels as two isoform bands - band 1 and band 2. Comparing the mean band 1 and band 2 intensities of Hsp 70 for both subtidal and intertidal groups of M. californianus over five weeks has shown that the intertidal group had elevated levels of Hsp 70 in comparison to the subtidal group for all weeks compared. Introduction In order for proteins to function properly they need to be able to reversibly change their conformations. As a result, proteins need to be marginally stable. That is, they need to be able to perform rapid changes in their three-dimensional configuration while at the same time remain adequately stable at physiological temperature. However, proteins are often exposed to temperatures above their normal physiological temperatures and as a result these proteins become denatured. Proteins can be reversibly or irreversibly denatured. Thus, cells need an elaborate system to either restore the function of reversibly denatured proteins or to dispose of irreversibly denatured proteins. One particular class of proteins that are involved in these "clean up" processes are known as heat shock proteins. In 1962, Ritossa observed that the chromosomes in the salivary glands of heat stressed Drosophila melanogaster showed a distinct pattern of "puffing" (Figure 1) This indicated that some class of genes was being strongly transcribed as a result of high temperatures (Somero, 1995). This response became known as the heat shock response and the resulting proteins became known as heat shock proteins. It is now known that there a number of different classes of heat shock proteins synthesized as a result of heat stress. The Hsp70 family is highly conserved across species and is the most widely induced in respond to heat stress. In nature, the temperature at which the synthesis of heat shock proteins is first induced, the threshold induction temperature, varies widely among species. This makes sense since different species are evolutionarily adapted to different temperatures and have proteins with different thermal sensitivities. Therefore, what might constitute heat stress for one species might be within the normal range of temperatures for another. However, induction temperatures are known to change with seasonal acclimatization and with laboratory acclimation (Somero, 1995). These changes in the induction temperature can be attributed to induced thermal tolerance In order to achieve induced thermal tolerance, also known as heat hardening, an organism must first be exposed to sub-lethal heat stress, which causes the synthesis of heat shock proteins, and then allowed to recover. If the organism is then exposed to severe heat stress it may exhibit tolerance to these new higher temperatures. It should be noted that heat shock proteins are not only synthesized in response to heat stress. Instead, they may be induced by a number of cellular stresses. Such stresses include chemical stress and physical stress. Thus it might be more appropriate to call the "heat shock response" the "stress response." Heat shock proteins are a subset of a broad class of proteins called molecular chaperones. In most, if not all, cells molecular chaperones are present during non¬ stressful times and additional proteins are induced in response to stress. In normal cellular function molecular chaperones are responsible for the proper folding and compartmentalization of proteins (Figure 2) The heat shock response does not occur without a great deal of energy being consumed. The source of ATP use is in the production of the heat shock proteins and the subsequent re-folding of denatured proteins. Thus, there is strict regulation of transcription and translation of heat shock proteins. The model of regulation presently in use suggests that the amount of free heat shock protein in the cell serves as a signal for the amount of transcription of Hsp genes that is needed (Craig and Gross, 1991). Furthermore, Craig and Gross suggest that there are three elements involved in the regulation of heat shock protein production (Figure 3). The first element is the amount of free heat shock protein. The second element is the concentration of heat shock factor (HSF). The third element is heat shock element (HSE), which is the gene regulatory element. Under normal conditions in the cell, Hsp70 binds to HSF to form a complex. Thus there is very little free HSF or Hsp70 in a cell without heat stress. As a result, no Hsp70 will be produced. Once heat stress occurs this complex breaks down and the Hsp70 binds to denatured proteins. HSF is then