Abstract: Six serotonin antagonists, cinanserin, methiothepin, spiperone, metergoline, ketanserin, and methysergide, were all found to delay the first two divisions of sea urchin embryos. Three serotonergic agonists, DOI, RU24969, and phenyl biguanide were also found to delay cleavage, although more weakly than the antagonists. Cleavage delays caused by 10 uM metergoline and 10 uM ketanserin were reversed by serotonin. Serotonin alone was found to speed up cell division over controls. Cytological studies showed the serotonin antagonists metergoline, ketanserin and methysergide delayed karyokinesis as well as cytokinesis. Introduction: Serotonin, or 5-hydroxytryptamine (5-HT), a potent mammalian neurotransmitter, was first reported in sea urchin embryos in the late '60's (Buznikov et al, 1964, 1970). The method originally used was a fluorescence assay (Buznikov et al., 1970; Toneby, 1977), and these findings were later confirmed with the more specific techniques of HPLC and thin-layer chromatography (Renaud & Parisi, 1981, Toneby, 1977). Two lines of evidence suggest that 5-HT is a regulator of sea urchin embryo development. First, fluctuations in 5-HT levels, coincide with early cell divisions (Buznikov et al. 1964). Secondly, serotonin antagonists inhibit development, and in particular cause a delay in early cleavages (Buznikov et al, 1970; Renaud & Parisi, 1981). Using the sea urchin species Paracentrotus lividus and Sphaerechinus granularis, Renaud & Parisi reported reversal of the cleavage inhibition, caused by the 5HT antagonists metergoline and gramine, by the simultaneous addition of serotonin to the incubating eggs. However, Denis LaRochelle in David Epel's lab found that this was not possible with Strongylocentrotus purpuratus eggs. Species differences can mean variable plasma membrane permeability. Since serotonin is a charged molecule at physiological pH, egg permeability could indeed be the reason for the seemingly negative results. I therefore decided to use the technique of electrically permeabilizing the eggs, adding a substrate, and then resealing the plasma membrane pores with low calcium sea water (method of Robert Swezey and David Epel, 1989). I achieved moderate success reversing the effects of 5-HT antagonists metergoline and ketanserin with serotonin. When high amounts of serotonin were used, cells treated with serotonin cleaved much earlier than controls. Renaud and Parisi (1981) had reported that gramine's effect on cleavage only included a delay in cytokinesis, not in karyokinesis, or chromosal replication and separation. So, in order to investigate the nature of serotonin involvement in development, I used 4,6-diamidino-2-phenyl-indole (DAPI) to fluorescently stain the chromosomes and observe karyokinesis in antagonist-treated eggs as compared to controls. I found that metergoline, ketanserin, and methysergide all delayed karyokinesis concurrent with the delay in cytokinesis. Recently, a great deal of neurological research has resulted in the characterization of three types of serotonin receptors: 5-HT1, 5-HT2, and 5-HT3 receptors. In addition, within the 5-HTI class, there are four distinct subclasses: 5-HTIA, 5-HTIB, 5- ITIC, and 5-HTID receptors. Each receptor type and subtype has different affinities for different serotonergic drugs. They are characterized by radioligand studies and by pharmacological differences. Most 5-HT receptors bind the same drugs; the difference is in the affinities for these drugs. I have included as table 1, a