Summary B-D-glucosidase activity increased during development of the barnacle, Pollicipes polymerus. The activity increased 18.7-fold from early blastula through the nauplius stage and at all stages exhibited a 3:l ratio of soluble to particulate form and was activated by the detergent Triton X-100. A similar activity was also found in the adult digestive tract. The possible roles of the exhibited activity are discussed. 1 Introduction Hydrolytic enzymes of Crustacea have been studied exten- sively in the adult stages but almost nothing is known about the embryonic synthesis of these proteins. Since the midgut cells become specified around the 33 cell stage, it seems probable that digestive enzymes might also be forming simultaneously(1). An outgrowth of cells in the posterior midgut of free-swimming larvae, or nauplii, of the barnacle Balanus balanoides, were found to be very similar to those of the adult digestive gland (2,3). Lack of knowledge concerning specific enzymes, either for the digestion of yolk proteins or for later use in the adult barnacle, prompted this study of a B-D-glucosidase during development in the barnacle Pollicipes polymerus. Activity of the enzyme was assessed for five developmental stages and, for comparison, in the adult barnacle. Materials and Methods Obtaining Embryos Adult Pollicipes were collected at Mussel Point near Monterey, California in April and May, 1982. The embryos are brooded in the mantle cavity in a pair of oval disks or ovigerous lamelli. The embryos were inspected and classified into one of the following five developmental stages: early blastula, just after the anterior and posterior midgut rudiment cells first become specified; limb rudiments, development just begun of the naupliar limb rudiments; naupliar appendages elongated; nonmotile nauplius; motile nauplius. Assay of Enzyme Activity The lamelli were gently homogenized on ice with a Dounce homogenizer in a chilled buffer solution of 0.05M Tris, O.05M Citrate, pH 4.0, unless otherwise specified. In the assays for the determination of intracellular compartmentalization, O.5M KCl was added to the buffer to insure an isotonic assay medium. Determination of B-D-glucosidase activity, using the synthetic substrate, p-nitrophenyl B-D-glucoside (Sigma Chemical Co.) was modified after that of Fedecka-Bruner et al (4). The assay mixture contained 0.2 ml of 0.02M substrate, 0.2 ml 1.0% Triton X-100, 0.4 ml homogenate, and 1.2 ml buffer. After incubation at 30°C (60 minutes unless specified other¬ wise), the reaction was terminated by addition of 1.0 ml of O.5M Naoh. The mixture was centrifuged at 27,000 g at 0°0 for 10 minutes and the supernatant then read in a Gilford spectrophotometer along with its corresponding blank, against distilled water at 420 mu. The blank was prepared by adding the homogenate together with the Naoh. The B-D-glucosidase activity is expressed in nanomoles of p-nitrophenol liberated per milligram protein per 60 minutes (4). Protein was measured by the method of Bradford using bovine serum albumin as a protein standard (5). Results ph Optimum and Linearity with Time Fig, 1 shows that the maximum activity of the enzyme occured at a pH 3.0 however, at this pH, the time course was not linear (data not shown). The activity at pH 4.0 is within 80% of the activity at ph 3.0 and the time course is linear for up to 60 minutes at this pH (Fig. 2). For this reason, the assays were done at pH 4.0 for 60 minutes. Linearity of Rate with Protein Concentration Fig. 3 shows that the enzyme activity is directly proportional to the protein concentration for up to 1800 ug of added protein. For this reason, the protein concentration was adjusted so that the final concentration was always less than 1800 ug with most assays containing between 500 and 1000 ug protein. Enzyme Activity in Development Fig. 4 shows that the enzyme is present in the early blastula stage of development and increased 18.7-fold through the nauplius stage. Even though the embryos were classified into five stages, there was very little variation except in the motile nauplius stage. This stage exhibited 337 +103 nanomoles per mg protein per 60 minutes. For this reason. five additional collections and assays of naupliar stages were made to insure that the results were indicative of that stage of development. The large deviation observed in the naupliar stage can easily be explained by the fact that the embryos are brooded for 30 days and as such, the stage classified as the naupliar stage could represent a longer time span than the other stages of development (6). This argument is strengthened by the fact that, whereas the ovigerous lamelli of the other stages have a characteristic texture and color, the color of the motile nauplius stages were seen to range from an orange-brown to a gray color. It was observed that this progression of color was associated with an increase in the accumulation of B-D-glucosidase activity. Enzyme Compartmentalization To determine if the enzyme is particulate at some point in development, the homogenate of the early