C O THE KINETICS OF DDT RESIDUES IN THE NUDIBRANCH HERMISSENDA CRASSICORNIS Ronald E. Marian Hopkins Marine Station of Stanford University The accumulation of DDT residues 'in higher trophic levels by magnification through the food chain is now well documented. However, the mechanisms for accumulation at the species level are not fully understood. There is presently no full account of the kinetics of DDT residues in a marine invertebrate. This report describes some aspects of DDT flow in the nudibranch Hermissenda crassicornis (Escholtz). A preliminary investigation indicated that a Hermissenda of any age will have been exposed to more DDT residues, available through feeding and surface uptake, than is reflected in the total body burden. This suggests a considerable turnover of the pesticide, either by a high rate of loss or by a physical equlibrium between tissue concentration and input dosage. Equilibria establishing a constant DDT residue concentration have (2,3,4) The been suggested in a variety of vertebrate systems. problem presented is one of establishing the pathways for DDi residue flow and their relative contributions in determining the amount of DDT residues in the animal. This problem is approached with a) the determination of field levels and the relation of DDT residue concentration to age, b) measurement of uptake by surface adsorption and feeding, c) measurement of losses of DDT residues, and d) an attempt to relate this information to what may be happening under natural conditions. DDT Residue Levels in Hermissenda Hermissenda for this study were collected subtidally from the pilings of Wharf No. 2 in the harbor of Monterey, California during the spring and summer. To determine the DDT residue levels in various sized specimens, a number of the animals were divided 59 into weight classes. Approximately 3 gram samples of each weight class were digested over steam by a l:l mixture of glacial acetic and perchloric acid, and the non-polar fraction extracted with The extracts were cleaned up using silica gel micro¬ hexane. 27 The concentrated samples were analyzed with a Beckman columns. (6) GC-4 gas chromatograph equipped with electron-capture detector Glassware for GLC analysis was combusted overnight at 400 C to remove any DDT contamination. The results, presented in Figure 1, show a definite increase in the total-body DDT residue concentration with increasing size. Since several specimens in the higher weight class samples contained spawn, possible accounting for the higher concentration, egg masses were collected and analyzed. Measured levels were too low for accurate quantification- less than 2 PPB (parts per billion). Another possibility for the higher concentration in larger animals would be a larger percentage content of lipid. To check this, Hermissenda of a full size range were weighed, dried and re-weighed, digested in the acid mixture, and extracted with ethanol and petroleum ether. The extracts were evaporated until no ether odor was detectable, and the residue weighed. The results (Eig. 2) show a constant percentage of ether-extractable lipids independent of size. This does not entirely rule out the possibility of a relatively higher number of DDT residue accumulation sites in the larger animals, since DDT residue storage might depend on the character and distribution of lipids as well as amount. Though size increases with age, the relation is unlikely to be linear. The growth curve in Hermissenda probably begins to flatten out around 0.8 grams weight as they begin to divert 360 3. food energy into spawn production. Eggs at the time of release accounted for 30% of the wet weight of a 0.78 gram specimen, and 18% of a 1.0 gram specimen. If the data in Figure l is to be considered in terms of DDT residue concentration vs. age, the weight scale would then be compressed at the lower end, resulting in somewhat straighter curves. Uptake of DDT From Seawater Measurement of surface uptake of DDT from water was accomplished using ring-labelled C+ DDT as a tracer. Hermissenda were held in closed one-gallon glass jars with 3 liters of unfiltered seawater containing the CDDT. The jars were kept in dim light at a constant 15° C. Before the addition of the animal, the jars were allowed to stand for 24 hours in order to allow the DDT to adsorb to equilibrium with the glass surface. To maintain a fairly constant concentration of DDT in the water and prevent stagnation, the water was changed daily. With animals present, the decrease of CDDT concentration over 24 hours ranged from 20% for an initial 30 PPT (parts per trillion) to 50% for an initial 5 PPT. Consequently, in order to obtain average concentrations of 5. 10. 20, and 30 PPT, the initial concentrations were prepared at 7. 