ABSTRACT Marine mussels Mytilus californianus and Mytilus edulis, hardy invertebrates resistant to pollution, were found to possess a multi¬ xenobiotic resistance mechanism analogous to multi-drug resistance (MDR) found in resistant mammalian tumor cell lines. This MDR-like efflux pump may provide defense against natural toxins in the aquatic environment. An assay using the fluorescent dye rhodamine B was adapted to measure MDR activity in Mytilus sp. gill tissue in vivo. Four pieces of evidence support the existence of a multi¬ xenobiotic resistance in Mytilus sp.: (1) accumulation of rhodamine B is sensitive to known inhibitors of MDR, such as verapamil; (2) verapamil inhibits an efflux pump; (3) Western blot analysis shows the presence of a protein immunologically related and similar in molecular weight to mammalian MDR P-glycoprotein; and (4) the Mytilus sp. efflux pump is sensitive to nanomolar concentrations of rhodamine B. MDR in Mytilus; Bard and Cornwall 199. INTRODUCTION Mussels (Mytilus sp.) are hardy organisms which are able to successfully colonize heavily polluted waters. This character suggests that these bivalves may possess a mechanism to resist the toxicity of the diverse array of compounds found in aquatic pollution. We have found in the marine mussels, Mytilus californianus and Mytilus edulis, a mechanism of toxin resistance similar to the multi¬ xenobiotic resistance found in the mussel Mytilus galloprovincialis by Kurelec and Pivcevic (1991), and analogous to the phenomenon of multi-drug resistance (MDR) found in mammalian tumor cell lines. MDR was first discovered in cancer patients undergoing chemotherapy who were found to become simultaneously insensitive to a wide range of structurally unrelated, cytotoxic drugs (Beck, 1987. Hofli and Nissen-Meyer, 1990). The clinical resistance to these drugs, marked by a decrease in drug accumulation within the tumor cells, was found to correspond to an increased expression of a 170 kD membrane P-glycoprotein (P-gp) (Pearce, 1990). The P-gp was later found to bind and export a wide array of compounds from the cell in an energy-dependent, saturable process (Pearce, 1990). Previous research has shown that certain drugs reverse the MDR activity in tumor cells (Hofsli and Nissen-Meyer, 1990). This observation has led to the discovery that certain compounds will competitively inhibit the efflux of other compounds from cells with P-glycoprotein. Hence the latter compounds will accumulate in the cell and, in effect, the cell is no longer resistant to them. Such MDR inhibitors include verapamil (Yusa and Tsuruo, 1989), forskolin MDR in Mytilus; Bard and Cornwall, 1992; 2 (Morris et al., 1991), quinidine (Cornwell et al., 1987), emetine (Samuelson et al., 1990), vinblastine (Tamai and Safa, 1991), and trifluoperazine (Cano-Gauci and Riordan, 1987), among many others. This competitive inhibition phenomenon has been used to detect MDR activity. Neyfakh (1988) found that multi-drug resistant tumor cells under normal conditions resisted staining by a number of fluorescent dyes. However, the cells accumulated high concentrations of the dyes in the presence of known inhibitors of MDR, such as verapamil, trifluoperazine, and weak detergents. This information was used to develop an assay to observe and characterize MDR-like activity: a marked increase in accumulation of rhodamine in the presence of MDR inhibitors, as measured by fluorescence microscopy, may signify the presence of an MDR-like mechanism. We modified this assay for our study of Mytilus sp., using epifluorescence microscopy to measure rhodamine B accumulation in single cells of intact Mytilus sp. gill tissue in vivo. The purpose of this study is to determine if the marine mussels Mytilus californianus and Mytilus edulis exhibit an efflux mechanism similar to the multi-drug resistance phenomenon described in mammalian