ABSTRACT The marine worm Urechis caupo exhibits a multixenobiotic resistance (MXR) similar to multidrug resistance (MDR) in mammalian tumor cells. Urechis oocytes from their developing stages in the coelomic fluid to at least the two-day larval stage possess a membranous protein of 160 kD that is immunologically related to the mammalian MDR P-glycoprotein of 170 kD. However, activity of the 160 kD protein is absent in developing coelomic oocytes but is detected once the oocytes reach the storage organs as immature oocytes. Further studies are necessary to investigate the causes for the activity increase of the MXR protein at this stage. INTRODUCTION A major focus of current cancer research is on the multidrug resistance phenomenon mediated by the multidrug transport protein or P-glycoprotein. Different chemotherapeutic drugs similar only in their moderate hydrophobicity are transported out by this protein, rendering clinical chemotherapy virtually ineffective (West, 1990). P-glycoprotein is a transmembrane protein with two ATP binding sites (Chen et al., 1986; Gros et al., 1986). Hydrophobic compounds including natural toxins and anti-cancer agents diffuse naturally into the tumor cell, and P-glycoprotein then utilizes ATP to transport the hydrophobic compounds out of the cell (Harper, 1993). This multidrug resistance to a variety of drugs is also accompanied by a decrease in the drug accumulation (Juliano, 1976) (Figure 1). However, the MDR extrusion pump can be saturated and thus inhibited by other MDR substrates such as verapamil. In this case, the MDR transport pump becomes non-functional and chemotherapeutic drugs and other hydrophobic compounds enter the tumor cell and effectively destroy it. A similar phenomenon to MDR is seen in some aquatic animals including mussels, sponges, fishes, and worms. In these animals, a multixenobiotic transport protein is as a possible defense mechanism against natural and man-made xenobiotics. Studies on the echiuroid worm Urechis caupo show that a protein immunologically and functionally related to the mammalian MDR protein is present in its oocytes and embryos. Urechis caupo live in polluted mudflats where they inhabit U¬ shaped burrows. They circulate water and oxygen through the tunnel by rhythmic peristalsis of their bodies, and feed by secreting a mucous net to trap small food particles. Gametes continuously develop in the coelomic fluid (Morris, Abbott, Haderlie, 1980). After reaching a certain stage of development, they are then sequestered by collecting organs and stored in three pairs of storage organs near the anterior region (Figure 2). A multixenobiotic resistance mechanism has been discovered in Urechis caupo using fluorescence assays and immunoassays (Toomey, 1993). The fluorescence assay measures the accumulation of the dye rhodamine B, which is a substrate for the transport protein (Neyfakh, 1988). Embryos or oocytes are incubated in rhodamine B with and without verapamil, a potent competitive substrate of the MDR protein. Oocytes in rhodamine have a lower fluorescence than oocytes in rhodamine plus verapamil. Since verapamil competes with rhodamine for export; less rhodamine efflux occurs and the cells fluoresce more. MXR activity is thus assayed by comparing the fluorescence of oocytes incubated in both rhodamine and verapamil to those incubated in rhodamine alone with a ratio of 2 to 8 usually indicating MXR activity. However, the ratio range is not absolute due to variance among oocytes from different female Urechis. Immunoassays used to detect a protein immunologically related to the mammalian P-glycoprotein include gel electrophoresis and Western blotting, which probe protein samples with an antibody to the mammalian MDR protein. R7 cells or other cell lines containing the mammalian protein are used to insure validity of the antibody probe and for comparison with the protein samples. Recent studies have investigated the MXR mechanism in mature oocytes and embryos of Urechis caupo without any specific focus on the different stages of development. In my study, I focused on investigating the presence and activity level of MXR from the coelomic oocyte to the