free to bind to HSE, the gene regulator, and transcription and translation of additional Hsp70 occurs. With increased heat stress more and more of the Hsp7O- HSF complex disassociates. In other words, the level of Hsp70 production is related to the intensity of the heat stress. Looking at heat shock expression in a particular species can give us insight to that animal's environment. Many species are often living at the edges of their thermal ranges. By looking at Hsp 70 expression in animals held in particular environments we can understand the thermal ranges of species and tease apart why certain species are found in different parts of the intertidal. In addition, if the pattern of Hsp 70 expression is followed over a period of time we can understand the ability of organisms to acclimate to thermal stress as well as to changes in their environment. This study looks at the expression of heat shock proteins in subtidal and intertidal Mytilus californianus in hopes of understanding some of these patterns. This study also looks at the expression of heat shock proteins in M californianus of different sizes. It has been shown that the body temperature of large mussels rises rapidly and remains high during low tide periods. The body temperatures of smaller mussels, on the other hand, fluctuate with environmental conditions. It is possible that mussels of different sizes express Hsp 70 in different quantities or at different times in order to deal with different body temperature patterns. Understanding such patterns could provide substantial insight as to how M californianus and other intertidal organisms survive heat shock and other stress during development. Materials and Methods Aquaria Setup and Mussel Collection Prior to the start of this experiment, I collected approximately 300 M. californianus and placed them in an indoor aquarium with a flow-through water system. These mussels were left in this tank for one week in order for them to acclimate to a common temperature. During this week two "tide pools" were set up, one intertidal and the other subtidal. Both pools were made out of kiddy pools. The bottoms of the pools were covered with rocks and these rocks were then covered with burlap. There was a drain in the side of each pool below the level of the burlap. This way the intertidal pool could drain completely and the mussels placed on the burlap would see complete emersion. Both pools had a flow-through water system. The subtidal pool was left running all of the time, and the flow-through system for the intertidal pool was outfitted with a timer which controlled the "tides." Low tide occurred every day from 10am to 2pm. ÄAfter the collected mussels had been in the indoor aquarium tank for one week 20 mussels with a wide range of body sizes were collected and kept as a control group. The remaining mussels were divided into two groups of equivalent size ranges and numbers (147 per pool) and placed in the two tide pools. Äfter one week eight mussels ranging in size from small to large were collected from each pool. In addition to the mussels collected from the two tide pools, eight mussels were also collected from the intertidal site where all of the mussels were originally collected. This sample of eight mussels also ranged in body size from small to large. This collection protocol was repeated weekly for five weeks. Once these samples were collected, all of the mussels were measured and dissected. The length, width and height of the shell were measured as well as the full body weight and the soft body weight. Both gills and the abductor muscle were kept. One gill from each mussel was then homogenized with a lysis buffer (30ml: 7.5ml 32mM Tris-HCL pH 6.8, 6ml 2% SDS (10% stock solution, 60ul 1mM EDTA (500 mM stock), 150ul 0.25mg/ml Pefabloc, 60ul 10ug/ml Pepstatin, 60ul 10ug/ml Leupeptin 16.70ml H20) in a 1:5 ratio and the protein concentration was quantified. Protein Analysis: SDS-PAGE and Western Blot Next, SDS-PAGE was used to resolve the proteins of each of the samples, which were run in duplicate. In addition, in each gel 3ul of Hsc 70 were run as a way to standardize each gel so that they could be compared. When the gels are transferred and finally exposed to film the resulting "picture" may not have the same intensity from gel to gel. By having Hsc 70, a band of known quantity, in the gel one can compare the intensity of that band to the rest of the bands in the gels when quantifying. Thus the resulting intensities of the bands from gel to gel for the samples will be standardized. All