ABSTRACT 1. Qualitative studies of reproduction and quantitative studies of total and individual carotenoid content in the stalked barnacle Pollicipes polymerus were carried out for animals in polluted and nonpolluted areas in the Monterey Bay area of California. 2. Reproductive activity was retarded in areas very close to point sources of pollution. 3. The total carotenoid content in the stalk fluid of Pollicipes was invariably lowest in animals close to point sources of pollution, concomitantly, the amount of carotenoid tended to increase with increasing distance from such pollution sources. 1. It was suggested that total carotenoid content may be fected by proximity to sewage effluent whereas astaxanthin content may be specifically effected by increaséd chlorine concentrations. 5. Possible mechanisms governing the decrease in Pollicipes carotenoid content are discussed. 96 INTRODUCTION A growing awareness of environmental pollution has led to recent attempts to evaluate the biological impact of local domestic sewage discharges into Monterey Bay. One of these studies (Holstrom, 1970) showed an effect on the stalked barnacle Pollicipes polymerus, a natural and abundant inter- tidal organism along the central California coast. Holstrom found that samples of populations adjacent to sewage outfalls had reduced reproductive capabilities. He also noted a qualitative difference in the amounts of carotenoid pigments in the animals, including an apparent total lack of astaxanthin, astaxanthin ester, and lutein in animals from highly polluted areas. This mutual effect on reproduction and on carotenoid content seemed to be linked to levels of chlorination rather than to any other factor. These apparent effects on carotenoid content are most intriguing in light of recent thoughts concerning the rela- tionship of carotenoids to reproduction in marine invertebrates (Cheesman et al., 1967). Some of the carotenoids in the animal, especially astaxanthin, are found as lipoprotein complexes (Holter, 1969). Glyco-lipoprotein complexes, which have been noted in the blood of many invertebrates, may be involved in the transport of carotenoids (Cheesman et al., 1967). Likewise, a carotenoid attached to a lipoprotein could possibly mediate the transport of large water-soluble mole- cules across lipid-bound membranes (Holter, 1969). Such properties would be importantat the onset of reproduction 79 when there is a transfer of nutrient materials to the egg. The blue pigment in the ovaries and developing embryos of Lepas fasicularis is a carotenoprotein with astaxanthin attached to euglobulin (Ball, 1944). Ball showed that developing nauplii change their color from blue to pink, representing the liberation of free astaxanthin from the protein complexes. Such phenomena are quite common in marine invertebrates (Cheesman et al., 1967). Recently suggestions have been made that these huge protein complexes may be food storage sites for early developmental stages (Zagalsky et al, 1967). The carotenoids are thought to stabilize the glyco-lipid proteins and the organism in question somehow frees these carotenoids, allowing the proteins to be utilized (Cheesman et al., 1967). The eggs of Pollicipes polymerus chang from an orange color to a brown color as they mature. However Lee and Gilchrist (1971) have found that a similar color chang in the sand crab, Emerita analoga, is strictly chromataphoric. Unextracted stalk fluid from Pollicipes polymerus in highly polluted areas is yellow-gray, as opposed to the bright orange color found in animals from unpolluted areas. This yellow-gray color could be the result of interference with either the synthesis of carotenoids, namely astaxanthin, or the formation of a stable linkage between carotenoids and proteins. An investigaton of the quantitative effects of sewage pollution on the pigments of Pollicipes polymerus is made easier by a recent study by Holter (1969) describing the 80 O carotenoid pigments in Pollicipes. He isolated and identifiid the following pigments: B-carotene; astaxanthin; astaxanthin ester, lutein, zeoxanthin; iso-zeoxanthin. The present study was designed to: (1) obtain a quantitative estimate of the effects of domestic sewage pollution on carotenoids; (2) compare qualitatively animals from a polluted area with animals from a healthy area; and (3) assess the possible relationship between carotenoids as effected by pollution and their reproductive role. 8 C MATERIALS AND METHODS Animals Barnacles were collected at six sites along the Carmel- Monterey coastline (Fig. 1 and 2) and one site in Southern