12, 23, and 33 PPT. Each day, before being moved to fresh water, the Hermissenda were allowed to feed on Obelia. Uptake with time was measured by periodic sampling of a few of the animals cerata, dorsal extensions of the body wall containing diverticula of the digestive gland. Comprising on the average 36% of the body dry weight, the cerata contain 95% of the animals' total DDTüresidues. Cerata samples were digested in tha acid mixture and extracted with hexane. Sample activities were counted 36/ in a Nuclear Chicago Unilux II liquid scintillation counter." Curves of the accumulation of CDDT in the cerata for the four water concentrations are shown in Figure 3. Points represent data from several runs, and concentrations are based primarily on wet weights, with dry weight concentrations set to the same scale by a wet/dry conversion factor of 12.15. While the uptake curves level off after 2-3 days for animals in water of 5 and 10 PPT CDDT, the curves for the higher concentrations do not level off at the same time or at proportionate values. Two possibilities accounting for this are: (i) an equilibrium between the total DDT concentration in the cerata and the con- centration in the water, with an increasin equilibrium constant for higher water concentrations, and (ii) an uptake pathway consisting of two consecutive steps or compartments, with the first compartment establishing an equilibrium DDT concentration when the concentration in the water is around 5-10 PPT. With some sort of limit on the DDT capacity of the first compartment, higher concentrations in the water result in an overflow into the second compartment where the DDT is continuously accumulated. An additional experiment lends support to the latter possibility: Two Hermissenda were first exposed to water with 30 and 60 PPT of unlabelled DDT for 60 hours, and then placed in water containing 5 and 10 PPT respectively of CDDT. The uptake curves of the labelled DDT (Figure 4) are very similar to those in the previous experiment, despite the initial period of uptake from a six times higher concentration in the water. This suggests that the cerata uptake curves resulting from DDT water concentrations of 5 and 10 PPT represent a turnover of a certain portion of the DDT in the Soa cerata, independent of the total amount present. Again, this might be explained by an "equilibrium compartment" and a "storage compartment" An earlier experiment in which the concentration of DDT in the water was continuously measured may also support this theory. As shown in Figure 5, as the DDT concentration in the water drops below 10 PPT, the curve for Hermissenda uptake (the entire animal in this case) begins to follow fluctuations in the water concentration curve, even DDT from the animal when the concentration showing a loss of the drops below 5 PPT. There is also basis for this theory in the strucure of the cerata themselves, since they consist of an outer layer of body wall tissue and a core of digestive gland tissue- with not neccessarily the same DDT affinities. DDT Uptake Through Feeding Hermissenda crassicornis is reported as primarily a non- specific hydroid feeder.0 Animals in this study accepted a variety of genera including Obelia, Aglaophenia, Sertularia, Eucopella, and Syncoryne. The hydroid appearing to be the primary food source on the wharf pilings was Obelia dichotoma. However, they were also observed to feed occasionally on the bryozoan Bowerbankia, on a small species of Dendronotus abundant on the Obelia, and readily on dead or disabled fellow Hermissenda. Original measurement of DDT residues in Obelia gave a value of approximately 15 PPB wet weight. However, these samples were collected from the sides of floating piers, presumably being exposed to higher levels of contaminants from surface fallout, and also consisted of entire stolons with some inseparable non- hydroid material. When the hydroid population on the submerged 36. pilings became abundant in the early summer, a number of samples were collected consisting of only the younger portion of the stolons, selectively grazed by Hermissenda. Very low levels of DDT residues were found, again precluding accurate quanti¬ fication, but appearing to be less than 1 PPB wet weight. To determine the general distribution of ingested DDT, 14 small Hermissenda were fed the chopped-up bodies of Hermissenda labelled with CDDT. The animals were placed in a flask of DDT-free seawater for 48 hours and then dissected into pooled samples of cerata, total viscera, and remainder of the body- consisting of the muscular foot and head. Of the C recovered from the bodies, 83.7% was in the cerata, 8.7% in the viscera, and 5.6% in the remainder. Feces were also collected from the flask and accounted for 3.9% of the total label recovered. Analysis of the water in the flask during the 48 hours showed no measurable increase, although a significant total amount in the two liters could have been undetected in the 8 ml aliquots sampled. Possible adsorption to the glass