tumor cells, and to determine if this mechanism could be effective against the low concentrations of toxins found in the aquatic environment. Four pieces of evidence suggest that the Mytilus possesses an MDR-like mechanism to efflux xenobiotics and avoid bioaccumulation of these toxins. First, accumulation of rhodamine B in the gill tissue is sensitive to known inhibitors of the MDR protein, such as MDR in Mytilus; Bard and Cornwall, 1992; 3 verapamil. Second, verapamil inhibits an efflux pump. Third, western blot analysis shows the presence of a protein immunologically related and similar in molecular weight to the mammalian MDR transport protein. Finally, the Mytilus sp. efflux pump is sensitive to nanomolar concentrations of rhodamine B. MATERIALS AND METHODS MDR ACTIVITY DETECTION ASSAYS MDR activity was measured in Mytilus sp. gill tissue. Gills were removed from freshly dissected Mytilus californianus and Mytilus edulis. The gills are comprised of four monolayer sheets of cells. Small (« 25 mm2), single cell layer tissue samples were cut from the dorsal and ventral rims of the medial layer of the gill. The gills of M. edulis had to be incubated in sea water for 10-15 minutes to flush out the large amounts of mucus. To assess MDR substrate competition, seven 5mL sea water solutions were prepared in 30mL beakers with 1 uM rhodamine B and one each of the following MDR-inhibiting drugs at the following concentrations: verapamil (22 uM), emetine (40 ug/mL), vinblastine (50ug/mL), forskolin (5 uM), trifluoperazine (22 uM), quinidine (22 UM), and sodium azide (10 mM). The control solution contained 1 MM rhodamine B only. Two tissue samples were incubated in each solution at 18-20 °C for one hour. The tissues were then removed from the incubation and swirled gently in 10-20 mL sea water for a MDR in Mytilus; Bard and Cornwall, 1992; 4 few seconds to remove excess rhodamine from interstitial spaces. The tissues were then placed, free-floating, in sea water in 5 mL petri dishes for examination. The rhodamine epifluorescence in individual cells in each tissue sample was observed with a 40X water-immersion lens on a Zeiss epifluorescence microscope. The intensity was measured by a light meter and recorded in volts by a digital multimeter. Measurements for each sample were completed in less than 10 minutes. In each tissue, 25-40 cells were measured, and means and standard deviations were computed. MDR ACTIVITY CHARACTERIZATION ASSAYS To assess rhodamine uptake over time, tissue samples were incubated in 5 mL of luM rhodamine/sea water solution with and without 22 uM verapamil for 0, 15, 30, 60, 90, and 120 minutes. The tissues were then rinsed and examined as described above. To assess rhodamine efflux over time, tissue samples were incubated for one hour in 1 uM rhodamine and were then placed in 5 mL sea water with and without 22 uM verapamil for 0, 15, 30, 60, 90, and 120 minutes. This protocol was repeated for tissue samples incubated for one hour in 2 uM rhodamine and 22 uM verapamil. Fluorescence measurements were made as described above. All sea water and solutions were kept at 18-20 °C, except during examination when the microscope light warmed the sea water dish. MDR in Mytilus; Bard and Cornwall, 1992; 5 WESTERN BLOTS Mytilus californianus gill tissue samples were tested by western blot analysis for the presence of a protein related to the mammalian MDR P-glycoprotein. Chopped samples of M. californianus gill tissue were homogenized in hypotonic lysis buffer (10 mM KCl, 1.5 mM MgCl2, 10mM Tris HCl, and 2 mM Phenylmethyl Sulfonyl Fluoride) and then sonicated in 5% SDS. Proteins from gill tissue samples and from human tumor K 562 R7 cells that overexpress the MDR P-glycoprotein were resolved on a 7.5% SDS polyacrylamide BioRad Mini-Protean II gel and transferred to nitrocellulose as described by Otter et al. (1987). The