m TITI INTRODUCTTON Investigations have shown that that portion of the Coliform group found in the gastrointestinal tract and feces of warm blooded animals has the ability to ferment lactose with the production of gas under suitable conditions involving restrictive media and elevated temperatures. Since bacteria from other sources are, for the most part, unable to produce gas under such conditions, this criterion has been used to indicate the presence of fecal Coliforms in bodies of water, and the presence of such bacteria has become a standard micro- biological parameter indicating water contamination. The reliability of this test for the marine environment has been questioned however, since the number of Coliforms detectable often fluctuates unpredictaly over short periods of time and may depend upon such factors as cloud cover (1) and ocean currents. The microfauna associated with marine sediments may not be subject to such fluctuations. The purpose of this paper is to indicate a second biochemical parameter which may reflect domestic sewage pollution, and which might be used to confirm or even replace Coliform determinations in the marine environment. The rationaie for this new criterion is related to the urease activity of the enteric Proteus vulgaris, a common bacterium in the intestinal tract of man. Amounts of the enzyme urease can be readily determined due to the ammonia which is produced upon hydrolysis of urea by the enzyme. This study is an attempt to correlate urease activity in marine beach sediments with proximity to ocean sewage outfalls. 240 - 2 - M p MATERTALS AND METHODS Marine Sediments Sands were always obtained where they were barely awash. Samples were taken at both low and high tide. The sediments were collected in 500 ml. wide-mouthed, plastic, screw-capped jars along with approximately 50 ml. of the ambient waters. In the laboratory, the samples were stored at sea water temperature (13-15 C.) until they could be tested. The time elapsed between collection and testing was never more than two hours. Urease Assay - 150 ml. of a test medium consisting of 30.0 grams Nacl and 50.0 grams urea CO(NH2)2 per liter of distilled water was filter ster- ilized and placed in a small-mouthed, 250 ml. glass bottle. Recently collected sand was dried for thirty seconds on a clean blotter, then 50.0 grams were weighed and placed in the test bottle. The ph was adjusted to 9.5 with 0.1 N Naoh and the bottles were incubated at 37.0°C. (+ 0.5° C.) in a water bath. Air which had passed through a cotton filter was bubbled through the test solution at the rate of 130 cc. per minute, and ammonia was trapped in 10 ml. of a saturate boric acid solution containing a mixed indicator (2) held in a 125 ml. Erlenmeyer flask. The amount of ammonia released from the test prep- aration and trapped in the boric acid was determined by titration at intervals of time with 0.01 N HCl. After each titration, a fresh boric acid trap was attached. a4 - 3 - Cultures- is and Escherechia coli used in Cultures of Proteus vulge these studies were obtained through the courtesy of Miss Adeline Larson of the Department of Bacteriology, University of California at Berkeley. Enu eration of Proteus vulgaris and Escherechia coli- The M.P.N. of E. coli was determined by standard methods (3). Difco urea broth was used to test for the presence of P. vulga is in survival experiments and to detect the presence of the genus Proteus in sea water. Plate counts (on Difco nutrient agar) were used to enumerate P. vulgaris. Enzyme Preparation - Jack Bean urease was prepared from Matheson Coleman and Bell tablets by grinding in distilled water. Urease preparations used in subsequent tests were prepared using two 25.0 mg. tablets per ml. of water. The urease was activated by the addition of 0.2 ml. of 14% sodium pyrophosphate solution. ats RESULT Urease Activity of a Jack Bean Urease Preparation - The action of several concentrations of Jack Bean urease upon the test medium was investigated. So as to mimic conditions used in tests upon ambient sands, 50 grams of sand sterilized for four hours (250 C., 15p.s.i.) was included in the preparation. As can be seen from Figure 1, the rate of ammonia evolution is directly related to the enzyme concentration. +47 Urease Acivit of Proteus vulgaris- The urease activity of various numbers of the urease containing bacterium P. vulgaris was investigated. The results of this experiment appear in Figure 2. The rate of urea breakdown can be related to the density of P. vulgaris. Although this relationship requires further quantitation, Figure 3 shows a plot of the rate of the reaction vs. the number of P. vulgaris, as revealed by this experiment. Relationship Between Sediment Size and Urease Activity The effect of sediment particle size on urease activity was investigated using sand obtained 30 feet from the Pacific Grove sewage outfall pipe (Station +10, Figure 6). This sediment was divided into three fractions with the aid of Tyler screens: "coarse" : 3.9 - 2.9 mm., "medium" : 2.9 - 1.9 mm., and "fine" : 2 1.9 mm. Figure 4 presents the results of this determination. A clear relationship between particle size and urease activity in sand from this polluted area is indicated. 