two-day larval stage using Western blots and the rhodamine fluorescence assay. My results showed the presence of a a protein immunologically related to the mammalian P¬ glycoprotein in Urechis from coelomic oocytes through the two-day larvae. However, MXR activity was absent in coelomic oocytes, present only in the immature oocytes in the storage organs, in the fertilized oocytes, and in the embryos. For clarification, developing oocytes reside in the coelomic fluid, and immature oocytes are stored in storage sacs. Oocytes reach maturity only when they have become fertilized. MATERIALS AND METHODS COLLECTION AND MAINTENANCE Adult Urechis caupo were collected at Elkhorn Slough near Moss Landing, California. They were maintained in tanks with running seawater and a layer of mud from the slough. SPAWNING Immature gametes were obtained by inserting a rounded smooth-tipped glass pipette into one of six gonadopores and gently rotating the pipette back and forth (Figure 3). Either sperm (white) or oocytes (pink, yellow, or olive) gushed from the gonadopore. The sperm was pipetted in its concentrated form into an eppendorf tube and stored in a refrigerator, able to retain its viability for 3-5 days. The oocytes were rinsed off the animal into a beaker with filtered seawater. They were stored at 17°C until use, and fresh oocytes were obtained every day. FERTILIZATION Urechis oocytes were fertilized by adding a drop of dilute sperm into a beaker of oocytes in filtered seawater. After a few minutes, the excess sperm were washed out by hand centrifugation and suctioning off the supernatant with an aspirator. The fertilized oocytes were then resuspended in fresh, filtered seawater. EXTRACTIONOE COELOMICOOCYIES Oocytes are continuously developing in the coelomic fluid of female Urechis (Miller, 1973). The coelomic fluid was extracted by puncturing the body wall near the posterior end with a needle and squeezing the fluid out into a small beaker. The fluid was then centrifuged in a swinging-bucket rotor for two minutes in an international clinical centrifuge at 1500 g (Gould, 1967). The developing oocytes form a light brown layer above the coelomocytes and were selectively removed with a pipette. This centrifugation step was repeated several more times to further purify the oocytes. RHODAMINE ELUORESCENCE ASSAY For each rhodamine assay, a 10 ml egg suspension was first obtained and then divided evenly into two 5 ml egg suspensions of approximately equal concentrations. To each egg suspension, 5 ul of either 1 mM or 5 mM rhodamine B were added for a final To rhodamine B concentration of either 1 uM or 5 uM, respectively. one of each pair of egg suspensions 25 ul of either 2 mg/ml or .2 mg/ml verapamil were added, depending on the desired final concentration of either 22 uM or 2.2uM verapamil. After the samples were incubated for, one hour at 17°C, they were spun in a hand centrifuge, the rhodamine supernatant was suctioned off with an aspirator, and the eggs were resuspended in 1 ml of filtered seawater. The egg cells were immediately positioned under a l6X lens of an epifluorescence microscope with filters for rhodamine and the aperture was closed to a fixed point. At the later stages of development (e.g. gastrulation and 2-day larvae), 37% formaldehyde was used to immobilize the moving embryos. Fluorescence measurements were taken on 10-20 healthy oocytes or zygotes by a photosensor attached to the microscope. The light emitted by each embryo was picked up by the photosensor and converted to a numerical value by a voltmeter. In immature and fertilized oocytes, mean values were calculated for each sample, and ratios of the mean values of cells with and those without verapamil were calculated as an index of MXR activity. The second set of experiments involved performing rhodamine fluorescence assays on coelomic and immature oocytes from the same female Urechis. Oocytes of different sizes develop in the coelomic fluid; the diameter of each coelomic oocyte was measured with a reticule and the fluorescence was measured as above. One unit on the reticule equaled 66.7 microns. WESTERN BLOTS Protein Sample Assays Oocytes at various stages of