P-glycoprotein specific monoclonal antibody C219 from Centocor, the epitope sequence of which was determined by Georges et al. (1990), was used to locate the P-glycoprotein in the MDR-positive R7 cell and gill samples. The blots were developed by the alkaline phosphatase assay described by Mierendorf et al. (1987). SOURCES OF REAGENTS Rhodamine B, Quinidine HCl, and Vinblastine were from Sigma Chemical Company (St. Louis, MO); Verapamil HCl from Knoll Pharmaceutical Company (Whippany, NJ); Emetine HCl from K&K Laboratories, Inc. (Plainview, NY); 1,9-dideoxy Forskolin from Calbiochem (San Diego, CA); Trifluoperazine from Smith Kline and French Labs (Philadelphia, PA); and Sodium Azide from Fisher Scientific Company (Fair Lawn, NJ). MDR in Mytilus; Bard and Cornwall, 1992; 6 RESULTS RHODAMINE UPTAKE WITH AND WITHOUT VERAPAMIL We incubated M. californianus gill tissues in 1 uM rhodamine with and without 22 uM verapamil for 15, 30, 60, 90, and 120 minutes to characterize rhodamine accumulation over time. As seen in Figure 1, a much greater accumulation of rhodamine occurred in the tissues which were incubated in the presence of verapamil. With verapamil, the fluorescence appeared to level off after one hour in the solution at approximately a 500% higher level than the tissues in the absence of verapamil. Without verapamil, the fluorescence remained low, peaking at around 30 minutes, decreasing slightly, and levelling off after one hour. INHIBITION OF RHODAMINE ACCUMULATION BY OTHER DRUGS Since rhodamine accumulation levelled off after one hour of incubation, we tested the other competitive inhibitors by measuring rhodamine fluorescence at the 60 minute time point only. As seen in Figures 2 and 3, gill tissue samples from both Mytilus californianus and Mytilus edulis showed increased accumulation of rhodamine in the presence of known MDR competitive inhibitors: verapamil, vinblastine, trifluoperazine, emetine, quinidine, and forskolin. M. californianus tissue samples exposed to the drugs displayed increased fluorescence greater than 500% of the control with a maximum of 1700% in verapamil (see Figure 2). The M. edulis tissue MDR in Mytilus; Bard and Cornwall, 1992; 7 samples incubated in these drugs demonstrated fluorescence greater than 350% of the control with a maximum 440% with forskolin (see Figure 3). In similar rhodamine assays, tissues were incubated in the presence of sodium azide (data not shown), an electron transport chain blocker (Neyfakh, 1988), to test for the ATP dependence of the efflux mechanism. No significant increase in rhodamine accumulation was found in either species. RHODAMINE EFFLUX We next attempted to determine whether verapamil increased rhodamine accumulation by inhibiting an efflux pump. To examine efflux, we loaded tissues with fluorescent dye and then measured efflux in the presence of verapamil. M. californianus tissues were incubated in 1 uM rhodamine for one hour and then incubated in sea water with and without 22 uM verapamil for 30, 60, 90, and 120 minutes. As shown in Figure 4, the tissues incubated in plain sea water showed a decrease in fluorescence to slightly above natural fluorescence levels after about 30 minutes. However, tissues incubated in sea water containing 22 uM verapamil showed a much slower decrease in fluorescence, remaining over seven times higher than natural fluorescence at two hours. (See Figure 6) We also incubated tissues in 2 uM rhodamine and 22 uM verapamil for one hour, and then incubated them in sea water with and without 22 uM verapamil for 15, 30, 60, 90, and 120 minutes. Under these conditions, unlike the 1 uM rhodamine incubation, there MDR in Mytilus; Bard and Cornwall, 1992; 8 was no significant difference between rates of fluorescence decrease in the presence or absence of verapamil over two hours. (See Figure 5; see Discussion section for further