3281 INTRODUCTION Most of our knowledge concerning the adaptation of proteins to varied thermal habitats comes from research on enzymes (Hochachka and Somero, 2002). According to the corresponding states theory, differences in the thermal sensitivity of Michaelis–Menten constants (K m ) of orthologous enzymes from poikilotherms adapted to different thermal regimes are driven by subtle changes in protein primary structure, which in turn lead to changes in conformational flexibility (Somero, 1978; Somero, 1983). These changes in conformational flexibility offset the function-altering effects of a change in temperature, thus conserving optimal function at physiological temperature. In thermodynamic terms, at lower temperatures less heat/energy is available to drive physiochemical reactions. Cold-adapted orthologs respond with a smaller net enthalpy change and a larger change in entropy than warm/temperate-adapted orthologs, which compensates for the reduced temperature/kinetic energy. This leads to a similar change in free energy and conserved binding ability at physiological temperatures (Somero, 1978; Somero, 1983; Somero, 1995; Jaenicke, 2000; Hochachka and Somero, 2002). Over evolutionary time scales, thermal compensation is accomplished through adjustments in protein primary structure. It appears that these compensating amino acid substitutions are generally excluded from the active site residues, which tend to be conserved to maintain substrate specificity (Wilks et al., 1988; Golding and Dean, 1998; Fields, 2001). In prior work, the model derived from enzyme systems was extended to the non-catalytic Ca 2+ -binding protein parvalbumin (Erickson et al., 2005; Erickson and Moerland, 2006). Parvalbumins (PVs) are small (~10–12 kDa), acidic (pI ~3–5) proteins that are unique to vertebrates and are present at high levels in the cytosol of fast-twitch skeletal muscle (Rall, 1996). The consensus view of PV function is that it acts as a soluble Ca 2+ buffer in fast-twitch muscle cells. By allowing faster unloading of troponin C, the presence of PV leads to faster contraction/relaxation cycles (Rall, 1996). Isoforms of PV purified from white muscle of cold-adapted Antarctic fish of the Perciformes sub-order Notothenioidei and from temperate counterparts displayed thermal sensitivity patterns similar to those of enzymes of species adapted to different temperatures. Specifically, at a common measurement temperature Antarctic fish PVs showed a weaker binding affinity, as evidenced by a higher Ca 2+ dissociation constant (K d ), than temperate counterparts, but at physiological temperatures function was highly conserved (Erickson et al., 2005; Erickson and Moerland, 2006). A specific structural mechanism leading to the thermal sensitivity pattern found in Antarctic fish PVs, however, has yet to be elucidated. SUMMARY Parvalbumins (PVs) from Antarctic notothenioid fishes display a pattern of thermal adaptation that likely reflects evolutionary changes in protein conformational flexibility. We have used ancestral sequence reconstruction and homology modeling to identify two amino acid changes that could potentially account for the present thermal sensitivity pattern of Antarctic fish PVs compared with a PV from a theoretical warm-adapted ancestral fish. To test this hypothesis, ancient PVs were resurrected in the lab using PV from the notothenioid Gobionotothen gibberifrons as a platform for introducing mutations comparable to the reconstructed ancestral PV sequences. The wild-type PV (WT) as well as three mutant expression constructs were engineered: lysine 8 to asparagine (K8N), lysine 26 to asparagine (K26N) and a double mutant (DM). Calcium equilibrium dissociation constants (K d ) versus temperature curves for all mutants were right-shifted, as predicted, relative to that of WT PV. The K d values for the K8N and K26N single mutants were virtually identical at all temperatures and showed an intermediate level of thermal sensitivity. The DM construct displayed a full conversion of thermal sensitivity pattern to that of a PV from a warm/temperate-adapted fish. Additionally, the K d versus temperature curve for the WT construct revealed greater thermal sensitivity compared with the mutant constructs. Measurements of the rates of Ca 2+ dissociation (k off ) showed that all mutants generally had slower k off values than WT at all temperatures. Calculated rates of Ca 2+ binding (k on ) for the K8N and K26N mutants were similar to values for the WT PV at all temperatures. In contrast, the calculated k on values for the DM PV were faster, providing mechanistic insights into the nature of potentially adaptive changes in Ca 2+ binding in this PV. The overall results suggest that the current thermal phenotype of Antarctic PVs can be recapitulated by just two amino acid substitutions. Supplementary material available online at http://jeb.biologists.org/cgi/content/full/215/18/3281/DC1 Key words: ancestral sequence reconstruction, EF-hand, environmental adaptation, Notothenioidei, protein structure/function, Southern Ocean. Received 25 January 2012; Accepted 23 May 2012 The Journal of Experimental Biology 215, 3281-3292 © 2012. Published by The Company of Biologists Ltd doi:10.1242/jeb.070615 RESEARCH ARTICLE Resurrecting prehistoric parvalbumins to explore the evolution of thermal compensation in extant Antarctic fish parvalbumins A. Carl Whittington 1, * and Timothy S. Moerland 2 1 Department of Biological Science, Florida State University, Tallahassee, FL 32306, USA and 2 Department of Biological Sciences, Kent State University, Kent, OH 44242, USA *Author for correspondence (awhittington@chem.fsu.edu) THE฀JOURNAL฀OF฀EXPERIMENTAL฀BIOLOGY