Is tyrosine kinase activity necessary for fertilization-induced glucose-6¬ phosphate dehydrogenase release in Strongylocentrotus purpuratus eggs? Geetika Agrawala Hopkins Marine Station Stanford University Abstract The activity of the pentose phosphate shunt increases soon after fertilization of Strongylocentrotus purpuratus eggs, and this increase is correlated with a change in the intracellular distribution of glucose-6-phosphate dehydrogenase (G6PD), the first and rate-limiting enzyme in the pentose shunt. This enzyme is found in a bound, inactive state in unfertilized eggs and in a soluble, active state in newly fertilized zygotes. The signaling pathway that links fertilization to the release of G6PD from the bound state is not known. In this study, I have investigated whether tyrosine kinase activity is involved in fertilization-induced G6PD release in sea urchin eggs. I determined that G6PD release does not occur in unfertilized eggs treated with bindin or antibody against the sperm receptor. These two treatments activate the specific tyrosine kinase that phosphorylates the sperm receptor. I also found that inhibition of general tyrosine kinase activity using the tyrosine kinase inhibitors genistein and tyrphostin 51 does not block G6PD release in sea urchin zygotes. As deduced by immunoprecipitation of phosphotyrosines, genistein is inhibiting tyrosine kinase activity while tyrphostin 51 is not. These preliminary data show that those tyrosine kinases which are inhibited by genistein are not involved with G6PD release after fertilization. I also discuss the possible reasons why tyrphostin 51, bindin, and anti-receptor antibody treatment may have given inconclusive data. Introduction The study of fertilization in sea urchin eggs has brought about many insights into the mechanisms cells can use to change from a dormant state to an active one (Epel, 1990). Currently we know much about the primary events of signal transduction at fertilization, however we do not know as much about what happens downstream. The pentose phosphate shunt is an alternative pathway to glycolysis. Through this pathway, glucose is turned into various biosynthetic products necessary for cell growth and division including NADPH which is necessary for DNA synthesis. Swezey and Epel (1995) showed that the shunt is activated shortly after fertilization, however the mechanism of this activation remains unclear. The first and rate-limiting enzyme in the pentose shunt is glucose-6-phosphate dehydrogenase (G6PD). Activity of this enzyme is a good indicator of activity of the entire pentose shunt pathway. G6PD is in an inactive form bound to particulate matter in the egg before fertilization and in an active, free, soluble form after fertilization (Swezey and Epel, 1986). While release of G6PD at fertilization does not seem to involve any covalent changes of the enzyme itself (Swezey and Epel, 1986), its release may be an important part of egg activation after fertilization. Another example of cell activation leading to an increase in shunt activity is growth factor stimulation of mammalian rat kidney cells (Stanton and Seifter, 1988). Interestingly, in these cells G6PD is in a bound form prior to stimulation by treatment with growth factors, and treatment causes the rapid release of G6PD (Stanton et al., 1991). Recently, Tian et al. (1994) discovered that cells transfected with platelet-derived growth factor receptor (PDGFR) mutants that were tyrosine kinase deficient would not release G6PD in response to platelet-derived growth factor (PDGF), the stimulating ligand of the receptor. Thus, in these cells G6PD release seems to require the activation of cellular tyrosine kinases. While tyrosine kinase activity is necessary for G6PD release in somatic mammalian cells, the correlation has not yet been made in sea urchin eggs at fertilization. It is known, however, that in sea urchin eggs two- to fourfold increases in tyrosine kinase activity (Satoh and Garbers, 1985) and the production of newly tyrosine- phosphorylated proteins (Ciapa and Epel, 1991) occur minutes after fertilization. One protein that is found to be tyrosine-phosphorylated soon after fertilization is the 350 kDa sperm receptor (Abassi and Foltz, 1994). This protein becomes phosphorylated in response to sperm as well as bindin, the purified ligand of the receptor (Abassi and Foltz, 1994). Hence, there must be activation of at least