explanation.) WESTERN BLOT We then tested for the presence of a protein related to the P- glycoprotein responsible for mammalian MDR. Western blot analysis of M. californianus gill tissue with the monoclonal antibody C219 revealed a single band, parallel to a 150 kD band from human tumor R7 cells which over express the MDR P-glycoprotein. (See Figure 6) RHODAMINE CONCENTRATION DEPENDENCE To determine the range of rhodamine concentrations over which activity of the efflux pump is detectable, we incubated M. californianus gill tissues in varying concentrations of rhodamine with and without 22 uM verapamil for one hour. As shown in Figure 8, there was no significant increase in rhodamine accumulation in the presence of verapamil at 2.5 uM rhodamine. Likewise, we found no difference in rhodamine accumulation with and without verapamil at 0.1 nM rhodamine, as shown in Figure 7. However, between 1 nM and 2uM rhodamine, there was at least a 100%, and up to a 500%, increase in rhodamine accumulation in the presence of verapamil, suggesting the presence of MDR-like activity. (See Figure 7) MDR in Mytilus; Bard and Cornwall, 1992; 9 MDR-LIKE ACTIVITY IN OTHER ORGANISMS A preliminary survey of MDR-like activity in other marine organisms was conducted. Eggs of the sand crab Emerita analoga and the solitary tunicate Ascidia ceratodes exhibited a 200% increase in rhodamine accumulation in the presence of verapamil. No increase in rhodamine accumulation on addition of verapamil was detected in eggs of the following species, Aplysia californica (sea hare), Patiria miniata (bat star), and Pisaster ochraceus (purple sea star). Eggs of Parastichopus parvimenesis (California sea cucumber) were incubated in rhodamine solutions containing verapamil, emetine, trifluoperazine, quinidine, sodium azide and forskolin. Rhodamine accumulation in the presence of these drugs was 20% and 40% below that of the control. We found no evidence for the MDR P-glycoprotein on the Western blot for any of the aforementioned species (all tested except Aplysia eggs). DISCUSSION From the results of the rhodamine assays and Western Blot analysis, we conclude that the marine mussels, Mytilus californianus and Mytilus edulis, possess an MDR-like mechanism which may provide defense against toxins in the aquatic environment. MDR in Mytilus; Bard and Cornwall, 1992; 10 COMPETITIVE INHIBITION ASSAYS The first piece of evidence is the enhanced accumulation of rhodamine B in the presence of MDR inhibitors such as verapamil. Rhodamine accumulation in sea water is low, but in the presence of verapamil, intracellular rhodamine content increases to over 800% of control. Since the concentration of verapamil in the incubation is much higher than that of rhodamine (11-22,000 -fold), verapamil competes successfully for binding sites on the P-glycoprotein. Therefore, verapamil is effluxed and rhodamine B is allowed to accumulate within the cells. The same result is found with the inhibitors vinblastine, trifluoperazine, emetine, quinidine, forskolin as shown for Mytilus californianus in Figure 2, and Mytilus edulis in Figure 3. ATP-DEPENDENCE We found that the metabolic inhibitor, NaAz did not inhibit MDR activity in Mytilus, although mammalian MDR has been found to be energy dependent (Horio et al, 1988). NaAz prevents reduction of cytochrome oxidase, thereby blocking the electron transport chain and the production of ATP via aerobic metabolism. Bivalves such as M. edulis are able to function under anaerobic conditions for several days producing over 60% of the ATP produced under normal conditions (de Zwaan and Wijsman, 1975). This ability would allow the MDR efflux pump to continue functioning and would account for MDR in Mytilus; Bard and Cornwall, 1992; 11 the low intracellular rhodamine concentration in the presence of NaAz. VERAPAMIL INHIBITS AN EFFLUX PUMP We found that verapamil