surface was not measured. Thus the value of 96% for the efficiency of retention of DDT from food is probably high. Being rather small, few of these specimens contained spawn. In order to check for accumulation in eggs and the accumulation in the cerata with time, a single 0.8 gram Hermissenda was allowed to feed continuously on Obelia labelled to a concentration of 7 PPB CDDT. Eggs were released during the 9th and 10th days, coinciding with a marked increase in the cerata concentration (Figure 9). At the time of the third sampling, the total amount of CDDT in the Hermissenda was calculated as 300 picograms, a 368 and the total recovered from the eggs was 285 picograms, meaning that during the first week 49% of the DDT retained in the animal accumulated in the eggs, and that once eliminated as an accumulations site, nearly all the DDT taken in was then accumulated in the cerata. The important role of egg production in DDT residue flow also became evident in a comparison of the pathways for DDT loss. Losses of DDT Following Surface Uptake Four Hermissenda of nearly equal size were held in seawater containing 40 PPT C DDT for a period of 48 hours. Each was then placed in a stoppered 2 liter flask containing DDT-free water. At one to two day intervals the animals were removed, sampled for concentration in the cerata, and returned to a fresh flask of water. DDT lost from the animal was recovered by shaking the entire contents of the flask with three washes of petroleum ether. On the first day feces were collected and analyzed separately and found to account for a mean of 8% of the C“ DDT recovered from the flasks. Feces collection was difficult due to rapid disintegration, and thereafter feces were extracted along with the rest of the flask contents. Large egg masses were deposited by all four animal during the first day. Smaller batches were released 12 to 14 days later. The concentration of CDDT in the cerata over the two weeks of the experiment is shown in Figure 6. There is no clear explanation for the fluctuation excpt to note that changes in the concentration might be due either to transfer of DDT between the cerata and the body, or to changes in the wet weight 165 of the cerata. It may also be noted that large decrease in concentration coincided with the release of the second batch of eggs, though the absolute amount of C+ DDT represented by the drop was not reflected in either the amount recovered from the eggs or from other losses. 1 recovered from the flasks presumably included all DDT contained in the water, feces, mucustrails, and adsorbed to the glass. Results are shown in Figure 7 in terms of the rate of loss from the animals. No correlation between rate of loss and concentration in cerata was found. The DDT contained in the eggs accounted for 28% of the total taken up and 73% of the total lost (Figure 8). The small amount of DDT in the second eggs indicates that though the eggs accumulate a sizable portion of the DDT as it is taken up, they cannot accumulate much of the DDT already stored elsewhere in the animal. DDT Residue Flow in Hermissenda Under Natural Conditions The major problem in describing the situation in the field is in predicting the actual input dosages. Data presented here has indicated that long-term uptake of DDT residues from water may be very slight or very great, depending on the ambient concentration. Estimates of DDT residue levels in inshore waters of the Pacific coast are in the range of a few parts per trillion.9) The harbor of Monterey acts as a catch-basin for the southern end of Monterey Bay, and would be expected to have higher than average levels of pesticide contaminants. Jog An estimate of between 5 and 15 PPT seems reasonable, and it would thus be likely that surface uptake in Hermissenda is either in equilibrium or accounts for a very slow accumulation. The question of effective food input dosage is complex and unclear. Hermissenda is a rapidly growing organism, with the amount of food being utilized for new tissue prodction probably far greater than that required for metabolic maintenance. If the rate of tissue production- including DDT accumulation sites- were to remain constant as were the feeding rate, then a constant residue concentration might be maintained. However, in three Opisthobranchs whose nutrition has been studied, the efficiency of conversion of food into new tissue and spawn decreases with age. Since the efficiency of removal of DDT residues from food would seem independent of the efficiency of food utilization, this suggests an increasing dosage from food in relation to the production of new storage sites. Thus a higher concentration of residues in older animals might reflect an equilibrium between tissue content and increasing dosage, as well as a continual accumulation from a constant dosage. Two other factors are probably operating to confuse the