one tyrosine kinase by the sperm receptor binding its ligand. Bindin is the species-specific protein isolated from sperm that helps sperm to attach to eggs during fertilization (Lopez et al., 1993). Therefore, if the signal for G6PD release is downstream of the activation of this tyrosine kinase, treatment with bindin would be a direct and simple way to test whether GéPD release involves tyrosine kinase activity. Along with bindin, antibodies against the sperm receptor have been shown to prevent fertilization (Foltz et al., 1993). Assuming this means that the antibodies are binding to the receptor, they may also be causing tyrosine phosphorylation of the receptor. If this is true, then anti-receptor antibody treatment would also be a simple way to determine if G6PD release requires the activation of this particular tyrosine kinase. In an effort to determine the general role of tyrosine kinases in the activation of the egg after fertilization, Moore and Kinsey (1995) have studied the effects of tyrosine kinase inhibitors including genistein and tyrphostin B42 on sea urchin eggs. Genistein, a flavinoid, competitively inhibits tyrosine kinases at their ATP-binding sites (see reference in Edgecombe et al., 1991), and the family of tyrphostins competitively inhibit tyrosine kinases at their substrate binding sites (Moore and Kinsey, 1995). While genistein and tyrphostin B42 inhibit overall fertilization-dependent tyrosine kinase activity, they do not prevent the early events of fertilization including elevation of the fertilization membrane; however, they do inhibit later events including DNA synthesis, cell division, and pronuclear migration (Moore and Kinsey, 1995). While these effects are known, the effects of general tyrosine kinase inhibition on fertilization-induced G6PD release by genistein and tyrphostin are not known. The purpose of this study is to determine whether a tyrosine kinase is involved in the increased activity of the pentose shunt at fertilization of sea urchin eggs by addressing the following questions. (1) Is activity of the specific tyrosine kinase that phosphorylates the sperm receptor at fertilization involved with G6PD release? (2) Does inhibition of general tyrosine kinase activity block fertilization-induced G6PD release? Materials and Methods Handling of Gametes Tinduced the spawning of Strongylocentrotus purpuratus by injecting 1-2 ml of 0.5 MKCl into the coelomic cavity, and collected eggs by placing the females with their oral sides up onto beakers filled with sea water such that their eggs shed directly into the sea water. Egg jelly was removed by passing the egg suspension 5-6x through an 80 um mesh and washing 2-3x with filtered sea water (FSW). To ascertain that this method actually removed egg jelly, I examined the dejellied eggs with colloidal ink and toluidine blue stain. The eggs were then resuspended to a 1% suspension, which I determined using a Bauer-Schenk graduated centrifuge tube, and kept at 16°C. I collected undiluted sperm by pipetting them directly from the surface of the urchin. Undiluted sperm were stored at 4°C. Typically, the eggs were fertilized by diluting dry sperm 1:100 in FSW and then again 1:100 into the egg suspension for a total dilution of 1:10,000. G6PD Assay The amount of G6PD bound to the particulate fraction was determined as described by Swezey and Epel (1986). I hand centrifuged 1 ml of egg or zygote suspension, resuspended it to 1 ml in ice-cold 50 mM 2-(N-morpholino)ethane sulfonic acid (pH 6.5 at 4°0), 6 mM EGTA, and 20 mM KC, and homogenized it using an average of 12-20 strokes of a tight-fitting dounce homogenizer. Homogenate was then spun for 5 minutes in an Eppendorf centrifuge (-12,000 g), and the supernatant (S1) was removed and stored at 4°C. I resuspended the pellet in ice-cold 20 mM Tris (pH 8.0 at 4°C) containing 0.1 MKCI (KC buffer) with a volume equaling S1. The high ionic strength of the KCl buffer caused the G6PD bound to the particulate fraction to become soluble. The suspension was then spun again for 5 minutes in an Eppendorf centrifuge (-12,000 g) and the supernatant (S2) was removed and stored at 4°C. 1determined the G6PD activity of S1 and S2 with a spectrophotometric assay. The assay contained 35 mM Tris-HCl (pH 8.5), 7 mM MgCl2, 1 mM G6P, 0.4 mM NADP, and 20-50 ul of sample in a total volume of 2 ml. G6PD activity was measured as the rate of increase in absorbance at 340 nm due to the production of NADPH. One unit of G6PD is defined as the amount necessary to catalyze the conversion of 1 umol NADP to NADPH per minute at 20°C. S1 contained G6PD that was unbound in the egg cells, and S2 contained G6PD that was released from the particulate fraction. The total amount of G6PD in the homogenate was the sum of the two, and the percentage of bound G6PD was equal to the percent of the total activity (activity in S1 + activity in S2) contained in S2. I assayed each Sl and S2 twice, and calculated percentages using mean values. 1took all fertilized samples 4-5 minutes after fertilization. NADPH Assay The amount of NADPH produced by the egg in vivo was studied as described by Epel (1964). 1 put 3 ml of 1% egg suspension into a cuvette and measured NADPH production by monitoring light emission at 460 nm when the cell suspension was excited at 365 nm. The cells were maintained in suspension with a stirrer, and the eggs were kept at 20°C throughout measurements. I added 1 ul of undiluted sperm to the egg suspension while it was in the fluorimeter to asses NADPH changes due to fertilization. Bindin A purified S. purpuratus bindin sample was obtained from K. Foltz at UCB. The bindin sample was kept at -80°C until needed. Prior to use, I thawed the sample at 4°C for three days, and then spun it for 30 minutes at 10,000 rpm (12,000 g) in an SS34 rotor at 4°C. The supernatant contained the soluble bindin whose concentration was determined using the Bicinchoninic Acid (BCA) assay. (Smith et al., 1985). Based upon those protein concentrations, I incubated unfertilized eggs in 0.06-60.0 ng/ ml of soluble bindin. Ttook samples for the G6PD assay 4-5 minutes after treatment with bindin. Antibodies Against the Sperm Receptor Purified anti-receptor antibodies were also obtained from K. Foltz. The anti-exo antibody was made to the extracellular region of the receptor, and the anti-cyto antibody was made to the cytoplasmic region of the receptor. I used the anti-exo antibody as the experimental primary antibody at a concentration of 6 ug/ml, and for the controls lused goat immunoglobulins (Sigma) or anti-cyto antibodies as primary antibodies, also at 6 ug/ml. Unfertilized eggs were incubated with primary antibody on an orbit shaker for 30 to 60 minutes at 16°C, then washed twice with FSW. Goat anti¬ rabbit IgG conjugated to the fluorescein derivative DTAF at a 1:62 dilution or anti-rabbit IgG conjugated to the rhodamine-based dye TRITC (Sigma) at a 1:200 dilution were used as secondary antibodies. I incubated the eggs in secondary antibody for 30 minutes on an orbit shaker at 16°C, then washed them once with FSW and took samples. Tyrosine Kinase Inhibitors 1made up 100 mM stock solutions of genistein (ICN) and tyrphostin 51 (Sigma) in DMSO. Ttreated unfertilized eggs with 100 uM genistein or 100 uM tyrphostin 51 for up to 90 minutes before fertilization (see Results for incubation times for each experiment). Controls were treated with 0.1% DMSO for equal amounts of time. Samples of treated unfertilized eggs were taken 15 minutes before fertilization, and the zygote samples were taken 4-5 minutes post-fertilization of the remaining eggs. Immunoprecipitation Immunoprecipitation was done using a protocol modified from Ciapa and Epel (1991). I concentrated 40 ml samples of 1% suspension to 5% and treated them with 5 mM aminotriazol (ATA). ATA weakens the fertilization envelopes (FEs) and thus helps the extraction buffer lyse the eggs. Äfter 5 minutes I fertilized the samples with a 1:2000 dilution of sperm. Thirty seconds after adding sperm, I checked the eggs under a microscope for FE elevation. Thirty seconds later the zygote suspensions were passed 8x through an 80 um mesh, washed with 10 ml FSW, and twice with 10 ml 1 M glycine, 1mMEGTA, pH 8.0 adjusted with 1 MTris. I then resuspended the final pellet with 3.6 ml (10% suspension) of extraction buffer, made of 50 mM HEPES (pH 7.4), 150 mM Nac, 10% glycerol, 10 mM EDTA, 1 mM MgC2, 1% Nonidet-P 40, including 2 mM sodium vanadate (ortho), 10 mM Na4P2O7, 10 mM NaF, 10 ug/ ml aprotinin, 10 ug/ml leupeptin, 10 ug/ml pepstatin, 50 ug/ml soy bean trypsin inhibitor, and 1 mM phenylmethylsulfonyl fluoride. This suspension was rotated at 4°C for 30 minutes. I spun the extracts for 10 minutes at 10,000g in an SS34 rotor at 4°C. One ml samples of supernatant were incubated with 5 ug/ml of the anti-phosphotyrosine antibody, PY-20 (ICN) for 4 hours, rotating, at 4°C. I also incubated two controls, one using 5 ug/ ml of non-specific mouse IgGpp (Sigma) with lysate, and the other using PY-20 with no lysate, T added 100 ul of a 1:1 dilution of agarose bead-conjugated anti-mouse IgG antibody (Sigma) in extraction buffer, and incubated the samples for 1 hour, rotating, at 4°C. The samples were then washed twice with 1 ml extraction buffer, once with 1 ml 0.5 M LiC. 0.1 MTris (pH7.4), and once with 1 ml 10 mM Tris (pH 8.0), 100 mM NaCl, 1 mM EDTA. Agarose beads were collected by centrifugation for 5 minutes in the Eppendorf centrifuge between each wash. I resuspended the final pellets in 80 ul each of electrophoresis sample buffer made of 2% SDS, 60 mM Tris (pH 6.8), 10% glycerol, 100 mM DTT, and a few grains of bromphenol blue, and placed them in an 80-85°C water bath for 10 minutes. The samples were cooled to room temperature and spun for 5 minutes in the Eppendorf centrifuge. The supernatants were removed to new tubes and frozen at -35° Tran these samples on a 10% SDS polyacrylamide gel (Laemmli, 1970), and the phosphotyrosines were revealed using a Western immunoblot (Towbin et al., 1979). The blot was blocked for an hour in 20 mM Tris (pH 7.6), 138 mM NaCl, 0.1% Tween-20, 3% BSA. Tused PY-20 as the primary antibody in a 1:2000 dilution, incubating for 1 hour, and goat anti-mouse IgG(H+L) HRPO (Southern Biotechnology Associates, Inc.) as the secondary antibody in a 1:2000 dilution, incubating for 1 hour. Before and after each antibody incubation, I washed the blots 4x 5 minutes with 20 mls of saline solution made of 20 mM Tris (pH 7.6), 0.8% Nacl, 0.1% Tween. The blot was developed using the chemiluminescence assay described by Thorpe et al., (1985). Results Effect of Bindin and the Antibody Against the Sperm Receptor on G6PD Release Tused two different approaches to determine whether the specific tyrosine kinase that phosphorylates the sperm receptor after fertilization is involved in G6PD release. The first was by treating unfertilized eggs with two concentrations of bindin: 60 pg/ml. (used by Abassi and Foltz (1994) to stimulate tyrosine phosphorylation of the sperm receptor); or 60 ng/ml (1000x as concentrated). Both concentrations of soluble bindin had little or no effect on G6PD release (Table 1). These eggs fertilized normally, (FE elevation of close to 100% of the eggs, as in controls) indicating that bindin was not preventing access of sperm to its receptor. While the BCA protein assay is generally accurate, there may have been some contaminants which gave an inordinately high concentration of soluble bindin. In this case, the amount of bindin I used may not have been enough to stimulate the egg. The second approach was to treat eggs with anti-receptor antibody. This treatment also seems to have no effect on G6PD release (Table 1). The secondary antibodies used in these experiments were conjugated to fluorescent dyes, and because the eggs did not fluoresce after treatment, it seemed that the primary antibodies were not binding to the cell surface. The eggs fertilized normally, again indicating that the receptor remained accessible to sperm. The high ionic strength of sea water may have been causing a disruption between the antibody-antigen interaction, yielding these results. Effect of Tyrosine Kinase Inhibitors on G6PD Release The method l used to learn if general tyrosine kinase activity is involved in causing the G6PD release after fertilization was to treat eggs with the tyrosine kinase inhibitors genistein and tyrphostin 51. Incubation of unfertilized eggs with 100 uM genistein for 1 hour pre-fertilization does not block fertilization-induced G6PD release (Figure 1) as 1 determined using the G6PD assay. This concentration of genistein was used because Moore and Kinsey (1995) have shown that at concentrations between 37 uM and 150 uM genistein effectively blocks tyrosine kinase activity without disrupting serine and threonine kinase activity. Fertilization of genistein-treated eggs occurs normally as evidenced by FE elevation 1-2 minutes after adding sperm, however development is arrested. Four hours after fertilization, division of genistein-treated zygotes to the 2-cell stage had not occurred. Similarly, incubation of unfertilized eggs with 100 uM tyrphostin 51 for 90 minutes pre-fertilization does not seem to have an effect on G6PD release (Figure 2). Again, Moore and Kinsey (1995) showed that this concentration would adequately block tyrosine kinase activity in sea urchin eggs. Fertilization of tyrphostin 51-treated eggs occurs normally. However, zygotes in this group appear to develop normally as well. Both control and tyrphostin-treated zygotes divided to the 2-cell stage by 4 hours post-fertilization. To ensure that genistein and tyrphostin 51 were actually inhibiting tyrosine phosphorylation, Iimmunoprecipitated zygotes after pre-treatment with genistein and tyrphostin with the anti-phosphotyrosine antibody, PY-20. I incubated a 1% suspension of eggs in 0.1% DMSO (controls) or in 100 uM inhibitor for 90 minutes, and then fertilized them and took samples. As expected, the resulting Western immunoblot shows that the unfertilized control (lane 1) does not show many bands in the 65-98 kDa region, indicating that tyrosine kinase activity is low. Also as expected, the fertilized 10 control (lane 4) shows several bands in this region, indicating that phosphorylation of tyrosine residues (tyrosine kinase activity) has increased after fertilization. The genistein-treated sample (lane 2), does not show these bands, verifying that genistein is inhibiting general tyrosine kinase activity. However, the tyrphostin 51-treated sample (lane 3) shows these bands, suggesting that tyrphostin 51 is not blocking tyrosine kinase activity. Lane 5 is the antibody control (no lysate), and lane 6 is the lysate control (non¬ specific primary antibody) in which no bands other than antibody were detected. Although genistein may not be inhibiting G6PD release, I wanted to determine its effect on activity of the pentose shunt. Using a fluorescence assay, I found that the rise in NADPH after fertilization in genistein-treated eggs was much less than the rise in controls after both 60 minute and 90 minute genistein incubations. There was a 77% reduction in NADPH fluorescence in genistein-treated zygotes. I deduced that a reduction of approximately 50% can be accounted for by non-enzymatic effects of genistein by the following experiment; The fluorescence of NADPH in filtered sea water, in the absence of eggs, was assayed, and after adding genistein the fluorescence signal reduced immediately by approximately 50%. This suggests that genistein is causing a 23% decrease in shunt activity. Discussion Fertilization activates the egg metabolism, causing the egg to restart the cell cycle resulting in growth and division. The activation of the zygote metabolism results from the stimulation of many different biochemical pathways including the pentose phosphate shunt. One hypothesis for the activation of the zygote metabolism includes signal transduction events involving tyrosine kinase activity (see reference in Moore and Kinsey, 1995). It has been shown that soon after fertilization, tyrosine kinase activity in the egg increases two- to fourfold (Satoh and Garbers, 1985), and various different newly tyrosine-phosphorylated proteins appear (Ciapa and Epel, 1991) including the 350 kDa sperm receptor (Abassi and Foltz, 1994). Although tyrosine kinase activity is known to increase after fertilization, its involvement in overall egg activation or in the activation of specific biochemical pathways is an area of continuing study. The pentose phosphate shunt is a very important pathway used by many cells to produce compounds necessary for cell growth and division including NADPH and ribose units. NADPH is required by various pathways in the cell, including lipid, DNA and protein synthesis, and riboses are needed for nucleotide synthesis. In sea urchin eggs, the pentose shunt has been shown to be activated soon after fertilization (Swezey and Epel, 1995). This activation is correlated with the release and activation of the rate- limiting enzyme in the pathway, G6PD. G6PD is in a bound, inactive state in unfertilized eggs, and in a free, soluble, active state in fertilized eggs (Swezey and Epel, 1986). The mechanism for G6PD release and activation of the pentose shunt in sea urchin eggs at fertilization is currently unknown. It has been shown however, that in mammalian rat kidney cells, the mechanism that activates the shunt through the release of G6PD requires tyrosine kinase activity (Tian et al., 1991). In this case, treatment of cells with PDGF causes the tyrosine kinase in the PDGFR to become active, which is necessary for G6PD release (Tian et al. 1991). The purpose