California. The areas were as follows: (1) the Pacific Grove sewage outfall area at Point Pinos (3 stations), on April 28th and May 27th, 1971; (2) the Carmel sewage outfall area north of Monastary Beach (5 offshore stations and inshore stations);(3) Mussel Point; (4) Hovden cannery, north of Mussel Point, on April 29th and May 6th, 1971; (5) Sea Otter Point, approximately ½ mile south of the mouth of Malpaso Creek along California Highway No. 1; (6) the Highlands Inn outfall at Carmel Highlands south of Point Lobos; (7) White's Point on the south side of the Palos Verdes Peninsula in Southern California, directly inshore of the Los Angeles County sewage outfall. The number of animals collected at each of these sitesranged from 30 to 65 (Table 1). The areas were selected to represent highly polluted areas: Point Pinos; Carmel; White's Point, areas polluted by relatively small discharges: Highlands Inn, and unpolluted areas: Hovden cannery, Mussel Point, Sea Otter Point. The white to orange ovaries and the orange to yellow-gray stalk fluid of the Pollicipes polymerus were used for measuring carotenoid content as Holter (1969) showed these two tissues to be the highest in carotenoid content. Stalk fluid was collected by cutting whole clumps 8 of barnacles from the rocks and allowing the stalk fluid to drain. The stalk fluid and the animals from which it was obtained were immediately placed on ice and transported to the laboratory as soon as possible. The animals were then dissected and the ovaries removed. The stalk fluid was centrifuged at 10,000 R.P.M. for 20 minutes to remove particulate matter. Acetone was added to both the fluid and the ovaries and they were refrigerated up to 12 hours until needed. Extraction of Carotenoids The ovaries and stalk fluid were extracted in acetone and transferred to di-ethyl ether, saponified, and re- dissolved in di-ethyl ether according to the methods of Lee (1966). Before saponification the extract was transferred to petroleum ether (B.P. 20-1000) and the absorption spectra (500-130 nm) of the extracted carotenoids determined with a Beckman DB-G gradiant spectrophotometer. These readings were used to calculate total carotenoid content by applying the formula: ug carotenoids/mg ovary - 1 X OD at peak x volume extracted or original amount ml fluid Pigment Identification The extracted pigments were applied to 20x20 and 5x20 Mannogram prepared silica gel-G thin layer chromatography plates. The plates were run in a mixture of 25% acetone in hexane. The separate bands were then scraped off the plates into a mixture of 10% acetone in petroleum ether 83 and the absorption spectrum was again determined and the amounts of the individual pigments were calculated as outlined above. These individual pigments were identified by the wavelength of maximum absorbance in petroleum ether and by comparison with pigment standards which were also applied to TLC plates and run under the same conditions. The sources of these standards were identical to those reported in Lee and Gilchrist (1971). 84 RESULTS Point Pinos The two Point Pinos samples taken in April and May each contained subsamples taken from three locations (Fig.1): area P, within 20 yards of the pipe and highly polluted; area B, a moderately polluted area west of the pipe; and area C, a slightly polluted area south of the pipe. Both samples from area P consisted of undersized individuals with rostro-carinal distances of 15-20mm(17.2mm is minimum size for reproduction; Hilgard, 1960). The average range encountered in all healthy populations was 25-35 mm. These animals all had yellow-gray stalk fluid as compared to the usual bright orange color. Few had developed ovaries and none had ovigerous lamellae. In both the April and May samples the amount of total pigment in the stalk fluid (Fig.3) was well below that found in the samples taken from areas B and C. The total pigment in the ovaries was comparable to that found in all other Point Pinos samples. The most abundant stalk fluid pigment in the April sample taken from area P (Fig.5) was lutein, which amounted to 74% of the total pigment complement of the animals. The samples from area B appeared healthy and had bright orange stalk fluid. Many had developed ovaries and ovigerous lamellae. The amount of pigment in the stalk fluid of both samples (Fig. 3) was approximately six times the amount of pigment in area P animals and 0.75 times the amount in area C animals. The amount of pigment in the 85 ovaries, however, was the highest recorded for any of the Point Pinos samples and almost equivalent to the amount