Abstract Tityustoxin block of wild-type and mutant SgkV1A channels from Loligo opalesceus neurons was studied in Xenopus oocytes using the two electrode voltage clamp method. The mutant channel was created by replacing a histidine residue at position 351 on the outer vestibule with a glycine. Wild-type channels show greatly reduced sensitivity to tityustoxin block at pH 6. The glycine mutant's sensitivity to tityustoxin was not pH-dependent. Block of both the wild type and mutant channels proved to be voltage dependent. Kp values ranged from 14 nm at 0 my to 70 nm at 100 my for both channels. K rates of H351 channels were not effected by voltage, whereas Ka rates of wild-type channels decreased slightly with voltage. Kg rates increased as voltage increased in both types of channels. Results suggests that a charged residue on the toxin enters the channel pore when tityustoxin blocks these channels, making the toxin sensitive to the membrane voltage. Introduction Tityustoxin is a small peptide of 30 amino acids found in scorpion venom and has been shown to be a potent K“ channel blocker (Werkman et al. 1993). Though much is known about other scorpion toxins, both functionally and structurally, tityustoxin is relatively new and unstudied. Understanding tityustoxin better can help in underständing the structure of the channels they bind to. Scorpion toxins have become important tools in understanding ion channels because they provide a rough map of the channel. Scorpion toxins can bind to channels at 8 or more positions. By knowing exactly which toxin residues bind to which channel residues, and what the structure of the simple toxin peptide is, a general map of a channel can be made. Fixing 8 or more residues in space sets dimensional limits on proposed structures of the channel. A great deal of work on understanding the structure and blocking mechanism of charybdotoxin, another scorpion toxin closely related to tityustoxin, has already been done. The accepted mechanism for charybdotoxin block is that the peptide binds to the outer vestibule of the channel and a lysine at position 27 enters the pore, thus blocking ion flow (Mackinnon and Miller, 1988). It is plausible that tityustoxin blocks by the same mechanism due to similarities in the peptide structure. However, there are structural differences in the proposed binding regions of these two toxins which could lead to different blocking mechanisms. The primary purpose of this paper is to determine whether tityustoxin blocks by the same mechanism as other scorpion toxins or if some other mechanisms needs to be invoked. A secondary goal is to show that a histidine at position 351 of SgkviA channels is necessary for the pH dependence of tityustoxin block of these channels. It has previously been shown that changing the homologous site in Shaker channels (position 425) from wild type phenylalanine to histidine causes the channel to become pH sensitive to charybdotoxin binding. Changing pH from 7-5.5 causes the channel to become 200 fold less sensitive to charybdotoxin (Perez-Cornejo et. al, 1998) It has also been shown by previous spring students, Sky Pittston (1996) and Uma Sanghvi (1997), that tityustoxin block of the wild type SgkviA channels in squid neurons is pH dependent. It was hypothesized that a histidine at position 351 is responsible for this pH dependence because its charge changes over the biological pH range. DEPC treatments were used to chemically alter the histidine residue, but did not conclusively show that histidine is responsible for pH sensitivity to tityustoxin. This paper will show more convincingly that this is in fact true by using a mutant channel in which this histidine is replaced by a glycine. Materials and Methods SgkviA channels containing a G87R mutation where expressed in Xenopus oocytes by cRNA injection as previously described by Rosenthal and Bezanilla(1997). After 2-3 days currents between 5¬ 30 uA could be recorded from wild type channels. Currents from H351G mutants were a little smaller. Currents were recorded by the two electrode whole cell voltage clamp method using p/4 leak subtraction. Only oocytes that had a small leak (under -0.2 uA at - 60 mv holding potential) and stable K“ currents of at least 4-5 uA were used. Electrodes were filled with 3 M KCl, and the external bath solution was either ND-96: 96 mM Nacl, 2 mM KCI, 1 mM MgCl,, 1.8 mM Cacl,, and 5 mM Hepes or a solution containing 90mM Nacl, 10 mM KCI, 2 mM Cacl,, 5 mM MgCl,, 10 mM Hepes at pH 7.15. For the pH-dependence experiments, solutions of 85 mM Nacl, 10 mM KCl, 2 mM Cacl,, 5 mM MgCl,,10 mM MES at pH 6 and 90 mM Nacl, 10 mM KCl, 2 mM Cacl,, 5 mM MgCl,, 10 mM MES at pH 8.2 were used. loxin was diluted in the same solution used in the bath to a concentration of 100, 50, or 10 nM. Solution changes were made by injecting 1.5-2 ml of the new solution into the bath while a vacuum removed the previous solution. Complete solution change could be done in under a minute, and leak generally improved during this period. Currents were recorded during 50 and 500 ms pulses to -40,-20. 