of my study was to determine whether the mechanism for G6PD release in sea urchin eggs after fertilization is similar to the mechanism used by mammalian somatic cells, requiring tyrosine kinase activity. Bindin and the Antibody Against the Sperm Receptor As Abassi and Foltz (1994) have shown, when eggs are treated with bindin, the sperm receptors within the egg membrane become tyrosine-phosphorylated, indicating that a tyrosine kinase has been activated. Incubating eggs with anti-receptor antibodies may also cause a similar response of tyrosine kinase activation. I studied the effects of treating eggs with bindin and anti-receptor antibodies to see if a G6PD release-response would be elicited due to the activation of this tyrosine kinase. According to my results, bindin is not causing G6PD release, however this conclusion may be particular to these experiments. Because bindin did not prevent sperm from fertilizing the eggs, there may not have been enough bindin to interact with its receptor. One way to ascertain whether bindin is interacting with the receptor would be to determine whether bindin-treatment is causing the receptor phosphorylation as described by Abassi and Foltz (1994). Similarly, the anti-receptor antibody treatments show no effect on G6PD release. However, in this case, the antibody-antigen interaction may be disrupted by the high ion content of sea water. That the eggs were not fluorescing when treated with fluorescent dye-conjugated secondary antibodies supports the idea that the antibody did not successfully bind the receptor. Previously, experiments done with these antibodies have been on in vitro membrane preparations and the jonic strength of solutions has been kept low (Abassi and Foltz, 1994). Binding of the antibody to live eggs can be enhanced by incubating the eggs in a solution that is isotonic to sea water. but has a low ionic strength. The osmolarity of this solution can be maintained by adding non-ionic compounds such as sucrose instead of ions. The effect of the anti receptor antibody treatments on G6PD release must be studied further by first ascertaining that these antibodies are, in fact, binding to the sperm receptor. Tyrosine Kinase Inhibitors Genistein and tyrphostin are both general tyrosine kinase inhibitors which prevent fertilization-induced tyrosine kinase activity in sea urchin eggs (Moore and Kinsey, 1995). In an effort to determine if general tyrosine kinase inhibition would block fertilization-induced G6PD release, I studied the effects of treating eggs with genistein and tyrphostin 51. Genistein does not inhibit G6PD release in sea urchin eggs. In addition, the Western immunoblot indicates that tyrosine phosphorylation is being inhibited under these conditions. Taken together, these results show that tyrosine kinases may not be involved in fertilization-induced G6PD release. Although genistein may not be preventing G6PD release upon fertilization, it may be affecting pentose shunt activity, Preliminary results from the in vivo NADPH assay show that there is a 77% reduction in the amount of NADPH fluorescence in genistein-treated zygotes. However, because a reduction of least 50% can be accounted for by non-enzymatic effects, it is unclear whether genistein is reducing the activity of the pentose shunt, or the reduction in fluorescence emission is due to some other factor. Further investigation of genistein effects on the pentose shunt will have to be done. Tyrphostin 51 also does not seem to inhibit G6PD release in sea urchin eggs However, as evidenced by the Western immunoblot, this compound does not seem to be inhibiting tyrosine phosphorylation. Moore and Kinsey (1995) studied the effects of tyrphostin B42, a compound in the same family of inhibitors as tyrphostin 51. They found that 100 uM tyrphostin B42 blocked tyrosine kinase activity. However, subtle differences in structure between these two compounds may account for the lack of inhibition by tyrphostin 51. For example, tyrphostin 51 may not be as permeant as tyrphostin B42. It is possible that tyrphostin 51 was not getting into the cells during the 90 minute incubation. This could explain its lack of tyrosine kinase inhibition as well as its lack of G6PD release and cell-division inhibition. Another possibility for the inability of tyrphostin 51 to block tyrosine kinase activity is that tyrphostin 51 is not effective at a 100 uM concentration. However, because