of pigment found in the ovaries of animals collected from unpolluted sites such as Sea Otter Point (Fig. 1). The most abundant pigment in samples from area B was astaxanthin which amounted to 66% of the total. The two area C samples appeared healthy although there were hardly any ovigerous lamellae seen in the individuals collected. These animals consistently had the highest amount of pigment in the stalk fluid as compared to the other Point Pinos samples (Fig. 3), and, in the ovaries, more pigment than individuals from area P but less pigment than individuals from area B (Fig.4). Similar to the results obtained from area B, the most abundant pigment in the April stalk fluid samples was astaxanthin, amounting to 61% of the total carotenoid content. In both April and May there appeared to be a definite gradient in the amount of pigment in the stalk fluid relative to the proximity of sewage effluent. The pigment in the ovaries however, did not show such a gradient. The predominant pigment in the animals that appeared healthy (areas B and C) was astaxanthin, while lutein was clearly dominant in the unhealthy animals (area P), almost fully replacing the astaxanthin in relative per cent. Carmel Offshore: All animals collected at these sites (Fig. 2) appeared to be healthy. The occurrence of developed ovaries 86 was highly variable in this group of samples. Station 1 animals which were collected very close to the outfall were relatively large (30-35mm) but had no developed ovaries and no ovigerous lamellae. Animals from stations 2,4, and 5 were smaller (25-30mm) but almost all had developed ovaries and ovigerous lamellae were often present. Animals from station 3 were small and half of them had developed ovaries. There were also ovigerous lamellae present. The stalk fluid from all these animals (stations 1-5) was bright orange. The amount of pigment in the stalk fluid was lowest in animals from station 1 and comparable to the level of pigment in the animals from station P at Point Pinos (Fig. 3). The stalk fluid pigment levels in animals from stations 2,3, and 5 were highest compared to all the offshore samples at Carmel, and were close to the levels found at station B at Point Pinos. Compared with 2, 3, and 5, the pigment level in station l animals was low. The pigment in the ovaries was lowest at station 1. The ovary pigment levels at 2 and 3 were approximately 1.5 times the level at station 1. The levels in the ovaries at 4 and 5 were approximately 2 times this level (Fig. 1). Astaxanthin was most abundant in animals from stations 1 and 5, amounting to 53% and 55% respectively. These astaxanthin levels are about 10% lower than those found at Point Pinos. B-carotene was most abundant at station 2, amounting to 59%. Lutein was most abundant at stations 3 and 4, amounting to 61% and 59% respectively. 9 Generally the amount of pigment in both the stalk fluid and the ovaries of these offshore samples increases as the distance south of the outfall (station 1) increases, although the levels at station are consistently low. Th relative amounts of individual pigments present show no definite trend as they appeared to in the Point Pinos samples. Inshore: The stalk fluid from all of these animals was bright orange although station 1 and 2 animals did not have many developed ovaries and only station 5 animals had ovigerous lamellae. The amounts of pigments in the stalk fluid of station 1,2, andl animals was low (close to the level L animals in the offshore samples). The stalk fluid pigment level for station 5 animals was very high, 6 times the amount at 1, 2, and and second only to the levels obtained for animals from Sea Otter Point (Fig. 3). The total amount of pigment in the ovaries was lowest for station as was the amount of stalk fluid pigment. The value for station 1, in the area of the pipe, was about 6 times the value for the other inshore stations. There was not enough pigment to obtain values for the indi- vidual pigments. Others: Animals from White's Point had bright orange stalk fluid although only 3 in 60 had well developed ovaries and no ovigerous lamellae. The amount of pigment in the stalk fluid was low, 33.6ug/ml, close to the value obtained at the Carmel inshore station 1. The amount of pigment in the ovaries was close to that in animals from area C at Point 88 Pinos. The sample from Highlands Inn appeared to be the health- iest of all the samples collected. The fluid was bright orange and almost every animal had a well developed ovary. However, the values for total amount of pigment were very low for both the stalk fluid (close to the value at White's Point and station 1 in the inshore Carmel series) and the ovaries (close to the value at station L in the inshore Carmel series). Lutein was the most abundant pigment, amount- ing to 60% of the total pigment. Few of the animals from Mussel Point had well developed ovaries. The stalk fluid was a dull orange. The amount of pigment in the stalk fluid was close to station C at Point Pinos in May (Fig. 3). The amount of pigment in the ovaries was highest of any of the samples collected. Astaxanthin (44%) and lutein (55%) were almost equally abundant. The animals from Sea Otter Point were healthy with bright orange stalk fluid,many developed ovaries, and ovi- gerous lamellae. The amount of pigment in the stalk fluid was higher than any of the other samples collected. The amount of pigment in the ovaries was slightly higher than that found at station B in May at Point Pinos. The animals from the cannery appeared healthy, with bright orange stalk fluid, many developed ovaries, and ovi- gerous lamellae in the later sample. However the amount of pigment in the stalk fluid was close to the levels taken in May at stations B and C at Point Pinos. The amount of 89 pigment in the ovaries of the earlier sample was very high, close to that of Mussel Point (Fig.4). DISCUSSION Tth results of this study coincide in part with Holstrom's (1970) observations of decreased reproductive capability in Pollicipes polymerus occurring in the areas of concentrated sewage pollution. Quantitatively, the levels of total carotenoid pigment in the stalk fluid, and less consistently in the ovaries, suggest that carotenoid pigments are somehow adversely effected by the sewage effluent. The data from Point Pinos shows the most obvious correlations. The area where the effluent is most concentrated (sample area P) shows evidence of decreased reproduction and a definite drop in carotenoid pigments in the stalk fluid as compared to the pigment in the animals from the healthier areas. The amount of pigment in the ovaries suggest a similar trend, although here is is not as marked or as consistent. There is some indication that astaxanthin in the polluted areas may decrease with a concomitant increase in lutein. The data from Carmel does not give as clear a picture, possibly because the currents around the outfall have been shown to be very complicated Chlorine residues at Carmel have been measured at 1-2 ppm whereas those at Point Pinos have been measured as high as 10 ppm. This greater amount of chlorine input at Point Pinos may explain the more definitive results here as compared with the Carmel stations, although the stalk fluid pigments at some Carmel sites seemed to be just as effected as those at Point Pinos. The carotenoid levels in the ovaries from Point Pinos and Carmel were generally similar. The amount of pigment in the ovaries at inshore station 1 seemed inordinately high. A possible explanation may be related to local current patterns. Polluted water from the outfall sweeping back towards shore (Fig. 2) may miss station 1. The values for the offshore stations, however, show a more consistent pattern with a lower amount of pigment being found in the areas closest to the outfall. These observations tend to support Holstrom's contentions that decrease in reproductive capability may be linked to a decrease in total amount of pigment. However, the only consistent change in the proportions of the individual pigments takes place in the Point Pinos samples where there is a larger concentration of chlorine in the water. It therefore may be suggested that increased chlorination may directly effect the oxidation of astaxanthin, whereas unchlorinated or minimally chlorinated effluent may effect total carotenoid content. It was found that if a sample were left at room temperature or refrigerated for 18 hours it would turn yellow-gray and show a decreased amount of total pigment. This seems to indicate that dena- turing the proteins in the stalk fluid effectsthe carotenoid level by maximizing the opportunity for oxidation. This in turn could mean that the sewage effluent is effecting the protein and therefore secondarily altering the pigment 90 complement of the animals. It was hoped that a quantitative study of the indivi- dual pigments would show some kind of relationship between amount of sewage pollution and relative abundance of B¬ carotene, astaxanthin, and lutein. However, the data obtained allows no such correlations to be made and appears to be inadequate. This was brought about by the fact that the amount of pigment in the individual