Identification and Induction of Heat Shock Proteins in Tigriopus californicus Theresa A. McEvoy June 3, 1993 Dr. R. P. Levine Stanford University Biology 175H ABSTRACT Using immunoblotting and enhanced chemiluminescence techniques, heat shock proteins of molecular weight 60 KD and 70KD were identified constitutively in Tigriopus californicus under control conditions of 19 degrees Celsius. Hsp 60 was induced during separate experiments under conditions of increased temperature and increased salinity concentrations. Western analysis could not definitively identify induction of hsp 70 during heat shock or salinity shock. This study serves as the basis for further study of heat shock proteins in marine organisms. Introduction All organisms possess mechanisms enabling them to endure or adapt to the common stresses of their environments. In the marine environment, common stresses may include variable temperatures, introduction of pollutants, or changes in pH. There are a variety of ways organisms may cope with stress. At the cellular level, one of the most important reactions to stress may be the increased synthesis of additional proteins commonly referred to as heat shock proteins or hspsé. The increased production of these groups of proteins in response to stress is commonly referred to as the heat shock response5. In addition to playing a vital role in normal cell activities, hsps protect the cells from the damaging effects of extreme temperature changes or other environmental stress4 . Heat shock proteins are among the most highly conserved genetic system known, indicating that they may play an important biological role in the adaptation and evolution of organisms5. Although heat shock response has been studied in fruit flies, yeast, chickens, mammals and bacteria, it has not been rigorously evaluated in marine organisms, many of which live in highly variable habitats associated with the periodicity of the tides. Tigriopus californicus is a marine copepod that thrives in the high splash pools associated with rocky coastlines. This hearty crustacean ranges from the coast of Glacier Bay, Alaska, south to Baja California2. This study identifies two groups of heat shock proteins in Tigriopus and attempts to observe increased production of the hsps in response to changes in temperature and salinity simulating harsher environmental conditions. Tigriopus californicus was chosen as the test organism for this nine week project because it is relatively abundant in the tide pools near Hopkins Marine Station and is easily maintained in the lab at room temperature. Materials and Methods Collecting Tigriopus californicus. Copepods were collected through a small collecting strainer from two high splash pools near Hopkins Marine Station in Monterey Bay, California. They were maintained in filtered sea water at room temperature and fed ground mussel approximately every twenty four hours. Obtaining protein. Protein samples were obtained by homogenization of Tigriopus californicus in homogenization buffer containing 10 ml PBS in 10 mM EDTA, 50uI PMSF, 10ul pepstatin, 1Oul leupeptin, 100ul chymostatin and 50ul ofNP-40 (.5%). Following centrifugation, supernatant from the sample was boiled for three minutes and protein content was determined using Coomassie stain reagent.' SDS PAGE. Solubilized protein from the sample was separated according to molecular weight by electrophoresis on a 10% SDS acrylamide gel. Prestained molecular weight standards were obtained from Sigma Chemical Corporation (St. Louis, MO.). The hsp 60kD standard was obtained from mouse protein and made available to the lab by Ildiko Kovacs at Hopkins Marine Station. The hsp 70KD bovine brain stress protein standard was supplied by StressGen Biotechnologies Corporation (Victoria, B.C.). Western Blotting. The western blotting procedure was carried out according to the protocol described by Harlow and Lanes. The primary heat shock monoclonal anti-body used for detecting heat shock proteins of the 60kD family was obtained from StressGen Biotechnologies Corp. Anti-hsp70 monoclonal antibody 3A3 was made available to the lab by Shawn Murphy at Northwestern University. The anti-GOKD antibody was diluted 1:1000. All other anti-bodies, including the secondary antibodies, were diluted 1:10000. Secondary anti-rabbit lgG peroxidase conjugate and anti¬ mouse lgG peroxidase conjugate were supplied by Sigma Immuno Chemicals. Enhanced Chemiluminescence (ECL). Films of the nitrocellulose membrane were developed in the dark room using Kodak film according to the protocol for ECL immunodetection supplied by Amersham International (Buckinghamshire, England). Heat and Salinity Shock Experiments. Protein samples used to detect induced hsps after exposure to heat shock were obtained from individuals acclimated to 19 degree sea water for twenty-four hours and then transferred to 32 degree Celsius sea water for a period of four hours. Similarly, copepods were acclimated at 50% artificial sea water for twenty-four hours and transferred to 100% or 200% artificial sea water to test for salinity shock. All salinity shock experiments were conducted at 19 degrees Celsius. Results Heat shock proteins with molecular weights 60 KD and 70 KD were present in Tigriopus californicus under control conditions at 19 degrees and 100% salinity as shown in figures 1 and 2 respectively. Each figure is a developed film of the nitrocellulose membrane after enhanced chemiluminescence following Western blotting. In figure 1, the mouse standard containing hsp 60 is illuminated in lane 4, and protein obtained from Tigriopus californicus is in lanes 1 through 3. Lanes1, 2, and 3 contain 12.6 ug, 25.2 ug, and 50.2 ug of protein, respectively. The dark bands directly across from the dark band of the standard indicate the presence of hsp 60 in the protein sample. Two bands of protein are visible in lane 1 in which the most protein was loaded. Figure 2 contains a bovine brain standard of hsp 70 in the far right lane. Protein extracted from Tigriopus californicus is present in lanes 1 through 3. Again, the dark bands across from the standard indicate the existence of hsp 70 in the protein sample obtained from Tigriopus californicus under control conditions. A slightly