blastula and motile nauplius were centrifuged (27,000 g for 30 minutes) in the presence and absence of 0.27 Triton X-100. The supernatants were removed by pipet and saved for later assay of activity; the pellets were resuspended in a volume of buffer equivalent to that of the supernatant. The assays were then run with 1% detergent present in each mixture. Ihe absence of Triton X-100 during the centrifugation resulted in 75% activity in the supernatant and 25% in the pellet. In the presence of Triton X-100, the activity shifted to 947 in the supernatant and 6% in the pellet. This behavior was true in both stages. A pH optimum curve, similar to Fig. 1, was run on the supernatant and pellet (27,000 g for 30 minutes) in the absence of Triton X-100 to determine if the soluble and particulate activity were due to different isozymes. In the assay mixtures buffered to pH 3.0, 4.0, 5.5, and 6.5, the activity, in each case, was 75% supernatant and 25% pellet. The total activity at each ph was found to be similar in ratio to the activity found in the earlier ph optimum curve (Fig. 1). Perhaps a 27,000 g spin was inadequate to pellet a particulate activity. Centrifugation was therefore carried out at 100,000 g for 60 minutes to ascertain if any additional activity could be sedimented. The same 3:1 ratio of activity was found, as in the two fractions of a 27,000 g spin. The assay was also run with both fractions in the presence or absence of 1% Triton X-100; an incréase in enzyme activity was seen in both insoluble and the soluble supernatant fraction when Triton X-100 was present (1.6-fold increase). This result indicates that the soluble enzyme is directly activated by the detergent. These results suggest that one enzyme is responsible for the activity. Twenty-five percent of the enzyme appears to be particulate and the soluble form is activated by the detergent, Triton X-100; the effect of Triton X-100 on the particulate fraction is related to its effect on the solubilization of the enzyme. A final enzyme assay was run on the intestinal tract of the adult barnacle. The juices of the intestine were obtained by inserting a fine-pointed pipet in the tract and extracting the juices contained in the lumen. The tract was then removed and homogenized. Assays were run on the juices and the supernatant and pellet (27,000 g for 30 minutes) of the homog. enate. The juices of the lumen contained a majority of the activity. The homogenized gut tract showed activity in the supernatant and pellet with a ratio of 3:1, supernatant:pellet, as was found in the embryonic stage. All fractions (juices and homogenized gut) were also activated by the detergent. . . . Discussion The results of this study show the presence of a B-D- glucosidase in Pollicipes embryos and nauplii. The activity, h increased 18.7-fold from the early blastula through the nauplius stage, exhibited a 3:l ratio of soluble to particulate form in every stage. The enzyme was activated by the detergent Triton X-100. A B-D-glucosidase activity was also present in the adult digestive tract and this enzyme was activated 1.5-fold by Triton X-100 and similarly exhibited a 3:1 soluble:particulate nature. No further comparisons were made. but these results suggest that the adult and embryonic forms are isozymes. There are two major possibilities for the presence of a B-D-glucosidase in embryonic stages. One hypothesis is that the enzyme is used during embryogenesis, as for digestion of yolk constituents. A second hypothesis is that the enzyme activity is accumulating in the midgut cells for later use in the swimming nauplius and following larval stages. If the first proposal is correct, the enzyme could be functioning intracellularly, as in a lysosome, or extracellularly. as a component of a developing but functioning embryonic gut. A lysosomal role would seem to be excluded by the largely soluble nature of the enzyme (the increased activity induced by the detergent did not result from release of the enzyme from a particle; as shown, the soluble enzyme itself was detergent activated). An alternate possibility however, is that the yolk cells themselves are acidic and functioning as a " cellular lysosome." If so, these large cells would be broken during the homogenization procedure and release the soluble enzyme. An extracellular function of the enzyme might also be possible. The yolk cells are present in the midgut during development and the midgut might be functional at this time in utilizing yolk constituents. A problem with the above concept of embryonic utilization is that there is no evidence for a B-linked carbohydrate in the embryo; the major known store is glycogen, which would be degraded by glycogen phosphorylase or an a4-D-glucosidase (7,8). The alternative explanation is that the enzyme is not. used during embryogenesis but represents accumulation of the enzyme for later use in the feeding larval stages. The role for a B-D-glucosidase activity then could be for digesting laminarin or cellulase, which would be major constituents of a planktonic or detrital diet. A