gels were run for one hour at 200 volts. The proteins on each gel were then transferred to a nitrocellulose membrane. The transfer was done at 80 volts for one hour and fifteen minutes (Laemmli, 1970). Next, Western Blots were run on each of the membranes. The membranes were placed in a blocking buffer (250ml: 25ml 1XTBS, 12.5g 5% non-fat dried milk, 0.05g 0.02% Thimesosol, 0.250ml 0.1% Tween, add H2O) for one hour. The primary alpha antibody MA3-OO1 was then added to the membranes for one hour. The membranes were then washed with 1XTBS with and without Tween. The second antibody, A8-4000, was then added for 30 minutes, and the membranes were then washed again. Finally a Protein A-peroxidase mixture was added to the membranes for one hour followed by the washes (Laemmli, 1970). The membranes were then exposed to equal volumes of Enhanced Chemiluminescence (ECL) reagents 1 and 2 for one minute and then wrapped in Saran wrap (Pierce Chemical Company, Super Signal: Western Blotting Substrates Handbook). Chemiluminescence is the reaction that occurs between an enzyme like horseradish peroxidase (HRP) and a chemiluminescent molecule. This reaction results in an intensified light emission which allows the band images to be captured on pre flashed, X-ray film (Kodak) when exposed. During the course of this study exposed time was set at 30 seconds and the film was then immediately developed. then scanned the developed film into a computer using Lab Scan, a digital computer scanning program. Each band on each gel was then quantified using Image Master 1-D Prime software. The results for each gel were standardized using the Hsc7O quantity for that particular gel. Finally, the statistical program Systat was used to compare the subtidal and intertidal treatments overall and per week. Temperature Data Temperature data were collected using StowAway XTI data logger chips stored in waterproof containers. Four data loggers were set out at the start of the experiment. One was placed in the subtidal pool to record water temperatures. The remaining three were placed in the intertidal pool, one to record water temperatures, one to record the body temperatures of a small mussel, and one to record the body temperatures of a large mussel. All of the data loggers were pre tested for accuracy and were then set to record the temperature every ten minutes throughout the course of the study. At the end of the experiment the data were retrieved. Only data from the small intertidal mussel data logger could be retrieved. Results Figures 4 and 5 show the mean band intensities for the two Hsp 70 isoforms - bands 1 and 2 - for the subtidal and intertidal treatments for weeks 1-3. The control point corresponds to the original twenty mussels that were dissected after being held in an indoor tank for one week. Figure 4 shows that for all three weeks the intensity of Hsp 70 - band 1 for the intertidal treatment was higher then the intensity of Hsp 70 - band 1 expression for the subtidal group. Statistical analysis using Systat shows that overall this difference is statistically significant (p-value= 0.008). Statistical analysis was also done to make pairwise comparisons of both treatments for each week. For band 1 intensity differences between treatments were significant only for week 2 (p-value = 0.021). Since there are presently no field data for week 1, the statistical tests did not incorporate this "treatment. Figure 5 shows the mean band 2 intensity data. Again, the intertidal treatment group had higher intensities of Hsp 70 expression for all three weeks. Overall, the treatment effects were statistically significant (p-value =0.000). Statistical comparisons were then done by week. For the band 2 intensities both weeks 1 and 3 were statistically different (week 1 p-value = 0.019, week 2 p-value = 0.005). The p¬ value for week 2 (p-value = 0.061) was close to being statistically significant. Once again, there are presently no field data for week one and, therefore, this group was not included in the statistical tests. Figure 6 shows the body temperatures of a small mussel in the simulated intertidal pool over the course of the study. The peaks corresponds to highest temperatures seen during low tide periods. The base line is roughly 15°C, the temperature of the water coming through the flow-through system. Discussion The results collected thus far suggest that the intertidal mussels are indeed experiencing heat stress. Both bands 1 and 2 are showing elevated levels of Hsp 70 expression in the intertidal treatment