C C Lipase Activity in Pagurus granosimanus (Stimpson, 1862) (Arthropoda: Decapoda) Daniel C. Cabrera Hopkins Marine Station Pacific Grove, California C Examination of the gut contents of the hermit crab Pagurus revealed both algae and many types of ani- mal foodstuffs. In view of the varied diet of Pagurus, it would seem probable that its digestive system contained enzymes capable of hydrolyzing carbohydrates, proteins and fats. Although the ability to hydrolyze fats had been demonstrated in other Crustacea (2) (6), a study remained to be done in Pagurus. The experiments here out- lined are designed to determine lipase activity—its distribution and optimal conditions, in the genus Pagurus MATERIALS AND METHOD Pagurus granosimanus, as the largest of the species common to the intertidal zone surrounding the Hopkins Marine Station, was selected as representative of the genus. The crabs used were collected at nearby Pinos Point and had an average wet weight of one gram. Preparation of enzyme The hepatopancreas were removed from forty P. granosimanus, dehydrated in acetone for two hours and defatted in petroleum ether for an addi- tional two hours. (In the case of the gut, sixty indi¬ viduals were necessary.) The dehydration and defatting were carried out a 5°C. One gram of this residue was ground to a fine powder in a mortar and extracted at 5°C in 100 ml. of 50% aqueous glycerol for twenty-four hours. The filtered extract was used as the source of enzyme. Substrate preparation A water-soluble, polyoxyethylene derivative of sorbitan mono-oleate, commercially known as Tween 80 (Sigma Chemical Co., St. Louis, Missouri) was used as substrate. The Tween 80 to be used as substrate was diluted to 50% with water and titrated with 17% phosphoric acid to the desired pH. All measure- ments of hydrogen ion concentration were made with a Beckman zeromatic pH meter. Enzyme assay The procedure followed was essentially that of Archibald (1). Three ml. of 50% neutralized Tween 80, 0.5 ml. of 0.2 M phosphate buffer, and 0.5 ml. of the enzyme preparation were placed in a 15 ml. centrifuge tube, thoroughly mixed with a glass stirring rod and incubated for 1 hour. After incubation, 1.0 grams of reagent-grade NapHøP04-H20 and 10 ml. of ether mixture " 5:1) were added. (diethyl ether, petroleum ether, b.p. Simultaneously, a blank was prepared containing all of the components of the assay mixture prepared immediately prior to extraction with ether. After mixing and centrifugation for 10 minutes at 4000 r.p.m., the ether layer containing the released fatty acids was withdrawn and placed in a 30 ml. beaker. The ether was removed by evaporation after the addition of O.5 ml. 2-methyl-2, 4-pentanediol (J.T. Baker Chemical Co, Phillipsburg, New Jersey). The vis- cous residue was then titrated with O.Ol N NaoH to the original pH. Lipase activity was estimated in terms of milli- equivalents of acid produced per hour. Activity was determined by the use of the following equation: A - D - C / 100 T where D is ml. of 0.O1 N NaoH used in titration of the reaction mixture, C is ml. of NaoH used in titration of the blank, and T is the reaction time in hours. RESULTS Direct measurement of the gut contents revealed a decrease in hydrogen ion concentration from the fore- gut (pH 5.5) to the hindgut and hepatopancreas (pH 7.4). The gut exhibited a relatively negligible amount of li- pase activity compared to that found in the hepatopan- creas (0.16 milliequivalents of acid / hour / 0.05 gram of dehydrated, defatted tissue at pH 7.2, 23.5 C). For this reason, further experiments were carried out using hepatopancreatic extracts only. Figure 1 illustrates the finding that lipase activity in P. granosimanus increases with increasing pH to approximately 7.2. It can be seen in Figure 2 that lipase activity varies with temperature and that its optimum temperature is approximately 35C. The effects of variations in substrate concentra¬ tion upon lipase activity in P. granosimanus are presented in Figure 3. Activity increases with increasing substrate concentration to a maximum at approximately 2.16 grams Tween / 0.05 grams of dehydrated, defatted tissue extract. The relative concentration of substrate used in the above studies was in excess of this amount. The lipase preparation was labile, losing approx- imately 60% of its activity after sitting for only two hours at room temperature (23 C). DISCUSSION Although esterases which attack simple ester link- ages are found in many animal tissues, lipases appear to 4. be confined to the pancreas and intestinal tract (4). No attempt was made to measure lipase activity in tissues other than those associated with the digestive tract. Digestive enzymes in Crustacea have been reported to have their pH optima in the slightly acid ranges (7), but it has been shown that with progressing purification of enzyme preparations, optima tend to move from lower to higher pH (3). In studies where lipase activity was greatest in the acid range, the gut contents were also slightly acid whereas some gut contents of P. granosi- manus are slightly alkaline. That the optimal temperature range for the lipase preparation should exist at about 35 C is in approximate agreement with that of 28 C found for glycerol-extracted pancreatic lipase described by Schwartz (8). The obser- vation of extreme temperature lability of lipase prepara- tions has been noted before (see 9). SUMMARY Optimum pH, temperature and substrate concen- tration were determined for the hepatopancreatic lipase present in Pagurus granosimanus. 1. The pH optimum was 7.2. 2. An optimal temperature of approximately 35 C was demonstrated. 3. Highest activity was reached at a substrate concen- tration of 0.432 grams Tween per ml. of lipase ex- tracted from 0.05 gram tissue. Figure 1. Determination of pH optimum of hepato- pancreatic lipase from P. granosimanus. Activity is expressed in milliequiva- lents of acid produced in one hour by an extract of 0.05 gram of dehydrated, de- fatted tissue. 8 1 J — N 1 0 0 G J 0 C Figure 2. Determination of temperature optimum for hepatopancreatic lipase from P. granosi¬ manus. Activity is expressed in milli- equivalents of acid produced per hour by an extract of 0.05 grams of dehydrated, defatted tissue at pH 7.0. — S — 2 D 0 0 8 0 0 QL 00 Figure 3. Determination of optimal substrate con- centration of hepatopancreatic lipase of ranosimanus. Activity is expressed in P. milliequivalents of acid produced in one hour by an extract of 0.05 gram of dehy- drated, defatted tissue at pH 7.0, 23 C. oo 7C O. C REFERENCES R.M. Archibald "Determination of Lipase Activity" Journal of Biological Chemistry, V. 165 (1946) pp. 443-48 Arthur D. Hasler "Physiology of Digestion in Plank- ton Crustacea" Biological Bulletin, 68, pp.208-14. 3. Colowick, S.P. and N.O. Kaplan, ed. Methods i Enzymology Vol. I, Academic Press Inc. (New York, 1955) 835 pp. Fatty Acids and Their Derivatives Ralston, A.W. John Wiley and Sons, Inc. (New Tork, 1946) 986 pp. Sumner, James B. and Karl Myrback eds. The Enzymes Vol. I, Academic Press Inc. (New York, 1950) 724 pp. Yonge, C.M. "The mechanism of feeding, digestion, and assimilation in Nephrops norvegius" Brit. Jour. of Experimental Biology 1: pp.343-389. Waterman, T.H. ed. The Physiology of Crustacea Vol. I, Academic Press, Inc. (New fork, 1960) 670 pp. Schwartz, B. "The Effect of Temperature on the Rate of Hydrolysis of Triglycerides by Pancreatic Lipase" in The Journal of General Physiology 27: pp.113-118. Sizer, I.W. "Effects of Temperature on Enzyme Kinetics" in Advances in Enzymology, V.3, (New York, 1943) p.35