issue: First, once Hermissenda reach sexual maturity, a portion of the DDT residue input is accumulated and eliminated in the spawn, thus periodically reducing the dosage to the rest of the body. Secondly, the dosage may vary as a result of a possible change in feeding habits eith age. Smaller Hermissenda were almost always found on a hydroid-bryozoan substrate, while larger ones were observed as often on colonies of Amaroucium. The largest specimens were consistently found on the muddy bottom among the fallout around the bases of the pilings. J67 10. Summary Results show an equilibrium for surface uptake, estab- lishing a constant DDT concentration in the cerata with a 5 to 10 PPT concentration in the water, a level likely to be present in the habitat. A two compartment model is pro- posed for the uptake mechanism. Spawning is shown to be the primary pathway for DDT output, eliminating as much as 50% of the residues taken up during each 10 to 20 day egg pro- duction period, but not eliminating DDT residues already stored in the cerata. Field levels show an increasing whole- body concentration with increasing age, probably dependent on feeding dosage, but difficult to determine without additional autecological knowledge of Hermissenda. 360 References and Notes 1. DDT residues include technical DDT and all it's non-polar metabolites. In this study, only p,p'DDT 1,1,1-trichloro- 2,2-bis(p-chlorophenyl)ethane, p,p'DDD 1,1-dichloro-2,2- bis(p-chlorophenyl)ethane, and p,p DDE 1,1-dichloro-2,2- bis(p-chlorophenyl)ethylene were detected and measured. 2. J. Robinson, A. Richardson, A. N. Crabtree, J. C. Coulson, and G. R. Potts, Nature 214 (5095): 1307-1311 (1967). 3. J. J. Jeffries and C. H. Walker, Nature 212: 533-534 (1966). J. W. Gillett, Bull. Environ. Contam. Toxicol. 4 (3) 159- 168 (1969). 5. A.M. Kadoum, Bull. Environ. Contam. Toxicol. 3, 65 (1968). Column coating was 5% mixed bed of DC-200 and QF-1 on Chromosorb W. All GLC parameters were those suggested in Pesticide Analytical Manual (U.S. Dept. of Health, Education and Welfare, Food and Drug Admin., revised 1968) vol.2. 7. Extracts were evaporated to.5 ml in scintillation vials, and 10 mls of scintillation fluid was added consisting of 4 grams PPO and .1 gran POPOP per liter toluene. 8. L. H. Hyman, The Invertebrates,vol VI Mollusca I (McGraw Hill, New York, 1967) 9. J. L. Cox, Ph.D. Thesis, Stanford University,1970. 10. T. H. Carefoot, Comp. Biochem. Physiol. 21, 627-652 (1967). 367 C C Acknowledgements I thank Mr. Robin Burnett for his patient assistance. This study was supported by NSF grant GY 8950 O O Fig. 1 Concentrations of DDT residues in Hermissenda of varying size. Concentrations are expressed as weight of residue per unit wet weight Hermissenda. Points are plotted at the mean weight per animal in the pooled samples representing each.2 gram size class. 100 80 60 50 30 FIGURE 1 TOTAL * * D 8 1 0 u. . DDT 3— X15 Xx— 2 4 .6 .8 10 1.2 14 1.6 1.8 GRAMS WET WEIGHT 37. O Fig. 2 Ether-extractable lipid content, expressed as percentage dry weight, of Hermissenda of varying size. O C Q L 0 O 0 0 9 Gid Naod 71 O Fig. 3 Increases in the concentration of CDDT with time in the cerata of Hermissenda during uptake from seawater containing 5, 10, 20, and 30 parts per trillion of the CDDT. Data is from several runs under the same conditions, with animals of the same approximate size. Concentrations are based on both wet and dry weights. 8 8 288 OeX 8 4 X 8 Noria dad siavd 40 . * S .00 0 90 o O 1 37 Fig. 4 Uptake in the cerata from water containing 5 and 10 PPT C"'DDT after an initial 60 hour exposure to water with 30 and 60 PPT unlabelled DDT. The broken lines are the predicted uptake curves based on data of Fig. 3. 0 0 00 60 o O0 00 o o 5 0 V O 8 8 Noug ad sLävd 5 70 O Fig. 5 Increase of total-body concentration of CDDT in Hermissenda exposed to 20 liters of seawater with varying concentration of CDDT. 95 • . ../. * * 0 11 S 9 —Q 10 8 &a 8 (alVN) Noralad sive (YGNASSIWNSH) Nortis asa siävd o0 O/0 O 3 00 8 0 380 O Fig. 6 Uptake of C DDT in the cerata of a.8 gram Hermissenda allowed to feed constantly on Obelia labelled to 7 PPB. Spawning occured on the 9th and 10th days. D6 FIGURE 6 —5 EGGS DEPOSITED — DAYS 10 30 C O Concentration of CDDT in the cerata of Fig. 7 four Hermissenda during the ten days following a 48 hour exposere to the labelled DDT. Values are based on wet weight only. 30 50 30 20 10 A 0 100 5 X O -—- HOURS FIGURE 7 . 200 300 38 Fig. 8 Rates of loss of CDDT from the four Hermissenda, expressed in grams of C DDT lost per hour. Rates were determined by the measurement of label recovered from the flasks in which they were maintained. 8 90 80 70 5 60 50 40 30 20 FIGURE 8 885 8 300 400 200 HOURS O 8 50 100 386 C Diagram representing the relative amounts Fig. 9 of CDDT lost by the four Hermissenda after initial uptake from water. 387 V101 j0 Nod 9 S a X1 uoO 388