over the subtidal treatment. These results are in agreement with the data that G. E. Hofmann and G. N. Somero gathered during their 1995 and 1996 studies. In comparison to the control mussels the Hsp 70 level after one week has increased. However, what is not clear is why the subtidal group seems to follow the same pattern of Hsp 70 expression but at a lower level. It is possible that the stress of being moved from the intertidal, being placed indoors for a week and then being returned to an environment, which may have no had a well established food supply, was sufficient to induce Hsp 70 expression. Add to that stress the heat stress seen by the intertidal group daily and you could explain the patterns of expression, as well as the elevated levels of expression in the intertidal group. As the weeks went on the subtidal group began to see an established community of algae in their pool. The intertidal group also saw the establishment of an algal community, but to a much lesser extent then the subtidal group. It is possible that this well-established algal community means that the subtidal pool is seeing high levels of nutrients and food, and subsequently the mussels in this pool might also be seeing high levels of food. These high food levels could give the mussels a larger energy budget from which to produce proteins like Hsp-70. Thus, the establishment of these algal communities is one way to explain the lower levels of Hsp 70 expression during week three. However, this is not the only hypothesis which might explain the lower levels. It is possible that around week three the mussels had begun to acclimate to their new environment and thus were less stressed. It is also possible that the lower levels of Hsp 70 expression in week 3 can be attributed to environmental conditions. The temperature data show that during the first two weeks the small mussel was seeing temperatures around 35°C almost every day. During the 3rd week, however, there were very few days where the temperatures got higher then 20°C. These lower temperatures could be sufficient to lower the Hsp 70 expression. This hypothesis could also explain the mirror pattern of the subtidal treatment. Even though the pools are designed as a flow-through system the rate of drainage is less the rate of water flow. This is done so that water will stay in the pool. As a result, it is possible that during hot sunny days the subtidal water was actually heating up causing heat stress. However, without the data logger information for this pool it is impossible to know exactly what the water temperatures were like during the course of this study. This hypothesis can be supported using Hofmann and Somero's (1995) study of Mytilus trossulus. This study showed seasonal variation of Hsp 70 expression in M. trossulus. In order to determine if environmental conditions are responsible for the patterns of Hsp 70 expression 1 will need to analyze the data for weeks 4 and 5. The temperature data for these weeks look very similar to the data from weeks 1 and 2. Therefore, if the expression is linked to the environmental conditions, I would expect to see an increase in the levels of Hsp 70 expression. However, if acclimation has occurred it would be more likely that the levels of Hsp 70 expression will remain low during weeks 4 and 5. It is interesting to note the relation of the field data to the subtidal data for both the band 1 and band 2 intensities. At week 2 the field Hsp 70 expression is below the level of subtidal Hsp 70 expression. However, at week 3 the field level of Hsp 70 expression is above the level of Hsp 70 expression for the subtidal group. I am not sure how to explain this pattern. One possibility is that by week 3 the subtidal group has settled in its new environment and is seeing more food then the field mussels. This will be determined by malate dehydrogenase (MDH) quantification. MDH is an enzyme used in the breakdown of food. By quantifying the amount of MDH present in a organism we can understand how much food it was collecting. This amount of food, as well as the MDH quantity, will define the energy budget of the mussels. If the subtidal mussels see higher food levels and thus have higher energy budgets this might also allow these mussels to expend more energy on the production of Hsp 70, This connection might be one way of explaining the pattern of Hsp 70 expression seen in week 3. Future Work Further studies to be done this summer will include analysis of the samples for weeks 4 and 5. I will also complete the analysis