higher molecular weight protein also reacted with the anti-hsp70 antibody as displayed by the three lighter marks directly above the dark bands. The results of exposing Tigriopus californicus to 30 degrees Celsius is shown by the five minute exposure film in figure 3. Here, the standard was loaded in lane 5 and increasing amounts of protein extracted from Tigriopus under the control condition of 19 degrees Celsius were run in lanes 1,2, 3 and 4. Lanes 6 through 10 contain increasing amounts of protein from copepods acclimated for twenty-four hours at 19 degrees and then transferred to 30 degrees Celsius for 3 hours. Equal amounts of protein are loaded in lanes 1 and 6, lanes 2 and 7, lanes 3 and 8, and lanes 4 and 9. The presence of induced hsp 60 is indicated by the multiple bands visible in the sample lanes 6 through 10 as compared to the corresponding control lanes 1 through 4 containing equal protein. Exposing Tigriopus californicus to salinities of 100% and 200% for four hours after 24-hour acclimation at 50% instant ocean induced production of hsp 60 (figure 4) but did not induce production of hsp 70 (figure 5). In each figure, lane 2 is the control, containing protein obtained from animals acclimated at 50% instant ocean and lanes 3 and 4 contain protein of Tigriopus californicus exposed to the increased salinity concentrations of 100% and 200%, respectively. Figure 4 displays an overloaded gel which nonetheless shows multiple bands in the sample lanes 2 (50%), 3 (100%), and 4 (200%) as compared to the standard loaded in lane 1. Although the copepods were acclimated at 50% artificial sea water, multiple bands are present in lane 2, perhaps indicating that they had not yet adapted to the change. Figure 5 shows only single bands in the three samples loaded in lanes 2, 3, and 4, from which definitive results cannot be discussed. Conclusions Heat shock proteins of the 60kD and 70kD molecular weight families were identified in samples of protein from Tigriopus californicus under optimal conditions of 19 degrees Celsius and 100% sea water. These constitutive proteins may enable the organisms to endure normal ranges of stress introduced by small changes in their habitat. Identification of these proteins verifies that cross reaction with the anti-hsp antibodies has occured. Inducible forms of hsp 60 found under both heat shock and salinity shock may enhance the survival rate of Tigriopus californicus for several hours or longer during an increase in temperature of 13 degrees Celsius and increased salinity This concentrations of up to four times the original concentration. production of proteins enabling survival under harsh conditions is an important component of this species' ability to live in the high splash pools. This study is only an initial investigation of heat shock proteins in marine organisms and provides the basis for correlating successful survival of organisms with heat shock protein synthesis and activity. Literature Cited 1. Bradford, M., 1976. Anal. Biochem. 72:248-254. 2. Haderlie, C., D. Abbott, and R. Caldwell. 1980. Intertidal Invertebrates of California. Stanford University Press. Stanford, CA. pp. 632-635. 3. Harlow, E. and D. Lane. 1988. Antibodies, A Laboratory Manual. Cold Spring Harbor Laboratory. pp. 474-506. 4. Langer, T., and L. Neupert. 1991. Heat Shock Proteins hsp60 and hsp70: Their Roles in Folding, Assembly and Membrane Translocation of Proteins. Current Topics in Microbiology and Immunology. 167: 3-24. 5. Lindquist, S., and E.A. Craig. 1988. The Heat Shock Proteins: Annual Review of Genetics. 2: 631-666. 6. Morimoto, Tissieres, Georgopoulos (ed.). 1990. Stress Proteins in Biology and Medicine. Cold Spring Harbor Laboratory Press pp. 1- 20. Figure Legends Figure 1. Film developed for one minute after enhanced chemiluminescence following standard western blot procedure showing identification of hsp 60 family in T. californicus acclimated at 19 degrees and 100% sea water. A 10ul sample of mouse standard is loaded in the far right lane (lane 4) and increasing amounts of sample protein are loaded in lanes 1 through 3, respectively. A prestained molecular weight sample was loaded in lane 5, not shown in the figure. Figure 2. Film developed for five minutes after western blotting and enhanced chemiluminescence using anti-hsp 70 antibody 3A3. Sample protein from organisms acclimated at 19 degrees was loaded in lanes 1 through 3 and 10ul of hsp 70 standard extracted from bovine brain (StressGen Technologies Corp.) was loaded in lane 4 Figure 3. Film developed after enhanced chemiluminescence of protein obtained from T. californicus under control conditions and under heat shock conditions of 30 degrees Celsius. Control protein is loaded in increasing amounts in lanes 1 through 4. Heat shocked protein is loaded in lanes 6 through 10, and the hsp60 standard is located in lane 5. Equal amounts of protein are loaded in lanes 1 and 6, lanes 2 and 7, lanes 3 and 8, and lanes 4 and 9. Figure 4. Film developed after western blotting and enhanced chemiluminescence of protein extracted from T. californicus acclimated at 50% artificial sea water (lane 2), and transferred to 100% and 200% artificial sea water (lanes 3 and 4 respectively). Hsp 60 standard is located in lane 1. Figure 5. Results of the salinity shock experiment probing for hsp70. Lane 1 contains the hsp70 standard. Lanes 2 contains the control condition of acclimation at 50% artificial sea water. Lanes 3 and 4 contain protein extracted from copepods transferred to 100% and 200% artificial sea water. Figure 1. 84kI 58kl Figure 2. Figure 3. Figure 4. 3 Figure 5. Acknowledgements wish to extend thanks to Dr. R. P. Levine for his immense enthusiasm and dedicated interest in this project. I would also like to thank Julie Golden for her incredible patience in teaching me the necessary technical skills of gel electrophoresis and western blotting. Additional thanks are extended to everyone who worked in Dr. Levine's lab for sharing precious lab space with me and providing an enjoyable work environment! And finally, greatful thanks are offered to the entire staff at Hopkins Marine Station and the other students participating in the spring program, for their help and encouragement.