enhances rhodamine accumulation by inhibiting an efflux pump. When tissues were incubated in a low concentration of rhodamine and then placed in sea water, verapamil significantly slowed the rate of rhodamine efflux. Suppose, as in Figure 9, that in sea water a concentration gradient and an efflux pump together decrease intracellular rhodamine concentration. the efflux pump is inhibited one would expect a slower rate of decrease of intracellular rhodamine, as seen in Figure 4. However, at high initial intracellular rhodamine concentrations, we see no decrease in rhodamine efflux rate in the presence of verapamil. The higher intracellular rhodamine concentration increases the concentration gradient when the tissues are placed in the sea water. Thus the concentration gradient provides a much larger fraction of the total efflux force than it does at low concentrations. Since the pump then represents only a very small fraction of the total efflux force, we can see no difference in efflux rate when the pump is inhibited. (See Figure 10) WESTERN BLOT ANALYSIS We employed western blot analysis to detect a protein in the M. californianus gill related to the P-glycoprotein found in resistant MDR in Mytilus; Bard and Cornwall, 1992; 12 mammalian tumor cells. The MDR-specific monoclonal antibody C219 (Georges et al., 1990) indicated a single band of similar molecular weight (about 150 KD) as a band resolved from a sample of tumor cells that over-express the MDR phenotype. (See Figure 6) From these results we conclude that the MDR-like activity in M. californianus involves a P-glycoprotein related mechanism. RHODAMINE CONCENTRATION DEPENDENCE Finally, we found that this MDR-like efflux pump is sensitive to extremely low concentrations of rhodamine. At 1 nM extracellular rhodamine, we were able to detect a 100% increase in rhodamine accumulation in the presence of verapamil. This result suggests that the MDR-like efflux pump is sensitive to very low concentrations of substrate. Thus, even though most toxins in the aquatic environment are found at nanomolar concentrations, the Mytilus efflux pump would be able to effectively prevent their accumulation. However, at extremely low concentrations (1 pM), virtually no rhodamine was accumulated either with or without the presence of verapamil. Also, at rhodamine concentrations above 2uM, we were unable to detect a significant increase in accumulation in the presence of verapamil. (See Figure 8) At such high extracellular concentrations, the inward diffusion may be so great that the fraction of influxed rhodamine exported by the saturable efflux pump is unresolvable by our assay, as depicted in Figure 10. . MDR in Mytilus; Bard and Cornwall, 1992; 13 „ CONCLUSION From the results of this study, we conclude that the marine mussels, Mytilus californianus and Mytilus edulis, possess a toxin efflux mechanism analogous to the multi-drug resistance described in mammalian tumor cells. Furthermore, since this efflux mechanism is sensitive to nanomolar concentrations of substrate, it may provide effective defense against natural toxins found in the marine environment. MDR in Mytilus; Bard and Co ACKNOWLEDGEMENTS We would like to express sincere gratitude to Dr. David Epel, Barbara HollandiToomey, Dr. Rob Sweezy, Paul Sund, and Chris Patton for the laboratories, knowledge, guidance, and enthusiasm; and the faculty and staff of Hopkins Marine Station and the other students of Biology 175H who provided us with an exhilarating introduction to marine biology research. We also wish to express our gratitude for a variety of loans, grants, scholarships, and work-study jobs from the Stanford University Financial Aid Office. MDR in Mytilus; Bard and Corny REFERENCES Bard, Shannon. The Effects of Pulp and Paper Mill Effluent on the Marine Environment. The State of the Strait: Proceedings of a Conference on the Health of Georgia Strait, 1991. B.C.: Quadra Printers Ltd., 1991. Beck, W.T. The cell biology of multiple drug resistance.1987. Biochemical Pharmacology. Vol.36, No. 18, pp.2879-2887. Cornwell, M. et al. Certain calcium channel blockers bind specifically to multidrug-resistant human KB carcinoma membrane vesicles and inhibit drug binding to P-glycoprotein. 