of the field data set so that this group can be compared to the two pool treatments. The MDH analysis will also be done so that we can understand the energy budget of the three groups. This summer Iwill also analyze the band intensities based on the size of the mussels in order to determine if there is any difference in Hsp 70 expression between small and large mussels. Conclusion Thus far, results have shown that subtidal vs. intertidal mussels do differ in their expression of Hsp 70 for at least the first three weeks. I am not sure how the field data will correspond to the above two treatments. However it seems that the mean band intensities are usually below the mean band intensities for the subtidal group. Week three is the only exception to this pattern so far and analysis of the samples for weeks 4 and 5, as well as MDH quantification should help to clarify this paradox. Finally, comparison of Hsp 70 expression by body size will give clearer understanding of how mussels deal with heat stress during development. Acknowledgment would like to thank George Somero, Lars Tomanek, Mark Denny and Brian Helmuth for all of their insight and guidance. Without their help none of these results would have been possible. References Craig, E. A. and Gross, C. A. Is Hsp70 the cellular thermometer? Trends in Biochemical Science. 1991; 16:135-140 Dahlhoff, E. P. and Menge, B. A. Influence of phytoplankton concentration and wave exposure on the ecophysiology of Mytilus californianus. Marine Ecology Progress Series. 1996; 144:97-107. Gosling, E. The mussel Mytilus: ecology, physiology, genetics and culture. Developments in Aquaculture and Fisheries Science. 1992. Elsevier Science Publishers, Amsterdam; vol. 25. Hofmann, G. E. and Somero, G. N. 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. 1995; 198:1509-1518. Hofmann, G. E. and Somero, G. N. Protein ubiquitination and stress protein synthesis in Mytilus trossulus occurs during recovery from tidal emersion. Molecular Marine Biology and Biotechnology. 1996; 5(3):175-184. Laemmli, E. K. Cleavage of structural proteins during the assembly of the head of bacteriophage T4. Nature. 1970; 227:680-685. Menge, B. A. et al. Benthic-pelagic links and rocky intertidal communities: Bottom up effects on top-down control? Ecology. 1997; 94:14530- 14535 Roberts, D. A., G. E. Hofmann and G. N. Somero. Heat-shock protein expression in Mytilus californianus: acclimatization (seasonal and tidal-height comparisons) and acclimation effects. Biol. Bull. 1997; 192:309-320. Somero G. The Heat Shock Response. Lecture Notes for Ecological and Evolutionary Physiology. 1998. Welch, W. How cells respond to stress. Scientific American, May 1993, 56-64. Figure Legends Fig. 1 Puffed chromosomes in the salivary glands of a heat stressed Drosophila melanogaster. From Welch et al. Scientific American, May 1993. Fig. 2 The role of molecular chaperones. Fig. 3 Hsp 70 regulation. Adapted from Somero 1998. Fig. 4 This figure shows the mean band 1 intensity of Hsp 70 expression for the intertidal, subtidal, and field groups over the first three weeks. The asterisk denotes statistically significant differences between the intertidal and subtidal treatments. Fig. 5 This figure shows the mean band 2 intensity of Hsp 70 expression for the intertidal, subtidal, and field groups over the first three weeks. The asterisk denotes statistically significant differences between the intertidal and subtidal treatments. Fig. 6 Body temperature data for a small intertidal M. californianus. Note the less extreme temperatures during week three. HEAT-SHOCKED CHROMOSOME Figure 1 COMPLEXING WITH STRESS PROTEINS UNFOLDED PROTEIN CHAIN 898 00 STRESS PROTEINS SELF-ASSEMBLY ASSISTEL SELF-ASSEMBLY FUNCTIONAL NONFUNCTIONAL FOLDED PROTEINS FOLDED PROTEINS PROTEIN FOLDING occurs spontaneously because of thermodynamic constraints imposed by the protein's sequence of hydrophilic and hydrophobic amino acids. Although proteins can fold themselves into biologically functional configurations (self-assembly), errors in folding can occasionally occur. Stress proteins seem to help ensure that cellular proteins fold themselves rapidly and with high fidelity. Weichctal¬ SCIENTIFIC AMERICAN May 1993 Figure 2 Dative Protei Hse70 gene 6 Heat Stas Figure 3 Ven Potein Hp mR 5 gene HSE 5 1.2 1.1 O.9 0.8 0.7 0.6 0.5 0.4 0.3 0 Hsp 70 Band Intensity * 2 Week Figure 4 + Subtidal + Intertidal + Field 4 Control Hsp 70 Band 2 Intensity * R * Week Figure 5 - Subtidal + Intertidal + Field Control O O C O — — — — Q- — 8 8 Sinjeledule 1