development were washed, hand centrifuged, and concentrated into about 100 ul in an eppendorf tube. A minimum amount of lysis buffer (approximately 170 ul) was added to the egg concentrate. The eggs were then homogenized into a milky solution and were put on ice for a while. Approximate 100 ul of 5% SDS was added to the homogenate which was then sonicated ten times for 3 seconds each. Protein concentrations of each sample were obtained using the BCA protein assay(Pierce). A standard curve using bovine serum albumin (BSA) diluted with 5% SDS was constructed using the following concentrations of BSA: 0 mg/ml, 0.1 mg/ml, 0.25 mg/ml, 0.50 mg/ml, and 1.00 mg/ml. 5 ul samples of each sample and dilutions of the egg samples were placed in triplicate in a 96 well micro-titer. 100 ul of BCA working reagent was then added to each well, and the samples were incubated at 60°C for 30 minutes. The protein concentrations of the unknown samples were determined using a Molecular Devices VMax plate reader at 550 nm. Each egg sample was mixed with an equal amount of sample buffer and boiled for five minutes in a water bath. The samples were then stored in a freezer at -200C. Gel Electrophoresis and Western Blotting Samples were loaded onto a 7.5% polyacrylamide gel at approximately 40 ug of protein per lane. The proteins were separated on a BioRad minigel apparatus using a tris/glycine running buffer and transferred to nitrocellulose membranes using a BioRad electrophoretic transfer system. The proteins were transferred at 13 V for 1 hour, 24 V for 2 hours, and 36 V overnight. The blots were blocked with PBS-Tween 20 (.05%)-BSA(lOmM) for 30 minutes and then incubated for 2 hours with C219 monoclonal antibody (Centocor) (1:250 in PBS-Tween 20-BSA,). The nitrocellulose membrane was washed for 10 minutes with 10 mls of the PBS- Tween20-PBS blocking solution three times and then incubated for 1 hour with goat anti-mouse IgG conjugated to alkaline phosphatase (Sigma) (1:1000 in PBS-Tween 20-BSA). It was then washed three times for ten minutes each with 10 ml of PBS-Tween 20 (.05%) and incubated in alkaline phosphatase developing buffer (100 mM Tris, 100 mM Nacl, 5 mM MgCl2, pH 9.5 with nitro-blue tetrazolium and 5-bromo-4-chloro-3-indolyl phosphate). RESULTS Rhodamine Fluorescence Assays In the later developmental stages of Urechis caupo, the embryos develop cilia and become motile. To stop motility, I found that 37% formaldehyde immobilized the embryos, enabling a more accurate fluorescence reading. A control was performed to test the effects of formaldehyde on rhodamine fluorescence since formaldehyde kills the cells. The control showed that formaldehyde decreases rhodamine fluorescence by approximately 44% (Figure 4). Rhodamine fluorescence assays showed that an MXR mechanism is active in unfertilized eggs, two-cell and four-cell embryos, gastrulae, and two-day larvaes since the + verapamil ratio at each stage was 2.3 or greater. The average + verapamil ratio was 2.3 at the unfertilized stage, 3.7 at the 2-cell stage, 2.7 at the 4-cell stage, 3.3 at gastrulation, and 2.6 at the 2-day stage. The + verapamil ratios corrected for formaldehyde at gastrulation and the 2-day stage were 6.3 and 4.9 (Figure 5). Rhodamine fluorescence assays were performed on the coelomic and immature oocytes of three different Urechis females at two rhodamine concentrations, 5 uM and 1.0 uM and at 2.2 uM verapamil. At .5 uM rhodamine B, the first trial had coelomic oocyte diameters ranging from 33 to 127 microns. No apparent trend was observed between the +verapamil and -verapamil graphs, which overlapped at two points (Figure 6). The second trial at 5 uM rhodamine involved coelomic oocytes with diameters ranging from 47 to 140 microns. The +verapamil graph was slightly higher in fluorescence than the -verapamil graph at all diameter sizes (Figure 7). The third trial at 5 uM rhodamine included coelomic oocyte diameters ranging from 47 to 120 microns. This trial also showed no apparent pattern between the +verapamil and -verapamil graphs, which overlapped at four places (Figure 8). The immature oocytes incubated at 5 uM rhodamine from the second and third female exhibit