1987. The Journal of Biological Chemistry. Vol. 262, No. 5. pp. 2166-2170. De Zwaan, A. and Wijsman, T.C.M. Review. Anaerobic metabolism in bivalvia (Mollusca). Characteristics of anaerobic metabolism. 1976. Comp. Biochem. Physiol. 1976. Vol. 54B. pp.313-324. Georges, E. et al. Detection of P-glycoprotein isoforms by gene specific monoclonal antibodies. 1990. Proc. Natl. Acad. Sci. U.S.A., 87: pp.152-156. Hofsli, Eva and Jon Nissen-Meyer. Reversal of Multidrug Resistance by Lipophilic Drugs. 1990. Cancer Research. 50, 3997-4002. Horio, M., M.M. Gottesman, and I. Pastar, 1988. ATP-dependent MDR in Mytilus; Bard and Cornwall, 1992; 16 transport of vinblastine in vesicles from human multi-drug resistant cells. Proc. Natl. Acad. Sci. U.S.A. 85, 3580-3584. Kessel, David et al. Characterization of multidrug resistance by fluorescent dyes. 1991. Cancer Research. 51, pp 4665-4670. Kurelec, B. and B. Pivcevic. Distinct Glutathione-dependent Enzyme Activities and a Verapamil-sensitive Binding of Xenobiotics in a Fresh-water Mussel Anodonta cygnea. (1989) Biochem. Biophys. Res. Comm. Vol.164, No. 2, pp.934-940. Kurelec, B. and B. Pivcevic. Evidence for a multi-xenobiotic resistance mechanism in the mussel Mytilus galloprovincialis. (1991) Aquatic Toxicology. 453, ppl-11. Mierendorf et al. Gene isolation by screening lambda GTII libraries with Ab's. 1987. Methods in Enz. 152: pp. 458-467. Morris et al. Interaction of Forskolin with the P-Glycoprotein Multidrug Transporter. 1991. Biochemistry. 30: pp. 8371- 8379. Neyfakh, Alexander. Use of fluorescent dyes as molecular probes for the study of multidrug resistance. 1988. Experimental Cell Research. 174, pp168-176. Otter, T. et al. A two-step procedure for efficient transfer of both MDR in Mytilus; Bard and Cornwall, 1992; 17 high mol. wght. (S400,000) and low MW («20,000) proteins. 1987. Anal. Biochem. 162: pp. 370-377. Pearce, H.L. et al. Structural characteristics of compounds that modulate P-glycoprotein-associated multidrug resistance. 1990. Adv. Enz. Reg. 301. pp357-373. Samuelson et al. Emetine-resistant mutants of Entamoeba histolytica overexpress mRNAs for multidrug resistance. 1990. Molecular and Biochemical Parasitology. 38: pp. 281-290. Tamai, I. and Safa, A. Azidopine noncompetitively interacts with vinblastine and cyclosporin A binding to P-glycoprotine in multidrug resistant cells. 1991. The Journal of Biological Chemistry. Vol. 266, No. 25, pp. 16796-16800. Yusa, K. and Tsuruo, T. Reversal mechanism of multidrug resistance by verapamil: Direct binding of verapamil to P-glycoprotein on specific sites and transport of verapamil outward across the plasma membrane of K562/ADM cells. 1989. Cancer Research. 49, pp. 5002-5006. MDR in Mytilus; Bard and Cornwall, 1992; 1 FIGURE LEGENDS Eigure 1 Rhodamine uptake kinetics. Verapamil enhances rhodamine accumulation. Tissue samples were incubated in 1 UM rhodamine with and without 22 uM verapamil for varying lengths of time. Percent increases are indicated above each point. Figure 2. Competitive inhibition by MDR inhibitors. MDR inhibitors enhance rhodamine accumulation. Mytilus californianus gill tissues were incubated for one hour in 1 uM rhodamine with and without known MDR competitive inhibitors: verapamil, trifluoperazine, emetine, forskolin, quinidine, and vinblastine. Fluorescence values are represented as percentages of control fluorescence (without inhibitors = 100%). Eigure 3. Competitive inhibition by MDR inhibitors. MDR inhibitors enhance rhodamine accumulation. Mytilus