26 5- Sands from the west beach of the Hopkins Marine Station (Station k7, Figure 5), a relatively unpolluted area of Monterey Bay, were similariy -r + examined. Only a trace of urease activity was detected in any of these sediment fractions. The slow rises before definitive slopes are established in Figure 4 may be attributed to fluctuations in the air flow, a condition which was corrected at 30 hours. In all subsequent urease tests, the "fine" sediments were used and the air flow was held constant. Urease Activity in Marine Sediments A study of beach sediments collected at various distances from two marine outfalls was undertaken. The entire study area, comprising some five miles of the southern shoreline of Monterey Bay is depicted in Figure 5, with sampling stations 1 - 8 indicated. Figure 6 is an enlargement of the Pacific Grove study area showing the positions of stations 9 - 12 relative to the outfall pipe. Sample stations 1 -6 were located in the vicinity of the Monterey outfall, along a beach made up of homogenously fine (1.9 - 0.9 mm.) sand. This outfall is subtidal and 800 feet from shore. Figure 7 indicates the amount of urease activity detectable on the day these sediments were sampled. Current studies in this area indicate a dominant onshore flow outside the surf zone in this area, and a net flow to the west, in the direction of the Monterey Municipal Wharf No. 2 (4). Urease activity reflects the current pattern as it is understood. Sample station 6lies very close to the aforementioned wharf ; this area receives an additional load of sewage from restaurants and moored boats. p9 Sample stations 9 - 12 were located within a 200 yard radius + This outfall is intertidal, and clearly of the Pacific Grove outfall. visible at times of low tide. Station 9 (Figure 6) lies across a small surge channel from the pipe and receives effluent only at high tide. Station 8 (Figure 5) is a public bathing beach. Figure 8 shows the amount of urease activity observed in sediments collected from these areas. The overlying waters at all stations were cultured for the presence of urease producing bacteria. In all cases these tests were negative. Survival of Escherechia coli and Proteus vulgaris in Sea Water and Se 100 ml. of unfiltered Monterey Bay sea water was placed in a 250 ml. glass bottle. 1.0 ml. of a suspension of either bacterium containing between 1X102 and 1X107 bacteria per mililiter was added, and the preparation was aereated at 200 cc. per minute. The bottles were incubated at sea water temperature (13 - 15° C.). At time intervals, the bottles were vigorously shaken and 5.0 ml. aliquots of liquid were removed for enumeration of surviving bacteria. Figure 9 shows the results of this experiment. The viability of both organisms under these con- ditions seems to be similar. Survival in wet sand was tested by placing 5.0 grams of sterile "fine" sand in 10 X 100 test tubes along with 0.5 ml. of sterile sea water. The tubes were innoculated with a dose of organisms similar to that used above. All tubes were incubated at sea water temperature and at time intervals were tested for growth of urease producing or lactose fermenting bacteria. Both species were able to survive for over a week in moist vuls tris survived for 7.5 sediments. In two separate experiments, ents 5 - 7 - and 8.5 days, while E. coli remained viable for over 9.0 days in both tests. prencer DISCUSSION The amount of urease activity in beach sediments along Monterey Bay appears to be related to proximity to sewage outfalls (from plants utilizing primary treatment processes only). Although in this study no attempt was made to determine the source (s) of this enzyme, the relationship between sediment particle size and urease activity suggests the presence of microorganisms. Further, the urease activity observed in local sediments can be mimicked through the use of suspensions of Proteus vulgaris. This organism shows appreciable survival in marine materials. Urease activity is not a conspicuous property of marine bacteria. Of 130 random bacterial isolates from the Monterey Bay intertidal, only 4 showed the ability to decompose urea (5). Bergey' Manual (6) lists only three marine organisms which show urease activity : Sarcina ureae, Bacterium ammoniagenes, and Bacillus pasteurii. All were originally isolated from sewage, feces, or decomposing urine, but are thought to be able to exist in salt water. Members of the genus Proteus, all of which show urease activity, have been isolated only rarely from air, soil, or fresh