characterization of 5-HTI and 5-HT2 receptors (from S. Peroutka, 1988). Different receptor types have also been correlated with different activities. For example, 5-HTIC and 5¬ T2 receptors have been proposed to affect phophotidylinositol turnover, whereas 5-HTlA receptors have been correlated with adenylate cyclase modulation. Although the putative intracellular receptors in sea urchin eggs are unlikely to be the same as any classified neural extracellular receptors, comparison of different drug affinities for these receptors is nevertheless a useful way of characterizing them. Therefore, I have done a series of concentration experiments with the serotonergic drugs metergoline, methysergide, spiperone, ketanserin, methiothepin, cinanserin, DOI, RU24969, and 1-phenyl biguanide in order to compare drug potencies and help characterize the hypothesized receptors. Structures of all drugs used are in tables 2 and 3. Methods and Materials: Fresh S. purpuratus gametes were collected by injecting 1-2 mls of .5 M KCl into gravid sea urchins. The eggs were kept stirring Eggs were always at 160C. Dry sperm was kept at 400. mechanically dejellied by passage through Nitex mesh and washed twice before use. Eggs were diluted or concentrated as necessary to keep a constant suspension of 28 (as measured by Bauer-Schenk centrifuge tubes). Eggs were then fertilized, and subsequently, the appropriate drugs added. Eggs were incubated in 24-microwell plates, .5 ml per well. Drugs that were able to freely diffuse through the egg membrane were simply added to the samples, the same amount of solvent being added to the control plate. Whether drugs were freely diffusible through the membrane was judged by trial and error, i.e. determining whether the drug had an effect on cleavage when simply added to the incubation plate. The two solvents used were distilled water and dimethyl sulfoxide (DMSO). If DMSO was used, the maximum amount added to the eggs was 2ul/ml of egg suspension. The fertilized, treated eggs were incubated at 1600. Samples of two-cell and four-cell stages were taken of the developing embryos at 100, 110, 120, 155, and 165 minutes and put into a 18 formaldehyde solution. 100 embryos were counted for each time stop of each plate and numbers of cleaved cells taken to be percentages. Electric Permeabilization of Eggs Whenever serotonin was used, it was necessary to permeabilize the unfertilized eggs to allow the 5-HT to enter the cells. For these experiments, after dejellying and washing the eggs, they were resuspended in zero calcium sea water and washed twice, then washed twice in transpermeabilization media (Trans Mix). The transpermeabilization media is intended to mimic the cytoplasm of the egg so that when eggs are electroporated, they do not lose too many nutrients to their surroundings, nor do they become activated by calcium or lysed by high sodium concentrations. This media consists of 225 mM potassium gluconate, 185 mM mannitol, 300 mM glycine, .5 mg/ml glutathione, 5 mM magnesium chloride, 4 mM ATP, 10 mM spermidine (to keep the membranes intact), 20 mM sodium chloride and 2 mM sodium bicarbonate. The eggs were then given 300 volts of electric current, with.6 microfarads capacitance, 1 pulse every 10 seconds, for a total of 5 pulses. The eggs were then transferred to Eppendorf tubes containing either serotonin in.058 ascorbic acid, or .058 ascorbic acid only (for controls). After 2 minutes, an excess of low calcium sea water (9:1 ratio of zero calcium sea water to fresh sea water) was added to each vial, the low concentration of calcium resealing the egg pores without activating the eggs. The eggs were washed once with 9:1 mix, then twice with fresh sea water for a final suspension of 28. The rest of the procedure is identical to the first method. DAPI Staining S.purpuratus eggs were prepared according to the above two methods, depending on whether serotonin was used or not. Instead of fixing eggs with formaldehyde, however, the DAPI staining method was used to kill the eggs and stain the chromosomes for viewing under a fluorescence microscope. At 70, 80, 90, and 100 minutes, 1 ml of egg suspension from each plate was washed twice in KGE mix (3 mM potassium gluconate, 3.2 mM glycine, .4 mM EGTA, and .4 mM magnesium sulfate). Eggs were then resuspended in 1 ml of .18 Triton detergent in KGE mix. 1 ul of a 1 mg/ml solution of 4,6-diamidino-2-phenyl-indole (DAPI) was added to each ml of prepared eggs. In addition, formaldehyde stops were taken at 90, 100, 110, and 120 minutes in order to see cytokinesis effects and compare them to effects on mitosis by the drugs. DAPI samples were then viewed under a fluorescence microscope. If the results were not obvious, plates were scored by counting 100 samples in each plate. When high amounts of serotonin antagonists were used, the results were obvious simply by viewing. Results: Delay of Cleavage by Serotonergic drugs Table 4 shows the effective concentrations of all drugs used. Cinanserin, a 5-HT2 antagonist, was found to be the most powerful drug in delaying cleavage. The graph of the delay in cleavage caused by 10 uM concentration cinanserin looks like delays caused by 100 uM concentrations of most other drugs (see figures 1-6). C Other potent drugs were Methiothepin, Spiperone, Ketanserin and Metergoline, all 5HT2 antagonists. Methysergide, a 5-HT2 antagonist, was somewhat less potent, but nevertheless significantly delayed cleavage at a concentration of 30 uM. Three selective agonists were used as well: RU24969, a 5- HTIB agonist; DOI, a 5-HT2 agonist; and 1-phenyl biguanide, a 5-HT3 agonist. None of these agonists had the expected effect of speeding up cleavage. On the contrary, as shown in figures 7-9, they all acted as serotonin antagonists by delaying cleavage. As shown in table 1 and figures 7-9, Phenyl biguanide was a very weak antagonist, effective only at very high concentrations, whereas DOI was the most potent and RU24969 showed a medium effectiveness (effectiveness as measured by the concentration of drug required to significantly delay cleavage). Effects of Serotonin As shown in figures 10-11, I was able to reverse cleavage delays by metergoline and ketanserin with serotonin. The concentrations of serotonin used are only approximate because, using the electroporation technique, it is impossible to know for any given experiment exactly how much substrate is entering into the cells. For the metergoline experiment, I found that "100 uM serotonin reversed the effects of 10 uM metergoline, but the 1mM serotonin sample was not sped up over controls. In the ketanserin experiment, however, I found that serotonin not only reversed the 10 uM ketanserin delay, but also, as shown in figures 11 and 12, embryos with concentrations of serotonin higher than 10 um divided significantly ahead of controls. Delay of Mitosis Usin the DAPI method, I examined the effects of metergoline, methysergide, and ketanserin on progression through mitosis. All antagonists were found to also delay karyokinesis to the