edulis gill tissues were incubated for one hour in 1 uM rhodamine with and without known MDR competitive inhibitors: verapamil, trifluoperazine, emetine, forskolin, quinidine, and vinblastine. Fluorescence values are represented as percentages of control fluorescence (without inhibitors = 100%). Eigure 4. Rhodamine efflux. Verapamil inhibits an efflux pump. Mytilus californianus gill tissues were incubated in 1 uM rhodamine for one hour and then placed in sea water with and without MDR in Mytilus; Bard and Cornwall, 1992; 19 verapamil for varying lengths of time. Time = 0 represents placement into the sea water rinses. Data reported as mean fluorescences with standard deviations. Percent differences are indicated above each point. Eigure 5. Rhodamine efflux. High rhodamine concentrations mask inhibition of efflux pump. Mytilus californianus gill tissues were incubated in 2 uM rhodamine with 22 UM verapamil, and then placed in sea water with and without 22 uM verapamil. Time = 0 represents placement into the sea water rinses. Data reported as mean fluorescences with standard deviations. Eigure 6. Western Blot. MDR-related protein found in Mytilus gill. Single band in lane six represents P-glycoprotein from human tumor R7 cells that over-express the MDR phenotype. Single band in lane two represents protein found in sample found in Mytilus californianus gill tissue. Proteins traveled toward bottom of page. Figure 7. Rhodamine concentration dependence. MDR activity found at 1 nM rhodamine. Mytilus californianus gill tissues were incubated for one hour in low, varying concentrations of rhodamine with and without 22 UM verapamil. Fluorescence represented as raw data. Data reported as mean fluorescences with standard deviations. Percent differences are indicated above each point. Figure 8. Rhodamine concentration dependence. MDR activity is unresolvable above 2.0 uM rhodamine. Mytilus californianus gill MDR in Mytilus; Bard and Cornwall, 1992; 20 tissues were incubated for one hour in high, varying concentrations of rhodamine with and without 22 uM verapamil. Fluorescence represented as raw data. Data reported as mean fluorescences with standard deviations. Percent differences are indicated above each point. Eigure 9. Efflux pump inhibition model. (a) Under normal conditions, diffusion and an efflux pump work together to decrease intracellulai rhodamine concentration. (b) With the efflux pump inhibited, as in the presence of verapamil, diffusion is the only major force driving the rhodamine out, so intracellular rhodamine concentration decreases at a slower rate. Eigure 10. Problems with high rhodamine concentrations. (a) When rhodamine diffusion and MDR efflux are on the same order of magnitude, the inhibition of the efflux pump is noticeable. (b) When the original rhodamine concentration is increased and verapamil is added, the initial (Time = 0) intracellular rhodamine concentration is greatly increased. Thus the concentration gradient driving rhodamine out of the cells in the rinse is on a higher order of magnitude than the MDR efflux pump. Therefore, inhibition of the efflux pump is not as noticeable. MDR in Mytilus; Bard and Cornwall, 1992; 21 L L L 1 O— —0— +-0 —0— O- 03 — 1 JONSOSO ANIWVGoHa 8 I L L Q + + — JONOSaOn ANINVGOHA TOAINO JO INa — Eu : 2 Z oo 2 o2 E 5u I 2 L L 2 — 7u. ZI Ov Zu. Zu 2 OLi —— t- — * JONSOSOT ANINVGOHA OAINO O INa L L d. -O O JONOSOnI ANINVdOHa 8 ON 8 8 L 2 1 Oe —O-+0— 100— — — +O—++0++ o JONSOSSOTA ANINVdOHA 8 6 Figure 6. WESTERN BLOT a- 170 KD 3 12 JONOSORT ANINVGOHA O L L O 0 E E + JONSOSO ININVdOHA S (a) (b) Figure 9. EFFLUX PUMP INHIBITION MODEL WITHOUT VERAPAMIL USION EFFLUX PUMP WITH VERAPAMIL DIFFUSION EFFLUX PUMP W. Figure 10. PRÖBLEMS WITH HIGH RHODAMINE CONCENTRATIONS (a) USION EFFLUX PUMP total efflux force: diffusion only: (b) DIFFUSION EFFLUX PUMP total efflux force: diffusion only: