THE SOURCES OF AMYLASE IN THE DIGESTIVE TRACT OF PAGURUS SAUELIS (Arthropoda: Decapoda) Philip Sullivan Hopkins Marine Station of Stanford University Pacific Grove, California June 5, 1965 An examination of the gut contents and feeding habits of Pagurus samuelis (Stimpson, 1857) revealed that their diet contains a wide variety of animal and plant matter, no doubt containing a significant amount of starch and possibly glycogen. A preliminary iodine test on starch substrate incubated with hepatopancreas extract showed that this organ does, indeed, contain a powerful amylase. An investigation of the literature revealed that very little work has been done on the origin of carbohydrases in decapods. Wolvekampo)found glands in the wall of the gut which he be- lieved to produce mucus and "perhaps amylase." Waterman (2) concludes that the secretion of digestive enzymes takes place "almost exclusively in the hepatopancreas." The pur- pose of this investigation was to locate the origin of amylase in the digestive tract, at the same time providing an indica- tion of possible sites of origin of other carbohydrases for another investigation being done at the same time. In addition, the properties of the amylase present in the hepatopancreas were investigated. MATERIALS AND METHODS Crabs were taken from the intertidal zones of China Point, the site of Hopkins Marine Station, and Point Pinos at Pacific Grove. They were kept in aquaria with fresh sea- water until needed. For the purpose of this investigation, the digestive tract was divided into five segments: foregut, extending from mouth to juncture of anterior midgut diverticula: midgut, from anterior midgut diverticula to posterior midgut diver- ticulum; hindgut, from posterior midgut diverticulum through the anus; hepatopancreas; and, anterior midgut diverticula. Before testing, the gut segments were split and thouroughly washed in distilled water to eliminate the amylase activity of the particulate contents as well as the amylase secreted elsewhere and transported to that portion of the gut. The tissues were then ground in an homogenizing tube and assayed immediately. The method of assay, also described by waksman(3), basically that of Wohlgemuth. One ml of.1% soluble starch (Baker and Adamson) was incubated with different dilutions of enzyme extracts for thirty minutes at room temperature (21922°0.). Two drops of iodine solution (Io.2%; KI.4%) and 3ml of Hø0 were added. The reaction mixture containing the lowest enzyme concentration that gave no blue color with iodine was taken as the end-point of the assay. The expression of enzmye concentrations in tissues is in mg of extrafcted tissue required to hydrolyze 1 mg of starch in 30 minutes. All tests were run in duplicate with starch solutions buffered at pH 5.4 (acetate) and pH 7.4 (tris-maleate). RESULTS The results of the investigation on the sources of amylase are presented in Table 1. By far the most important organ in the secretion of amylase appears to be the hepato- pancreas. It has over twenty time the activity of the stomach and forty times the activity of the hind and midguts. The optimum pH for the amylase present in the hepato- pancreas was determined in citrate-phosphate buffers varying by 0.4 of a pH unit over the range from 5.8 to 7.8. One ml of 11% starch was incubated for 30 minutes with varying amounts enzyme extract at each pH. and the end-points determined as before. The results of this test are presented in Table 2. The optimum temperature for the amylase present in the hepatopancreas was determined by the same method. Here, the reaction mixtures were buffered at the optimum pH (7.0)and were incubated at five temperatures from 10° to 40°0. Since reaction mixtures at each temperature showed the same end-point, colorimeter readings were taken on those reaction mixtures which still showed blue staining. From these readings, the reaction rates appeared to increase with increasing temperture up to 35°, decreasing thereafter. 4 The final hydrolysis prooducts were determined by in- cubating 2ml of 1% starch with.lg of enzyme extract at 1506 for 10 hours. Analysis was made by paper chromatography after the method of Jeanes(5) using a pyridine, butanol, water solvent in the ratio of 3:2:1.5 over a period of 20 hours. The developing spray reagent was that quoted by Gordon (6) as CD-1. Two test spots were made in addition to one control spot each of maltose, glucose, and a mixture of maltose and glucose. While the control spots showed good separation of maltose and glucose, the test spots showed a high content of glucose and only the faintest trace of maltose. This result would strongly indicate the presence of a maltase powerful enough to break down the maltose as fast as it is produced by the amylase. An investigation of the presence of a ß-amylase was made using .1% concentrations of amylose (Nutritional Biochemical Corp.) and amylopection (Calbiochem). Two samples of enzyme extract from the same source were used, one sample being heated at 57° for 20 