MDR activity with + verapamil ratios of 1.7 and 1.9, respectively (Figure 9). At 1 uM rhodamine concentration, the coelomic oocytes from the first trial ranged in diameter size from 60 to 134 microns. No trend was observed between the +verapamil and -verapamil graphs, which overlapped in three places (Figure 10). For trial 2 at 1 uM rhodamine, the coelomic oocyte diameters ranged from 40 to 134 microns. The -verapamil graph is slightly higher in rhodamine fluorescence than the +verapamil graph for all oocyte diameters (Figure 11). Finally, the coelomic oocytes in the third trial at 1 uM rhodamine have diameters ranging from 33 to 127 microns. No apparent trend was seen between the +verapamil and - verapamil graphs, which overlapped in five places (Figure 12). The immature oocytes from the three female Urechis incubated in 1 uM rhodamine showed the following + verapamil ratios, respectively: 2.1, .87, and 1.9, indicating MDR activity in the first and third trials (Figure 13). Western blots were performed at the following stages of Urechis caupo: coelomic, 2-day, and gastrulation. All three stages showed a band at around 160 KD (Figure 14). DISCUSSION The + verapamil ratios of immature oocytes and also the embryos at the 2-cell, 4-cell, gastrula, and 2-day stages suggest that these cells possess MXR activity. Furthermore, the Western blot analysis shows that gastrulae and 2-day old embryos possess a protein of MW 160 kD that is labeled by a monoclonal antibody to the conserved ATP-binding region of the mammalian P-glycoprotein. These results indicate a multixenobiotic resistance mechanism similar to the MDR resistance in mammals is present in Urechis early embryos. The control performed on immature oocytes with and without formaldehyde indicates that formaldehyde does decrease rhodamine considerably. Another way of immobilizing the later ciliated stages of Urechis embryos should be found and used, preferably a way that does not damage the embryo. Mireles has found methyl cellulose to be an effective but harmless immobilizer for Urechis embryos (Mireles, personal communication). The rhodamine assays performed on the coelomic and immature oocytes from the same female show the absence of MXR activity in the coelomic oocytes but the presence of MXR activity in immature oocytes. In the first and third trials, assays with both .5 uM and 1.0 uM rhodamine B show no significant differences between the +verapamil and -verapamil graphs of the coelomic oocytes. These results indicate that verapamil does not inhibit the transport function of the MXR protein because the protein in coelomic oocytes is not yet active or simply not present. The rhodamine assays of the immature oocytes in the first and third trials at both rhodamine concentrations suggest MXR activity with + verapamil ratios of 1.7 or greater. The second trial of coelomic oocytes did not give as clear results as the first and third trials. At 5 uM rhodamine concentration, the +verapamil graph was always above the -verapamil graph. The + verapamil ratios between the two graphs never exceeded 1.3. These results suggest some MXR activity in the coelomic oocytes. One possible explanation for this is that this particular worm may have been stressed, having some MXR activity in its coelomic oocytes. In addition, + verapamil ratios from the coelomic oocytes were not as valid as those from the immature and fertilized oocytes because the +verapamil and -verapamil graphs involved coelomic oocytes of different sizes. During each rhodamine assay, finding coelomic oocytes of one particular size to measure their fluorescence was difficult so the + verapamil and -verapamil graphs did not always consist of the same-sized oocytes. Both coelomic and immature oocytes were saturated at 1 uM rhodamine but not at .5 uM rhodamine as indicated by the + verapamil ratio of 87 in the immature oocytes at 1 uM rhodamine and the +¬ verapamil ratio of 1.7 at 5 uM rhodamine. The former ratio is less than one, indicating that adding verapamil to 1 uM rhodamine made no difference in fluorescence, although verapamil enhanced fluorescence at 5 uM rhodamine. Therefore, the data from the second trial at 1 uM rhodamine should be disregarded due to oversaturation of the oocytes by rhodamine. Western blot analysis also shows that a 160 kD protein is present in coelomic oocytes. This result demonstrates the presence of a protein immunologically related to the mammalian P¬ glycoprotein. However, rhodamine fluorescence assays indicate a lack of MXR activity in coelomic oocytes, suggesting that the MXR protein is present but inactive in the coelomic oocytes. However, this protein is present and active in immature and fertilized oocytes. What then activates MXR in Urechis coelomic oocytes? One possible explanation is that the oocytes in the coelomic fluid undergo some kind of post-translational modification, specifically phosphorylation, before becoming immature oocytes in the storage organs. A past study has indicated approximately a 50% increase in MXR activity between unfertilized and fertilized Urechis oocytes 2(Toomey, personal communication). This increase in MXR activity at fertilization and the increase between coelomic and immature oocytes may be due to phosphorylation. Center showed that the mammalian P-glycoprotein transporting function can be modified by phosphorylation. An increase in P-glycoprotein phosphorylation produces a decrease in drug accumulation and an increased resistance to the drugs (Center, 1985). Both protein kinase C and cAMP-dependent protein kinase catalyze phosphorylation in MDR cells (Chambers et al., 1990; Ma et al., 1991; Miyamoto et al., 1990). Inhibitors to the two kinases such as staurosporine and H-7, respectively, decrease the drug efflux from the cell, whereas protein kinase C activators such as phorbol esters increase drug efflux (Ma et al., 1991; Miyamoto et al., 1990). To test if either kinase is involved in the MXR activity increases between coelomic and immature oocytes and/or immature and fertilized oocytes, further rhodamine assays should be conducted using staurosporine and H-7 as inhibitors at the more active stage. Environmental conditions of the oocytes may also influence their MXR activity. Coelomic, immature, and fertilized oocytes live in different media in nature. Coelomic oocytes develop in the coelomic fluid surrounded by erythrocytes and proteins. Immature oocytes are collected from the coelomic fluid and stored in storing organs. Finally, immature oocytes become fertilized in seawater where sperm can swim to them. These environments are different in many ways, one of which may be their pH. The coelomic oocytes may be activated by a change in pH. Furthermore, the different environmental conditions may serve as a trigger to phosphorylation. Coelomic oocytes reside within their mother, sheltered from any external hazards. Thus, the coelomic oocytes may not need yet to exert a self-defense mechanism. They can use the mother's defense mechanisms. In addition, the MXR protein binds to many hydrophobic substrates and transports them out of the cells. While still developing, the coelomic oocytes may need for certain hydrophobic compounds to be retained in the cell. Thus, MXR inactivity may be beneficial to the oocytes at their developing stages. Discovering why MXR activity is turned on as Urechis caupo oocytes mature can prove helpful in further understanding both MXR activity against pollutants in aquatic animals and MDR activity against anti-cancer drugs in tumor cells. If MDR activity can be turned off in tumor cells as it is in Urechis coelomic oocytes, then chemotherapy would become much more effective. In addition, further research on MXR may provide insight on its natural role in the cell. The transport function of the MXR protein is inherent in many marine organism, not requiring induction by pollutants or drugs(Kurelec, 1992). Also, the MXR protein exists and is taxonomically highly conserved across many species (Kurelec, 1992). This information implies that this mechanism has a role(s) that is important in the functioning of certain cells. One possible role may be to excrete natural toxic products in the diet or endogenous metabolites (Gottesman, 1988). Another role of P-glycoprotein in mammals may be to secrete progesterone and other steroids in mammalian adrenal cortex (Qian, 1990). Regardless of other possible roles, the MXR mechanism plays an important role in detoxifying cells in marine and terrestrial life. ACKNOWLEDGEMENTS I would like to thank the Epel lab for all the time, patience, and support given to me during my stay here at Hopkins Marine Station during this past quarter. Thank-you, Dave, for all the time and advice you gave me over the quarter. I really had fun and learned a lot during lab meeting and lunches. Thank-you, Barbara, for sharing with me your knowledge on Urechis, rhodamine assays, and Western blots. Thank-you, Beth, for sharing your lab bench with me, and also for your smiles in times of frustration. Thank-you, Paul, for sharing your insights on how to do things easier such as skating in the mud. Thank-you, Robin, for your help in the lab including showing me where things were hiding. Thank-you, Francois, for your interests and sense of humor in my project. Thank-you, Chris, for making us laugh in frustrated times, developing wonderful pictures, and making corny jokes about pre-meds. Thank-you, Molly, for being a great T.A., developing great slides, and for being a all-around wonderful person. Thank-you, Maria, for being my Urechis buddy and helping to dig me out of the mud. Finally, thank-you, Annie and Jenny, for being wonderful labmates as well as housemates and Esther, for being a great housemate. Without you all, my quarter would have been not the same. REFERENCES Center, M. S., Mechanisms regulating cell resistance to adriamycin: evidence that drug accumulation in resistant cells is modulated by phosphorylation of a plasma membrane glycoprotein. Biochemical Pharmacology, 34, 1471, 1985. Chambers, T. C., Chalikonda, I., and Eilon, G., Correlation of protein kinase C translocation , P-glycoprotein phosphorylation and reduced drug accumulation in in multidrug resistant human KB cells. Biochemical Biophysical Research Communications, 169, 253, 1990. Chen, C.-J., Chin, J. E., Ueda, K., Clark, D. P., Pastane, I., Gottesman, M. M., and Roninson, I. B., Internal duplication and homology with bacterial transport proteins in the mdrl (p-glycoprotein) gene from multidrug-resistant human cells. Cell, 47, 381, 1986. Gottesman, M. M., Pastan, I., The Multidrug Transporter, a Double¬ aged Sword. The Journal of Biological Chemistry. 263, 12163, 1988. Gould, M. C., RNA and Protein Synthesis in Eggs and Embryos of Urechis caupo. Stanford University, 1967. (dissertation) Gros, P., Croop, J., and Housman, D. E., Mammalian multidrug resistance gene: complete cDNA sequence indicates strong homology to bacterial transport proteins. Cell, 47, 371, 1986. Harper, K., The Relationship of MDR P-Glycoprotein and the Swelling Activated Chloride Channel. Stanford University, 1993. (Honors Thesis) Juliano, R. L. and Ling, V., A surface glycoprotein modulating drug permeability in Chinese hamster ovary cell mutants, Biochemical Biophysical Acta, 455, 152, 1976. Kurelec, B., The Multixenobiotic Resistance Mechanism in Aquatic Organisms. Critical Reviews in Toxicology. 22, 23, 1992. Ma, L., Marquardt, D., Takemoto, L., and Center, M. S., Analysis of P¬ glycoprotein phosphorylation in HL6O cells isolated for resistance to vincristine, Journal of Biological Chemistry, 266, 5593, 1991. Miller, J. H., Studies of Oogenesis in Urechis caupo: Method for Separating Different Size Classes of Oocytes. Developmental Biology, 32, 219, 1973. Mireles, M., Hopkins Marine Station, Stanford University, Pacific Grove, CA, personal communication. Miyamoto, K. I., Wakusawa, S., Nakamura, S., Koshiura, R., Otsuka, K., Naito, K., Hagiwara, M., and Hidaka, H., Circumvention of multidrug resistance in P388 murine leukemia cells by a novel inhibitor of cyclic AMP-dependent protein kinase, H-87, Cancer Lett., 51, 37, 1990. Morris R. H., Abbot, D. P., Haderlie, E. C., Intertidal Invertebrates of California. Stanford University Press., Stanford, 1980. Newby, W. W., The Embryology of the Echiuroid Worm Urechis caupo. The American Philosophical Society. Philadelphia, 1940. Neyfakh, A., Use of fluorescent dyes as molecular probes for the study of multidrug resistance, Experimental Cell Research, 174, 168, 1988. Qian, X., and Beck, W. T., Progesterone photoaffinity labels P- glycoprotein in multidrug-resistant human leukemic lymphoblasts, Journal of Biological Chemistry., 165, 18753, 1990. TToomey, B. H., Multixenobiotic transport in Urechis embryos: Protection from environmental toxins. Hopkins Marine Station, Stanford University, 1993. (unpublished) 2Toomey, B. H., Hopkins Marine Station, Stanford University, Pacific Grove, CA, personal communication. West, I.C., What determines the substrate specificity of the multidrug-resistance pump?, TIBS, 5, 42, 1990. FIGURE LEGENDS Figure 1. Mechanism of P-glycoprotein transport function. Moderately hydrophobic compounds diffuse into the cell. P¬ glycoprotein binds to the compounds and transports them out using ATP as its energy source. Figure 2. Anatomy of Urechis caupo. Immature gametes are stored in the storage organs ready to be spawned, and developing gametes are in the coelomic fluid. Oocytes do not reach full maturity until they are fertilized when they finish meiosis II. Figure 3. Spawning of Urechis caupo. A glass probe is inserted and gently rotated into one of six gonadopores. Extrusion of sperm (white) and eggs (pink, yellow, olive) follows. Figure 4. Effects of formaldehyde on rhodamine B fluorescence in U. caupo oocytes. Formaldehyde decreases rhodamine fluorescence by 44%. Figure 5. + Verapamil ratios of U. caupo oocytes at different stages incubated in 1 uM rhodamine B and 22 uM verapamil. Ratios corrected for formaldehyde are also shown. Figure 6. Trial 1: Coelomic oocytes in 5 uM rhodamine B and 2.2 uM verapamil. No apparent trend between +verapamil and -verapamil graphs. Figure 7. Trial 2: Coelomic Oocytes in 5 uM rhodamine B and 2.2 uM verapamil. +Verapamil graph is higher than -verapamil graph at all diameter sizes of oocytes. Figure 8. Trial 3: Coelomic oocytes in 5 uM rhodamine B and 2.2 uM verapamil. No apparent trend between the +verapamil and -verapamil graphs. Figure 9. + Verapamil ratio of immature oocytes incubated in .5 uM rhodamine B and 2.2 uM verapamil. Both trial 2 and trial 3 indicate MXR activity with + verapamil ratios of greater than 1.7 Figure 10. Trial 1: Coelomic oocytes in 1 uM rhodamine B and 2.2 uM verapamil. No apparent trend between the +verapamil and -verapamil graphs. Figure 11. Trial 2: Coelomic oocytes in 1 uM rhodamine B and 2.2 uM verapamil. -Verapamil graph is higher than the +verapamil graph at all diameter sizes of oocytes. Figure 12. Trial 3: Coelomic oocytes in 1 uM rhodamine B and 2.2 uM verapamil. No apparent trend between the +verapamil and -verapamil graphs. Figure 13. + Verapamil ratios of immature oocytes Incubated in 1 uM rhodamine B and 2.2 uM verapamil. Trial 1 and trial 3 indicate MDR activity with + verapamil ratios greater than 1.7. Figure 14. Western blot of the different development stages of Urechis caupo. A band at 160 kD is seen in coelomic oocytes, gastrula, and 2-day larvae. FIGURE 1 HYDROPHOBIC COMPOUND A AT 6 S P-GLYCOPROTEIN STORAGE ORGANS Immature Gametes 4 FIGURE 2 ANTERIOR COELOM Developing Gametes u POSTERIOR GONADOPORES FIGURE 3 MOUTH — — — — MV SETAE ANUS naehe lien Figure 4 0- mature 2-ce Figure 5 4-cell — gastrul. 2-day E CORRECTED □ OBSERVED Figure 6 10— 2 - kvv- — 0- 0.0 0.2 0.4 0.6 0.8 1.0 1.2 1.4 1.6 1.8 2.0 Size (1 un. = 66.7 microns) —— Ver —— 4Ver Figure 7 18 + 14 12 - k vkva- oaaa 0.0 0.2 0.4 0.6 0.8 1.0 1.2 1.4 1.6 1.8 2.0 2.2 2.4 2.6 2.8 3.0 Size (1 un. = 66.7 microns) — — -Ver —— 4Ver 30 - Figure 8 O 0.0 0.2 0.4 0.6 0.8 1.0 1.2 1.4 1.6 1.8 2.0 Size (1 un. = 66.7 microns) ——Ver —— 4Ver 2.5 2.0 1.0 0.5- 0.0 + Trial 2 Trial 3 Figure 9 Figure 10 60 50 A 30- 20 10 0 + — 0.0 0.2 0.4 0.6 0.8 1.0 1.2 1.4 1.6 1.8 2.0 2.2 Size (1 un. = 66.7 microns) ——Ver —— +Ver Figure 11 100 90 - 80 70 60 40 30 20 - 10 - O+ 0.0 0.2 0.4 0.6 0.8 1.0 1.2 1.4 1.6 1.8 2.0 2.2 2.4 2.6 2.8 3.0 Size (1 un. = 66.7 microns) ——Ver —— 4Ver Figure 12 p 70— 60 - 50 - 40 - 30 20 10 - O + 0.0 0.2 0.4 0.6 0.8 1.0 1.2 1.4 1.6 1.8 2.0 Size (1 un. = 66.7 microns) —Ver —— 4Ver 2.5 2.0 1.0 0.5 0.0 + Trial Figure 13 2 Trial 2 2 Trial 3 200 KD 97.4 KD 69 KD 46 KD 30 KD FIGURE 14 WESTERN BLOT: Different Development Stages of Urechis caupo