water that has not been contaminated with fecal material (7). Therefore, the measurement of urease activity in marine sediments shows promise as a measure of the area contaminated by sewage outfalls. A lag of from 14 to 22 hours before ammonia can be detected is evident in tests involving natural sediments and at all but the highest concentration of P. vulgaris in innoculated sands. Yet only a minimal lag appeared when Jack Bean urease was tested. Attempts to remove this lag by pre-incubation for 24 hours in 3% NaCl before addition of urea, increased air flow, and the addition of appropriate amounts of ammonium chloride all met with failure. Growth of P. vulgaris in nutrient broth containing 1% urea for 24 hours prior to harvest and testing succeeded in lowering the time lag, but only to 8 hours. Therefore, it seems unlikely that the observed lag is caused by a purely adaptive enzyme system. Although natural sediments contain some organic matter, growth must be minimal. No growth permitting substances were included in the urease assay medium. The duration of the lag did not seem to affect the rate of observed urease activity. and this rate could be directly rélated to either the amount of Jack Bean urease or the number of P. vulgaris added. Further research is necessary to determine the source or sources of urease present in the sediments studied. Also, an accurate. simple assay must be developed before urease activity in marine sediments can be used as a convenient test for sewage pollution. This study indicates that such further research is warranted. 2 - 9 SUMMAR! 1. A relationship between the amount of urease activity in marine beach sediments and proximity to sewage outfalls has been demonstrated. 2. The amount of urease activity detectable is directly related to sediment particle size and can be related to the number of Proteus vulgaris added to sterile sediments. vulgaris, a typical urease producer and an inhabitant 3. Proteus of the human gastrointestinal tract, shows substantial survival in marine materials. 2 ADTTON FIGURE CAPTIONS -754 Figure 1. Urease Activity of Jack Bean Urease Preparations. A : 5.0 ml. urease; B : 1.0 ml. urease; C : 0.5 ml. urease; d : 0.1 ml. urease. Figure 2. Urease activity of Proteus vulgaris. A : 1.6 X 1010 bacteria; B : 1.2 X 106 bacteria; C : 1.1 X 104 bacteria. Figure 3. Relationship Between Number of Proteus vulgaris and the Rate of Ammonia Evolution. Figure 4. Relationship Between Sediment Size and Urease Activity. A : "Coarse", 3.9 - 2.9 mm.; B : "Medium", 2,9 - 1.9 mm.; 0 : "Fine", 2 1.9 mm. Figure 5. The Monterey Bay Shorline Study Area. Numbers indicate beach sediment sampling stations. Figure 6. Enlargement of the Pacific Grove Outfall Study Area. Numbers indicate beach sediment sampling stations. + Figure 7. Urease Activity in Marine Beach Sediments Collected in the Vicinity of the Monte Outfall. + Numbers correspond to sampling stations indicated in Figure 5. e. EIGURE CAPIIONS (Cont.) Figure 8. Urease Activity in Marine Beach Sediments Collected in the Vicinity of the Pacific Grove Outfall. Numbers correspond to the sampling stations indicated in Figures 5 and 6. ). and Escherechia coli in Figure 9. Survival of Proteus vulgari Sea Water. Monterey Bay 28 102 L — L 68 51 34 17 10.2 O Time: Hours 40 5 D — 5.1. 3.4 1.7 40 Time: Hours O D S 0.34 0.085 0.17 mg NH, Liberated per Hour U S 13.6 11. 10.2 + 0.9 — — o 6.8 5.1 3.4 .7 20 Lime: Hours a 12 38 scale: — ++ Pacitic 8 Grove 41 Monterey LIEI 51. 1 1 mile t 5 Outfall U S Pacific Grove Outfall 28 6 5 9 2. — 10 D 2 è scale. 10 yards O 2 86 D 20 Time: Hours 5.1 3. 1.7. + 8. — o 6.8 5.1 3.4 1.7 20 i 48 50 Time: Hours o S D5 o — 20 — Vulgaris 41 90 Survival Time: Hours E. Cl 100 110 20 25 0 RTOT ADIV BIBLIOGRAFHI Trumbauer, David S., "A Coliform Bacteria Survey of Monterey Bay off Del Monte Beach", M.S. Thesis, U. S. Naval Posugraduate School, 1966. Kabat, E. and Mayer, M., Experimental Immunochemistry, Charles C. Thomas, Springfield, Illinois, 1961. St Standard Methods for the Examination of Water and Wastewater, Ed. 12 American Public Health Association, Inc., 1965. Stevenson, C.D., "A Study of Currents in southern Monterey Bay", M.S. Thesis, U. S. Naval Postgraduate School, 1964. Phillips, John H., June, 1970, Personal communication. -+5 Bergey's Manual of Determinative Bacteriol ogY, 6 Ed., Williams and Wilkins Co., Baltimore, 1948. Levine, M., 1942, "An Ecological Study of Proteus", J. Bact., 13: 34. JKNC LEDGEMEN I thank Dr. John H. Phillips for encouragement and advice in the course of this work, and Drs. C. B. Van Niel and W.B. Watt for critically reading this manuscript. I further express my gratitude to the faculty, students, and staff of the Hopkins Marine m Station for their enthusiastic support. Ihls work was supported in part by the National Science Foundation Undergraduate Research Program, Grant No. GY - 7244. 6