minutes. Four ma of each enzyme preparation (heated and unheated) was incubated at room temperature with 2 ml of each substrate (amylose and amylo- pectin). The mixtures were buffered at pH 6.8. One-tenth ml aliquots were taken at 20-minute intervals and tested accord- ing to the Somogyi(7) method for the production of reducing sugars, and a rate of sugar production was determined. The difference in susceptibility of amylose and amylopectin to hydrolysis by the amylase in the hepatopancreaslis presented in Fig. 1. DISCUSSION Although the hepatopancreas is by far the strongest producer of amylase, the foregut, containing the esophagus and stomach, does show an activity twice as great as that of the muscle, which probably owes its activity to the presence of amylase in the blood and hemolymph. Amylase in the blood and hemolymph of another decapod, Astacus, was demonstrated by Damboviceanu(8). The hind and midguts also showed activity corresponding to this base level. The even lower activity of the diverticula may be due to that organ's small size and smooth surface which allow a more efficient washing as compared to the other bulkier, more irregular organs tested, which probably keep a larger portion of their original fluids. In the determination of the pH optimum, the use of tris- maleate buffer in place of citrate-phosphate buffer showed no significant difference in amylase activity. The finding, in the final hydrdysis products, of glucose and very little maltose corresponds with the findings of Hourani (9) of maltse activity in the hepatopancresa and weak maltase activity in the foregut. While £-amylase is generally considered to be solely a plant enzyme, evidence for its presence in other decapods is given by Yonge(10). The sensitivity of O-amylase and the resistence of Ø-amykse to heating is discussed by Waksman(11). The differences in activity of heated and unheated preparations of hepatopancreas extract, and the differences in susceptibility of amylose and amylopectin to hydrolysis suggest the possible presence of a ß-amylase in this organ of P. smmuelis. SUMMARY The hepatopancreas was found to be the most important producer of amylase in Pagurus samuelis. 2. The foregut, though much weaker, was also shown to have significant amylase activity. 3. The other portions of the digestive system had activities equal to or lower than muscle tissue. This activity is probably the result of amylase in the hemolymph and blood. 4. Under laboratory conditions, the pH optimum was found to be 7.0. 5. Under the same conditions, the temperature optimum was found to be near 35°0. Some evidence for the possible presence of aß-amylase was found. REFERENCES Wolvekamp, H.P., 1947, Sur la presence de deux amylases 1. dans les suc gastrique des decapods. Actualites Biochim,, 10:19-21. noted in Waterman, p. 298. 2. Waterman, T.H., Physiology of Crustacea, Academic Press, New York, 1960, p. 298. Waksman and Davidson, Enzymes: Properties, Distribution, Methods, and Applications, Williams and WIlliams, Baltimore, 1926. p. 159. 4. Wohlgemuth, J., Ueber eine neue Methode zu quantitativen Bestimmun des diastatischen Fermentes. Biochem. Z., 1908, 9:1-9. noted in Waksman and Davidson, p. 159 5. Jeanes, Wise, and Dimler Improved techniques in paper chromatography of carbohydrates. Analytical Chemistry, 23:3, March, 1951. 6. Gordon, Thornburg, and Werum, Rapid paper chromatography of carbohydrates and related compounds. Analytical Chemistry, 28:5, May, 1956. Somogyi, M., 1945, Determination of blood sugars. J. of Biol. Chem., 160, pp. 69-73. and 1952, Notes on sugar dtermination. J. of Biol. Chem., 195, pp. 19-23. 8. Damboviceany, A., 1932, Composition chemique et physio- chemique du liquide cavitaire chez les crustaces decapodes, Arch. Romanes Pathol. Expel. Microbiol., 5:239-309. noted In Waterman, p. 152. 9. Hourani,B., Carbohydrase activity in the intestinal tract of Pagurus. samuelis. unpublished article, Hopkins Marine Station, Pacific Grove, Ca ifornia. 10. Yonge, C.N. 1924, The mechanism of feeding digestion, Brit. J. Exptl. and assimilation in Nephrops norvegicus. Biol., 1:343-389. nõted in Waterman, p. 289. 11. Waksman and Davidson, p. 159. TABLE 1 CONCENTRATION OF AMYLASE IN TISSUES OF P. SAMUELIS HEPATO- HIND AND ANTERIOR MUSCLE FOREGUT DIVERTIC PANGREAS MIDGUTS — 85 150 300 153 pH 5.4 153 85 150 300 pH 7.4 mg of extracted tissue required to hydrolyze 1 mg of starch in 30 minutes. — 50 TABLE 2 DH OPTIMUM OF HEPATOPANCREAS AMYLASE 6.6 77. 6. 5.8 5.4 L 25 12 12 12 25 50 — ing of extracted hepatopancreas required to hydrolyze 1 mg of starch in 30 minutes. 7.8 — 25 175 h 1965 Pagarus O FIG.GI RATE OF HYDROLYSIS OF AMYLOSE AND AMYLOPECTIN BY HEATED AND UNHEATED HEPATOPANCREAS EXTRACT 200 150 roncentråtion ofgreduding sugars iniquot aliquotsiof reaction 100 mixture mg/10 ml . 50 40 min. 60 min. 20 min. amylopectin + unheated enz. amylose +unheated enz. amylopectin + heated enz............. amylose + heated enz.- - incubated a 57°0. for 20 minutes before introduction of substrate 297