same degree that cytokinesis was delayed. If a low concentration of drug was used, the same percentage type delay ensued in both cytokinesis and in karyokinesis. When a high concentration of drug was used, drug-treated eggs were 1008 delayed over controls in both cytokinesis and karyokinesis. Please see Table 5 for results of each experiment. Discussion: Although serotonin receptors have not yet been characterized in sea urchin eggs or embryos, all my results point to the conclusion that serotonin receptors do exist in these embryos. Six selective serotonin antagonists all delayed cleavage of activated eggs. In addition serotonin appears to be involved in early cell division, both cytokinesis and karyokinesis. Cytological studies showed that eggs treated with high amounts of antagonist (100 uM ketanserin and 50 uM metergoline) accumulated in prophase, whereas controls moved on to other phases of mitosis. The most interesting aspect of these experiments is the reversal of metergoline and ketanserin inhibition by serotonin, Serotonin seems to interact competitively with these two antagonists, acting in a concentration-dependent way. The experiments with ketanserin especially show that the higher the serotonin concentration used, the faster cell division occurred. While the putative sea urchin egg serotonin receptors are affected by all the serotonergic drugs I assayed, known to be effective on nerve cells, these receptors do not seem to be comparable to nerve receptors. In terms of the antagonist affinities, sea urchin receptors seem to be comparable to 5-HT2 receptors, ordinarily found in mammalian cerebral cortex cells. However, the potent 5-HT2 agonist DOI had the effect of acting as an antagonist and delaying cleavage. Similar results were seen with the 5-HTIB agonist RU24969 and the 5-HT3 agonist phenyl biguanide, indicating that sea urchin receptors cannot be 5- ITIB, 5-HT2, or 5-HT3 receptors. The only other characterized receptor types are 5-HTIA, 5-HTIC and 5-HTID. However, the fact that the cinanserin, ketanserin and spiperone all potently inhibited development would discourage the conclusion that sea urchin egg receptors could be one of these three remaining subtypes-these three antagonists have very low, if any affinity Most nerve receptors are for these three subtypes. extracellular. But this study indicates sea urchin egg receptors are probably intracellular; in order to get an effect from serotonin, it was necessary to permeabilize the egg so that the substrate could enter the cell. Therefore, sea urchin receptors may be a novel receptor type or subtype, as yet uncharacterized. An interesting finding is that the only agonist that has been found to act on these receptors is serotonin itself. The receptors appear to bind similar substrates, but not be activated by them in the same way as its intended substrate, serotonin. As shown in figure 12, serotonin not only reverses the effect of the antagonists ketanserin and metergoline, but by itself, speeds up development. Further studies on serotonin's role in sea urchin egg development could clarify many remaining questions. The use of 5-HTIA, 5-HTIC, and 5-HTID agonists would confirm whether or not sea urchin egg receptors are comparable to known nerve cell receptors. Radiolabeling, antibodies, or other methods could help confirm the existence of the receptors, and possibly locate them in the cell. I did in fact attempt a standard radiolabeling experiment in Steve Peroutka's lab at Stanford University, but found