laminarinase has been found in the midgut of adult barnacles, Balanus nubilus and a cellulase is present in the " sterile midgut of adult lobster and crawfish with a ph optimum of 4.0 to 4.5 which appears to be much lower than the pH optimum of 5.0 to 6.0 found for other carbohydrases (9,10,11). Studies on synthesis of adult digestive enzymes could explain the 3:1 soluble:particulate nature of this enzyme and activation by detergents. If it is indeed digestive, the enzyme is probably being accumulated in the hepatopancreatic gland. In adults, digestive enzymes are stored in enzymatic granules which are distended with fluid, forming a large vacuole, or mature secretory cell (11,12). The contents of these cells are extruded into the lumen for extracellular digestion. It has been shown that a refractory period is necessary for mature cells and enzyme granules to form (11). The soluble activity could represent the enzyme present in mature or almost mature secretory cells, while the particulate activity could represent enzyme granules or newly forming cells. Homogenization could release the enzymes from secretory cells prematurely since it was found that even slight pressure on the cover slip of a slide of hepatopancreatic gland cells caused the breakage of the distended mature cells (12). As regards activation by detergent, it is interesting that the hepatopancreatic gland also stores and secretes bile salts into the lumen; the activating effect of Triton X-100 might mimic the activity of a natural detergent in the intestine(Il). There is insufficient data to decide between these various alternatives. Clearly, further studies on the digestive capabilities of barnacle embryos would be of interest. O Special thanks to Dr. David Epel for his help in this study and in the preparation of this manuscript. His insights and constructive criticisms were indispensable in the production of this text. References 1 Anderson, D. T., On the embryology of the cirripede crustaceans, Tetraclita rosea (Krauss), T. purpurascens (Wood), Chthamalus antennatus (Darwin) and Chamaesipho columna (Spengler) and some considerations of crustacean phylogenetic relationships, Phil. Trans. R. Soc. B. 256(1969) 183-235. 2 Walley, L. Jane, Studies on the larval structure and metamorphosis of Balanus balanoides (L.), Phil. Trans. R. Soc. B, 256 (1969)237-280. 3 Anderson, D. T., Embryology and Phylogeny in Annelids and Arthropods, Pergamon Press, Oxford, 1973, pp. 322-329. 4 Fedecka-Bruner, B., Anderson, M. and Epel, D., Control of enzyme synthesis in early sea urchin development: aryl sulfatase activity in normal and hybrid embryos, Develop. Biol., 25(1971)655-670. 5 Bradford, Marion M., A rapid and sensitive method for the quantitation of microgram quantities of protein utilizing the principle of protein-dye binding, Analyt. Biochem., 72 (1976) 248-254. 6 Morris, R. H., Abbott, D. P. and Haderlie, E. C., Intertidal Invertebrates of California, Stanford University Press, Stanford, 1980, pp. 514-515. 7 Green, J., Crustaceans. In G. Reverberi (ed.), Experimental embryology of marine and fresh-waster invertebrates, North- Holland Publishing Company, Amsterdam, 1971. pp. 312-362. 8 Barnes, H., Studies in the biochemistry of cirripede eggs, J. mar. biol. Ass. U. K., 45(1965)321-339. 9 Harnden, D. G., Digestive carbohydrases of Balanus nubilis (Darwin, 1854), Comp. Biochem. Physiol., 25(1968)303-309. 10 Kooiman, P., The occurence of carbohydrases in digestive juice and in hepatopancreas of Astacus fluviatilis Fabr. and of Homarus vulgaris M.-E., J. Cell. Comp. Physiol. 63(1964)197-201. 11 Vonk, H. J., Digestion and Metabolism. In T. H. Waterman (ed.), The Physiology of the Crustacea, Vol. 1, Academic Press, New York, 1960, pp.291-316. 12 Van Weel, P. B., Processes of secretion, restitution, and resorption in gland of mid-gut (glandula media intestini) of Alya spinipes Newport (Decapoda- Brachyura), Physiol. Zool., 28 (1955)40-54. Legends Fig. 1. pH optimum of B-D-glucosidase activity in the motile nauplius stage. Activity is expressed as 10 2 mole substrate hydrolyzed/mg protein/60 minutes. Fig. 2. Linearity of B-D-glucosidase activity as a function of time. Activity is at ph 4.0 and is expressed as 10-2 mole substrate hydrolyzed/mg protein. Source of enzyme was the motile nauplius stage. Fig, 3. Linearity of rate as a function of protein concentration. Results are expressed as change in optical density/60 minutes of assay mixture. Source of enzyme was the motile nauplius stage. Fig, 4. B-D-glucosidase activity during developmental stages of Pollicipes polymerus. For the motile nauplius, n-8; for all other stages, n-3. Vertical lines indicate range, bars indicate mean, and colored bars indicate standard deviation. Activity is expressed as 10-9 moles substrate hydrolyzed/mg protein/60 minutes. 500 400 300- 200 10 m 600 500 L 400 300 200 100 D ph 60 TIME (minutes) 30 90 120 : -.- 6 L 1000 2000 PROTEIN CONCENTRATION (ug) 3000 500 400: 300 20 100 (n=3) motile nauplius-(n=8) L limb naupliar nonmotile early blastula rudiments appendages nauplius motile naupsius