the ICso of tyrphostin 51 is 800 nM (Sigma catalog, 1995), the 100 uM concentration should have been more than sufficient to cause inhibition. Conclusions My study suggests that the activity of the tyrosine kinases blocked by genistein is not necessary for G6PD release in S. purpuratus eggs at fertilization. These results lead me to the following general questions which must be answered to get a better understanding of the mechanisms involved in G6PD release and pentose shunt activation at fertilization of sea urchin eggs, as well as the involvement of tyrosine kinases in development. (1) Are there tyrosine kinases that are not inhibited by genistein which lead to G6PD release? While genistein is a general tyrosine kinase inhibitor, it most likely does not inhibit every tyrosine kinase in the cell. To be sure that tyrosine kinase activity is not required for G6PD release, effects of various other inhibitors would have to be studied. (2) Are any early developmental events blocked by genistein-inhibition of tyrosine kinases? We know that some of the later events of egg activation, including pronuclear migration, DNA synthesis, and cell division, are blocked by genistein. We also know that the early event of fertilization membrane elevation is not blocked (Moore and Kinsey, 1995), indicating that the early intracellulai Caz rise is occurring. However, we do not know how genistein effects some of the other early events of fertilization, including the significant pH rise needed for proper development. (3) How would inhibiting tyrosine phosphatase activity affect fertilization-induced G6PD release? By inhibiting tyrosine phosphatase activity, the relative amount of tyrosine phosphorylation would rise over time and might cause a release of G6PD if tyrosine phosphorylation is required for release in sea urchin eggs Answers to these questions will help to elucidate the mechanism involved with G6PD release at fertilization of sea urchin eggs, and will help to determine whether this mechanism is similar to that used by somatic mammalian cells. These mammalian cells differ substantially from sea urchin eggs, both in type of cell and event that causes G6PD release. The rat kidney cells are somatic mammalian cells whereas the sea urchin eggs are germ-line cells. G6PD release in the rat kidney cells occurs through hormone treatment and requires tyrosine kinase activity, while sea urchin eggs release G6PD at fertilization. The hormone treatment can occur numerous times in the life of the kidney cell, whereas fertilization occurs only once in the life of the egg cell. Because of these differences, the mechanism that releases G6PD may be quite different for these two types of cells, and tyrosine kinase activity may not be necessary for G6PD release in sea urchin eggs. If tyrosine kinases are not involved in G6PD release in sea urchin eggs at fertilization, then the intriguing question is what is the mechanism of this activation. and how else do the mammalian and urchin mechanisms differ? Works Cited Abassi, Y. A. and K. R. Foltz. 1994. Tyrosine phosphorylation of the egg receptor for sperm at fertilization. Developmental Biology. 164: 430-443 Capa, B. and D. Epel. 1991. A rapid change in phosphorylation on tyrosine accompanies fertilization of sea urchin eggs. FEBS. 295: 167-170. Edgecombe, M., R. Patel, and M. Whitaker. 1991. A cyclin-abundance cycle independent p34ede tyrosine phosphorylation cycle in early sea urchin embryos. The EMBO Journal. 10: 3769-3775. Epel, D. 1964. A primary metabolic change of fertilization: Interconversion of pyridine nucleotides. Biochemical and Biophysical Research Communications. 17: 62-68. Epel, D. 1990. The initiation of development at fertilization. Cell Differentiation and Development. 29: 1-12. Foltz, K. R., J. S. Partin, and W. J. Lennarz. 1993. Sea urchin egg receptor for sperm: Sequence similarity of binding domain and hsp70. Science. 259: 1421-1425. Laemmli, U. K. 1970. Ceavage of structural proteins during the assembly of the head of bacteriophage T4. Nature. 227: 680-685. Lopez, A., S. J. Miraglia, and C. G. Glabe. 1993. Structure/ function analysis of the sea urchin sperm adhesive protein bindin. Developmental Biology. 156: 24-33. Moore, K. L. and W. H. Kinsey. 1995. Effects of protein tyrosine kinase inhibitors on egg activation and fertilization-dependent protein tyrosine kinase activity. Developmental Biology. 