no receptor activity. However, these results are not conclusive since this test is designed for high density nervous tissue, such as rat brain. In fact this test does not find activity in lower density receptor tissue such as cardiac tissue, which has known, characterized serotonin receptors (S. Peroutka, personal communication). So, a different radioassay would have to be designed to definitively find activity. Finally, as noted in the introduction, serotonin receptors in other systems are known to affect phosphatidylinositol turnover, and adenylate cyclase activity. Therefore, studies measuring the effect of serotonin on calcium and cAMP levels in sea urchin embryos, or phosphotidylinositol turnover could help 10 c clarify the mechanism by which serotonin affects development. A most intriguing result, given the apparent intracellular nature of these receptors, is that the mode of action may be by some yet undescribed mechanism. table 5-HT RECEPTOR SUBTYPES A summary of drug potencies at each of the five known S-HT binding site subtypes is provided in Table 2. These data are discussed in greater detail in the following section. Table 1 Characteristics of 5-HT, S-HT», 5-HT,c, 5-HTp, and 5-HT, binding sites S-HT 5-HTc S-HTp 5-HT, 5-HTA H-S-HT H-S-HT H-S-HI H-Spiperone H-S-HT Radiolabeled 1231.CYI H-Mesulergine H-Mesulergine H-8-OH¬ DPAT Linans 1231-LSD 1231.LSD H-Ipsapirone (rat and H-Ketanserin H-WB 4101 mouse only) Mianserin H-Buspirone H-N-methylspiperone 'H-PAPP 1231. Methyl-LSD H-DOB Layer IV Raphe nuclei Substantia Choroid Basal High plexus nigra ganglia cortex density Hippocampus Globus pallidus Table 2 Drug affinities for 5-HTA, S-HTI», 5-HTIC, S-HTD, and 5-HT, receptors Drug potencies S-HT S-HT 5-HTp 5-HT, S-HT (K., nM) 5.CT 10 RU 24969 Mesulergine Spiperone 5.CI 5-CT 5-HT Mesulergine 8-OH-DPAT Metergoline 5S-HT 5-HT Methysergide Methysergide Metergoline RU 24969 Metergoline Mianserin d-LSD d-LSD Methysergide Metergoline Metergoline Mianserin 10-1000 Methysergide 5-HT Mianserin Methysergide RU 24969 8-OH-DPAT d-LSD Spiperone 5-CT d-LSD Mesulergine d-LSD RU 24969 RU 24969 Mesulergine » 1000 Mianserin Mianserin Spiperone 5-HT 8-OH-DPAT Spiperone Spiperone 8-OH-DPAT Mesulergine 8-OH-DPAT Data given are derived from Peroutka & Snyder (1979), Peroutka (1986), Hoyer et al (1985b), Heuring — Metergoline. Cen, NO C3 Spiperone. )e-a,d, N KETANSERIN table 2 ANTAGONISTS Methysergid(e). G, , don N N— W e 5 ch, METHIOT HEPIN ci CINANSERIN E Serotonin. Sachane R(-)-DOI NH, cn. e oen, Phenyl Biguanide. NH NH CgligNHCNHCM, RU 24969 cn,o table 3 AGONISTS TABLE 4 RESULTS OF SEROTONERGIC DRUG CONCENTRATION EXPERIMENTS SEROTONERGIC DRUG LOWEST EFFECTIVE CONCENTRATION/POTENCY —————— ———————————. CINANSERIN 10 uM (PROBABLY LESS)/VERY HIGH METHIOTHEPIN 10 uM / HIGH METERGOLINE 10 uM / HIGH SPIPERONE 10 uM / HIGH KETANSERIN 10 uM / MEDIUM ZTHYSERGIDE 30 uM / LOW 10-50 uM / MEDIUM DOI (agonist) 100 uM/ LOW RU24969 (agonist 1mM / VERY LOW PHENYL BIGUANIDE (agonist) TABLE 5 RESULTS OF KARYOKINESIS (DAPI STAINING) EXPERIMENTS EXPERIMENT/PLATE MITOSIS STAGE —————— ——-——---———- - I. KETANSERIN (20 uM) 408 PROMETAPHASE +1 / CONTROL/ 90 MINUTES 608 METAPHASE 708 PROMETAPHASE +1 / 20 uM KETANSERIN/ 90 MIN 308 METAPHASE 78 PROMETAPHASE +1 / CONTROL/ 100 MINUTES 208 METAPHASE 698 ANAPHASE 88 PROMETAPHASE +1 / 20 uM/ 100 MINUTES 528 METAPHASE 418 ANAPHASE ——— II. METHYSERGIDE 38 PROMETAPHASE +2 / CONTROL/ 90 MINUTES 908 ANAPHASE 78 TELOPHASE 128 PROMETAPHASE +2 / 100 uM METHYSERGIDE/ 90 MIN 148 