Pollicipes polymerus is very small and it is therefore difficult to obtain a good working volume of extract. Furthermore, astaxanthin, the major pigment in Pollicipes, is very labile and is readily oxidized even after extreme precautions have been taken. The mechanisms which bring about the changes in the amounts of total pigment are unknown. They may be due to replacement of carotenoids and carotenoid precursors in the diet of Pollicipes polymerus by non-nutrient containing particulate matter from the effluent; they may be due to some substance in the effluent which effects the biochemical processes of pigment production; or they may be due to denaturation of the protein structures, specifically the stalk fluid and egg carotenoproteins, also by some substance in the effluent. Whatever the mechanism, sewage pollution appears to have a definite measurable effect on total carotenoid levels in Pollicipes polymerus. 13 REFERENCES Ball E. G. (1911) A blue chromatoprotein found in the eggs of the goose-barnacle. J. biol. Chem. 152, 627-631. Cheesman D. F., Lee W. L., & Zagalsky P. F. (1967) Caroteno- proteins in invertebrates. Biol. Rev. 12, 131-160. Hilgard G. H. (1960) A study of reproduction in the inter- tidal barnacle Mitella polymerus, in Monterey Bay, California. Biol. Bull., Woods Hole 119(2), 169-188. Holstrom M. V. (1970) Distribution, reproduction, recruit- ment, and pigments of the stalked barnacle Pollicipes polymerus in the vicinity of sewage outfalls at Pacific Grove and Carmel, California. unpublished MS on file at Hopkins Marine Station Library. Holter A. R. (1969) Carotenoid pigments in the stalked barnacle Pollicipes polymerus. Comp. Biochem. Physiol. 28, 675-681. Lee W. L. (1966) Pigmentation of the marine isopod Idothea montereyensis. Comp. Biochem. Physiol. 18, 17-36. Lee W. L., Gilchrist B. M. (1971) Carotenoid metabolism and reproduction in the sand crab Emerita analoga (crustacea, anomura). in preparation. Zagalsky P. F., Cheesman D. F., & Ceccaldi H. J. (1967) Studies on carotenoid-containing lipoproteins isolated from the eggs and ovaries of certain marine inverte- brates. Comp. Biochem. Physiol. 22, 851-871. 24 O CAPTIONS Figure 1: Pacific Grove sewage outfall at Point Pinos, showing current patterns and collection sites. Station P was 20 yds from the pipe. Figure 2: Carmel sewage outfall, located between the Carmel River and Monastary Beach. Stations 1-5 on the right are the inshore collection sites; those on the left are the offshore sites. Figure 3: Total carotenoid pigment in the stalk fluid of Pollicipes polymerus. Carotenoid levels are given in ug/ml for each collection site. The collection sites from left to right are: Point Pinos, April and May,1971, P, B, and C are the areas shown on Fig. 1; Carmel, offshore and inshore areas as shown on Fig. 2; others include White's Point (W), Highlands Inn (H), Hovden cannery in April and May, 1971, (C), Mussel Point (M), and Sea Otter Point (S). Figure 1: Total carotenoid pigment in the ovaries of Pollicipes polymerus. Carotenoid levels are given in ug/g. The collection sites are as in Fig. 3. Figure 5: Individual carotenoid pigment in the stalk fluid of Pollicipes Polymerus. Top graph shows the per cent values for the collection points at Point Pinos (P,B,C as in Fig.1) in April, Carmel offshore samples (Fig. 2), Highlands Inn (H), Mussel Point (M). The bottom graph shows amounts for the same locations as as above, in ug/ml. Table 1: Dates of collection, number of animals collected, and amount of total carotenoid pigment in the collected samples. Amounts are in ug/ml and ug/g. 96 point pinos OUTFALIO K 6 P NEXT TO PIPE. B SOME EFFLUENT C NO APPARENT EFFLUENT OUTFALL OFFSHORE COLLECTION CARMEL OUTFALL AREA 195 Fig 2 INSHORE COL LECTION -- MONASTARY BCH CARMEL R. :::. kikii . 34 5 BC BC OFFSHORE APRIL MAY POINT PINOS CARMEL Collection Sites 2 4 5 INSHORE . WHICC OTHERS a . POINT PINOS 2183315 234 FHORE 12SHO CARME COLLECTION SITES WHCGM OTHERS kän in . . 9 8 . — 3 Fig 5 10 2 COLLECTION SITE POINT PINOS CARMEL offshore inshore 5 OTHEI Mussel Pt. Hovden Onry Highlands White's Pt. Hovden Cnry Sea Otter Pt. TABLE 1 DATE ug carot. of ANIMALS govary 1/28 30 756 1/28 990 1/28 60 714 5/28 138 5/28 1067 5/28 655 30 5/28 1110 5/28 665 5/28 625 997 30 5/28 950 30 5/30 50 5/8 1690 989 5/8 30 157 5/10 30 716 5/10 30 10 5/4 1911 60 5/6 1810 5/29 30 115 5/15 768 176 30 5/29 50 5/12 1197 ug carot. ml fluid 21 121 175 86 20 129 132 105 55 25 76 63 32 31 13 312 102 C KNOWLEDGEMENTS I would like to thank Dr. Welton L. Lee for his aid and advice in the lab and with this paper. 103