168: 1-10. Satoh, N. and D. L. Garbers. 1985. Protein tyrosine kinase activity of eggs of the sea urchin Strongylocentrotus purpuratus: The regulation of its increase after fertilization. Developmental Biology. 111: 515-519. Sigma Chemical Company 1995 Catalog. 1031. Smith, P. K., R. I. Krohn, G. T. Hermanson, A. K. Mallia, F. H. Gartner, M. D. Provenzano, E. K. Fujimoto, N. M. Goeke, B.J. Olson, and D. C. Klenk. 1985. Measurement of protein using bicinchoninic acid. Analytical Chemistry. 150: 76-85 Stanton, R. C. and J. L. Seifter. 1988. Epidermal growth factor rapidly activates the hexose monophosphate shunt in kidney cells. American Journal of Physiology. 253 (Cell Physiology 22): C267-C2 Stanton, R. C., J. L. Seifter, D. C. Boxer, E. Zimmerman, and L. C. Cantley. 1991. Rapid release of bound glucose-6-phosphate dehydrogenase by growth factors. The Journal of Biological Chemistry. 266: 12442-12448. Swezey, R. R. and D. Epel. 1986. Regulation of glucose-6-phosphate dehydrogenase activity in sea urchin eggs by reversible association with cell structural elements. The Journal of Cell Biology. 103: 1509-1515. Swezey, R. R. and D. Epel. 1995. The in vivo rate of glucose-6-phosphate dehydrogenase activity in sea urchin eggs determined with a photolabile caged substrate. Developmental Biology. in press. Thorpe, G.H. G., L. J. Kricka, S. B. Moseley, and T. P. Whitehead. 1985. Phenols as enhancers of the chemiluminescent horseradish peroxidase-luminol-hydrogen peroxide reaction: Application in luminescence-monitored enzyme immunoassays. Clinical Chemistry. 31: 1335-1341. Tian, W., J. N. Pignatare, and R. C. Stanton. 1994. Signal transduction proteins that associate with the platelet-derived growth factor (PDGF) receptor mediate the PDGF-induced release of glucose-6-phosphate dehydrogenase from permeabilized cells. The Journal of Biological Chemistry. 269: 14798-14805. Towbin, H., T. Staehlin, and J. Gordon. 1979. Electrophoretic transfer of proteins from polyacrylamide gels to nitrocellulose sheets: Procedure and some applications. Proceedings of the National Academy of Sciences, USA. 76: 4350-4354. TABLE 1 Effects of Bindin and Anti-Bindin Receptor Antibodies on G6PD Release in Unfertilized S. purpuratus Eggs (Data expressed as percentage of bound G6PD) Control Bindin 60 ng/ml Bindin 60 pg/ml Experiment 1 52.0 45.0 52.0 Control Anti-Exo IgG Control IgG Experiment 2 55.6 47.6 44.4 Experiment 3 68.5 66.3 56.2 Note: Unfertilized eggs were treated with either 60 ng/ ml or 60 pg/ ml soluble bindin in experiment 1. Anti-exo receptor IgG antibodies were used in both experiments 2 and 3. The control IgG for experiment 2 was goat immunoglobulins, and the control IgG for experiment 3 was anti-cyto receptor IgG antibody. In all experiments, G6PD bound after fertilization of controls was less than or equal to 10%. Each value in the table was calculated from the mean of two assays on each sample. Figure Legends Figure 1: 1% egg suspensions were incubated for 1 hr with 100 uM genistein before fertilizing and assaying for G6PD activity. Controls were incubated in 0.1% DMSO. Both unfertilized samples were taken 15 minutes before the fertilized samples. The graph shows the means of two experiments, and bars represent ranges of these values. Figure 2: 1% egg suspensions were incubated for 90 minutes with 100 uM tyrphostin 51 before fertilizing and assaying for G6PD activity. Controls were incubated in 0.1% DMSO. Both unfertilized samples were taken 15 minutes before the fertilized samples. Data are from one experiment. Figure 3: Eggs were treated with 100 uM genistein and 100 uM tyrphostin 51 for 90 minutes before fertilization and subsequent sampling for immunoprecipitation. Unfertilized and fertilized controls were treated with 0.1% DMSO for 90 minutes as well. All samples were immunoprecipitated using the anti-phosphotyrosine antibody PY-20. Unfertilized control, lane 1. Genistein, lane 2. Tyrphostin 51, lane 3. Fertilized control, lane 4. An antibody control using no lysate and a control using non-specific mouse IgG as a primary antibody were also done (lanes 5 and 6 respectively). 20 EFFECTS OF CENISTEIN ON GGPD RELEASE 100- 80 60 40 20 UNFERT FERT UNFERT FERT GENISTEIN CONTROLS FIGURE 1 a EFFECTS OF TYRPHOSTIN 51 ON GGPD RELEASE 100- 80 60 40- 20 UNFERT FERT UNFERT FERT TRPHOSTIN 51 CONTROLS FIGURE 2 Tyrosine Kinase Inhibition by Genistein and Tyrphostin 51 KDa 200 97.4 69 46 30 * 21.5 Figure 3