METAPHASE 738 ANAPHASE 18 TELOPHASE ————— —————— — — ——— -——— III. KETANSERIN (100 uM) +3 / CONTROL/ 80 MINUTES ALL IN PROMETAPHASE AND METAPHASE +3/ 100 uM KETANSERIN/ 80 MIN ALL IN PROPHASE +3 / CONTROL/ 90 MINUTES ALL IN ANAPHASE AND METAPHASE MOST IN PROPHASE +3 / 100 uM KETANSERIN/ 90 MIN SOME IN PROMETAPHASE MOST IN TELOPHASE +3 / CONTROL/ 100 MINUTES SOME IN ANAPHASE MOST IN METAPHASE +3 / 100 uM KETANSERIN/ 100 MIN SOME IN PROMETAPHASE ----—- —— IV. METERGOLINE +4 / CONTROL/ 90 MINUTES 1008 IN METAPHASE 1008 IN PROPHASE #4 / 50 uM METRGOLINE/ 90 MIN +4 / CONTROL/ 100 MINUTES 1008 IN ANAPHASE 1008 IN PROPHASE +4 / 50 uM METERGOLINE/ 100 MIN FIGURE LEGENDS 1. Delay of cell division by 10 uM cinanserin, 2-cell stage. 2. Delay of cell division by 10 and 20 uM spiperone, 2 and 4¬ cell stages. 3. Delay of cell division by 10 and 50 uM methiothepin, 2- and 4-cell stages. 4. Delay of cell division by 10 uM ketanserin, 2 and 4-cell stages. 5. Delay of cell division by 10 uM metergoline, 2-cell stage. 6. Delay of cell division by 30 and 100 uM methysergide, 2 and 4-cell stages. 7. Delay of cell division by 10, 50, and 100 uM DOI, a 5-HT2 agonist. Delay of cell division by 1 mM phenyl biguanide compared to delay by 10 uM metergoline, 2 and 4-cell stages. Delay of cell division by 20, 30, 50, and 100 uM RU24969, a 5-HTIB agonist, 2 and 4-cell stages. 10. Reversal of the effects of 10 uM metergoline by serotonin, 2-cell stage. 11. Reversal of the effects of 10 uM ketanserin by serotonin, 2-cell stage. 12. Serotonin speeds up cell division, lmM concentration, 2 and 4-cell stages. CINANSERIN STRONGLY DELAYS CLEAVAGE 110 100 ——e ———0 90+ 80+ 70 5 20 •—• CONTROL A--A 10 UM CINANSERIN 09 90 100 110 120 | 130 | 140 | 150 | 160 MINUTES POST-FERTILIZATION figure EFFECT OF SPIPERONE ON CLEAVAGE O—O CONTRO A--A 10 HM SPIPERONE D 20 AM SPIPERONE —— — 75 og — 110 125 140 155 170 185 MINUTES POST-FERTILIZATION figure 2 EFFECT OF METHIOTHEPIN ON CLEAVAGE O—O CONTROI 100 A--A 10 AM METHIOTHEPIN □—D 50 AM METHIOTHEPIN o A 110 125 140 155 MINUTES POST-FERTILIZATO EFFECT OF 10 uM KETANSERIN ON CLEAVAGE • CONTRO 100 •--° 10 AM KETANSERIN 6 75 25+ 00 9-2-----4 100 140 120 MINUTES POST-FERTILIZATION figure 4 EFFECT OF 10 MM METERGOLINE ON CLEAVAGE 100 O 804 O—O CONTROL - 10 AM METERGOLINE o 100 120 140 160 180 200 MINUTES POST-FERTILIZATION figure 5 EFFECT OF METHYSERGIDE ON CLEAVAGE O—O CONTROL 100 A--A 30 MM METHYSERGIDE D—D 100 AM METINSERCRE 6 75 50 O 2 o 110 125 140 155 DOI, A 5HT2 AGONIST, ANTAGONIZES O CONTROL A—A TOAM D0 D— 50 AM D0 8—2 •—• 100 AM DO 4—2 175 MINUTES POST-FERTILIZATION figure 7 PHENVL BIGUANIDE, A 5HT3 AGONISI COMPARED TO METERGOLINE, A GENERAL 5HT ANTAGONISI 110 9—0 CONTROL A—A 10 AM METERGOLINE •-- ImM PHENYL BIGUANIDE 2 180 MINUTES POST-FERTILIZATION figure 8 RU24969, A 5-HTIB AGONIST, ANTAGONIZES •—• CONTROL 100 —• 20 M RU24969 O— 30 AM RU24969 A—A 50 UM RU24969 80 D—D 100 AM RU24969 40 2 110 125 140 155 MINUTES POST-FERTILIZATION ure 110 REVERSAL OF METERGOLINE EFFECTS BY SEROTONIN 100 80 8 60+ O-O CONTROL 40 •— 10 AM METERGOLINE d 20 A-A 10 EM METERGOLINE + 100 MM SEROTONIN — 100 120 140 160 180 200 MINUTES POST-FERTILIZATION figure IO REVERSAL OF KETANSERIN BY SEROTONIN 110 •— CONTROL •-- 10 AM KETANSERIN Ooneansgen +IOAM SEROTONIN A—A 1 mM SEROTONIN MINUTES POST-FERTILIZATION figure1 EFFECT OF SEROTONIN ON DIVISION 0—e CONTRO A—A 1 mM SEROTONIN 06 2— MINUTES POST-FERTILIZATION 110 REFERENCES Buznikov, G.A., I.V. 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