0, 20, 40, 60, 80, and 100 my in toxin free-solution. The toxin solution was then washed in, and currents were again recorded for the same duration and voltages. Time constants were obtained by fitting a single exponential to the slow rise of current traces in toxin. The exponential was fit from the time at which the control current reached a maximum to the time at which the current in toxin reached a maximum (Fig. 1). This was done to avoid problems caused by rapid activation of the unblocked current. Results: SqkviA Channels SqkviA is a K“ channels cloned from a CDNA library prepared from the stellate ganglia of Loligo opalescens (Rosenthal et al. 1996). It was previously shown that this channel shares many homologous regions with Shaker B channels including the outer pore region. A point mutation was made to the channel at position 351 by replacing a histidine with a glycine. This position is homologous to position 425 in ShakerB, a proposed binding site for charbdotoxin (Goldstein and Miller, 1992). In all experiments both the wild-type and H351G channels were used. pH-dependence of block by tityustoxin pH-dependence of toxin block was shown by comparing Kt current before and after application of 50 nM tityustoxin at pH 8.2 and pH 6. The effects of toxin on H351G channels showed no detectable pH¬ dependence. At pH 8.2, 51.4% of the current was blocked. Similarly, at pH 6, 57% of the current was blocked. (see figure 2 A,B) However, the wild-type channels did display pH-dependent block by toxin. 57% of the current was blocked at pH 8.2(fig. 2 C), whereas only .05% or less was blocked at pH 6 (fig. 2 D). Similar resusits were obtained in one other experiment. Voltage Dependence of Toxin Binding The Kp of toxin binding was calculated at each voltage using the equation: Ko - ioxinl Toxin/(contro + toxin) Where lg represents the current when no toxin is present after a 500 ms pulse and lgn represents the current in the presence of toxin after a 500ms pulse. The K, of toxin binding increases as voltage increases, as is shown in fig. 3. The increase in K, is similar in both the wild type and H351G channels. Change in Ke and Ke rates The time constant (t) of current increase in the presence of toxin was measured by fitting a single exponential to the curve. Using the 1= 1/(Kltoxin) + Kor) equations, and Ko- KoKon it is possible to solve for Kgg and Kan. It was not possible to fit an exponential to current traces from voltage steps below 40 my for the H351G. Using wild-type channels, exponentials could not be fitted to voltage steps below 60 mv. In H3516 channels, K... increases from .006 at 40 my to .027 at 100 my, whereas K., remains relatively constant (Fig. 4). In wild-type channels, K., decreases slightly from .00023 at 60 my to .00018 at 100 my, and Ky increases from .021 to .029 over the same range(Fig. 5). Discussion It is clear from the results of this study that a histidine at position 351 is necessary and sufficient to confer pH sensitivity to toxin block in SgkviA channels. This is likely due to the fact that at low pH histidine is a positively charged residue, whereas glycine is always neutral. However, it is also possible that steric differences between histidine and glycine could account for the differences in pH-sensitivity. Results obtained in this study also seem to indicate that tityustoxin blocks SgkviA channels by a mechanism similar to that shown by other scorpion toxins, at least in the H351G mutant. Changes in Kp, Kan, and Kay values are consistent with those found using charybdotoxin. Goldstein and Miller graphed the Ky values of charybdotoxin binding to Shaker channels by use of the same log scale that was used in this paper (Goldstein and Miller, 1993). In their data the K, increases by about a factor of .063-.079/my compared to .072/my for tityustoxin acting on SgkvlA channels. However, Goldstein and Miller only showed data from -20 to 20 my. it is not known how the Kp of charybdotoxin changes above 20 mv. Goldstein and Miller also showed that Kg of charybdotoxin increases with voltage by about a factor of .079/my, while Kay remains constant. This is similar to the results found in this study with the H351G mutant. The apparent decrease in Ka, in the wild-type channels is likely due to the small sample size of wild-type experiments; this anomalous result merits further investigation. The similarity between results presented in this paper and those found for charybdotoxin suggest that tityustoxin is binding to SgkviA channels by the same mechanism by which Charybdotoxin binds to Shaker channels. In this model, the peptide binds to the outer vestibule with lysine-27 entering the pore, inhibiting ion flow. At more positive membrane voltages, the voltage drop across the membrane and Kt ions trying to exit the channel force the toxin peptide off the channel. This increases the Kp and Ky values at that voltage. Literature Cited: Goldstein, S.A.N. and Miller, C. 1992. A point mutation in a Shaker Kt channel changes its charybdotoxin binding site from low affinity to high affinity. Biophys. J. 62:5-7. Goldstein, S.A.N. and Miller, C. 1993. Mechanism of charybdotoxin block of a voltage-gated K“ channel. Biophys. J. 65:1613-1619. Mackinnon, R. and Miller, C. 1988. Mechanism of charybdotoxin block of Ca2t activated K“ channels. J. Gen. Physiol. 91:335-349. Rosenthal, J.J.C., and Bezanilla, F. 1997. Evidence for RNA editing in squid giant axon. Am. Zool. 37:1 90a. Rosenthal, J.J.C, Vickery, R.G., and Gilly, W.F. 1996. A candidate for a delayed Rectifier K“ channel in squid giant axon. J. of Gen. Phy. 108(3): 207-219. Perez-Cornejo, P., Stampe, P, and Begenisich, T. 1998. Proton probing of the charybdotoxin binding site of Shaker K“ channels. J. Gen. Physiol. 111:441-450. Pittston, S. 1996. Unpublished results. Hopkins Marine Station spring student. Sanghvi, Uma. 1997. Unpublished results. Hopkins Marine Station spring student. Werkman, T.R., Gastason, T.A., Rogowski, R.S., Blanstein, M.P., and Rogawski, M.A. 1993. Tityustoxin -K-Alpha, a structurally novel and highly potent K“ channel peptide toxin, interacts with the alpha-denrotoxin binding site on the cloned Kv1.2K“ channel. Mol. Pharm. 44(2): 430-436. Fig. 1- Upper trace is Kt current before tityustoxin aplication. Lower trace is K“ current in the presence of tityustoxin. The current in toxin reaches a maximum much more slowly. A single exponential was fitted to this slow rise between the arrows. 10 nm P15A tityustoxin was used. Fig. 2- (A) H351G at pH 8.2. The top trace is the control current, the bottom trace is the current in the presence of tityustoxin. (B) H3516 at pH 6. The amount of current blocked by tityustoxin is similar to (A). (C) Wild type channels at pH 8. In the presence of toxin, current reduction is similar to H351G channels. (D) Wild type at pH 6. Almost no current is blocked by tityustoxin. In all cases 50 nM tityustoxin was used. The H351G traces are from a 500 ms voltage step to +40 mv. The wild type traces are from a 500 ms step to +30 mv. Fig. 3- Wild-type Ky values are the average of three experiments. H351G Kp values are the average of 5 experiments. Kp's are graphed as the log of the ratio of the K, at each voltage divided by the K, at 0 mv. The Kp of toxin binding increases with voltage in both wild type and H351G channels. Fig. 4- Average of five Ka, and Kgy rates of tityustoxin acting on H3516 channels. Ka and Kgy are graphed as the log of the ratio of Kopof at each voltage divided by Kepr at 40 mv. Fig. 5- Average of two Ka and Kgn rates of tityustoxin acting on wild-type channels. Ko and Kgr are graphed as the log of the ratio of Konof at each voltage divided by Kpof at 60 mv. Fig.1- Current traces with and without tityustoxin present 15 uA 150 ms aaataaa- A H3516 -60 mV Wild-type Fig.2- pH dependence of toxin block PH 6.0 pH8.2 B aenen eneit — 5 UA m t 200 ms —+40- senennan 5 UA -40 Fig. 3- Wild-type and H351G Kd values 0.8 0.6 0.4 - 0.2 - -20 20 40 60 80 100 -0.4 - Voltage (my) —°— Wild type —H3516 0.7 0.6 0.5 0.4 0.3 § 02 0.1 40 -0.1 50 Fig. 4- Kon and Koff of H3516 60 70 80 Voltage (my) 90 100 —Koff — Kon 0.15 - 0.1 0.05 O 2 60 5 -0.05 -0.1 -0.15 - -0.2 Fig. 5-Wild-type Kon and Koff values 90 70 80 Voltage (my) 100 — 2 — Koff 4 Kon