United States Environmental Protection Agency Health Effects Research Laboratory Cincinnati OH 45268 vvEPA Research and Development EPA-600/S1-81-010 Apr 1981 Project Summary Effects of Halogenated Aromatic Compounds on the Metabolism of Foreign Organic Compounds Gary P. Carlson This work was initiated to extend our previous findings on the induction of xenobiotic metabolism by the halo- genated benzenes. Particular interest' was focused on studying further the relationship between their long-term induction and their storage in body fat. A second objective was to determine if the brominated benzenes caused he- .patic porphyria, similar to that observed with the fungicide hexachlorobenzene. A third aim was to extend our observa- tions to other halogenated aromatic compounds. The final objective was to examine the role of the halogenated benzenes in the enhancement of es- teratic pathways of xenobiotic me- tabolism. Sprague-Dawley rats were used for all experiments involving animals, with the exception of Swiss- Webster mice (Laboratory Supply Co., Indianapolis, IN) being used to mea- sure esterases and pesticide toxicity. In contrast to hexachlorobenzene, the brominated benzenes, including the fully substituted hexabromoben- zene, did not induce hepatic porphyria to any significant degree and did not cause increases in the excretion of porphyrins. A number of trichlorophenols were assessed for their potential to increase xenobiotic metabolism. They did not increase any of the indicators of induc- tion. The brominated diphenyl esters. commercial mixtures used as fire retardants, were found to be potent inducers of xenobiotic metabolism. Administration of low doses for 90 days resulted in effects which were prolonged far beyond the period of administration. The chlorinated di- phenyl ether isomers did not share this potent induction ability. The chlorinated benzo-p-quinones examined were not found to be in- ducers, but did demonstrate a very strong cumulative toxicity. Studies on the distribution and elimination of 1,2,4-trichlorobenzene and 1,2,4-tribromobenzene indicated their prolonged inductive effects were related to storage and slow release, particularly in adipose tissue. Aroclor 1254 caused prolonged increases in xenobiotic metabolism, which could also be enhanced by starvation. The halogenated benzenes induced esterases associated with the metabo- lism of acetanilide, procaineand phen- yl acetate. They were able to protect against the lethality and inhibition of cholinesterase activity associated with the organophosphate insecticides parathion and malathion, plus their active metabolites, paraoxon and malaoxon. This protection was accom- plished by enhancing the metabolic detoxification of these compounds via both exterases and mixed function oxidases. ------- This Project Summary was developed by EPA's Health Effects Research Laboratory, Cincinnati. OH. to announce key findings of the research project which is fully documented in a separate report of the same title (see Project Report ordering information at back.) Introduction There is great interest in the induction of xenobiotic metabolism by halogenated aromatics, and the resultant interactions of these compounds with the actions of- concomitantly administered chemicals or naturally occurring chemicals, such as hormones. Most studies, however, have focused on the polychlorinated biphenyls, polybrominated biphenyls, and chlorinated dibenzo-p-dioxins. Pre- vious studies in our laboratory have indicated that the chlorinated and brominated benzenes are also inducers of xenobiotic metabolism. There are definite structure-activity relationships, with brominated benzenes more active than chlorinated analogs. In general, the greater the degree of halogenation, the greater the degree of induction. Second, effects are prolonged beyond the period of administration of the halogenated benzenes. Observations pertaining to the actions of halogenated benzenes on mixed function oxidases led to the necessity of extending the investigation to; actions on porphyria and esterase activity, examining the relationship between storage of halogenated benzenes and their long-term effects, and exploring the possibility that other halogenated aromatic compounds might also be inducers of xenobiotic metabolism. Hepatic Porphyria Hexachlorobenzene has been ob- served in a number of laboratory species and in humans to cause more porphy- rinogenic effects than do the less chlorinated benzenes. Brominated com- pounds are often more active than chlorinated analogs. Therefore it be- came important to investigate the effects of the fire retardant hexabromobenzene (HBB) on porphyrin synthesis. In the present studies, the effects of two less halogenated benzenes, 1,4-dibromo- benzene and 1,2,4-tribromobenzene, were also examined. Halogenated Aromatics as In- ducers of Xenobiotic Metabo- lism Chlorinated benzenes induce micro- somal enzymes associated with xeno- biotic metabolism. Very little is known of the potential of chlorinated phenols. It appeared possible that the chlorinated benzenes may not be direct inducers of xenobiotic metabolism, but indirectly with conversion to chlorinated phenols. This study was undertaken to determine whether or not trichlorophenols could alter xenobiotic metabolism. Brominated diphenyl ethers are struc- turally similar to several halogenated aromatic compounds known to induce xenobiotic metabolism. These com- pounds are commercial mixtures, making it imperative to compare them with diphenyl ether itself, bis(p-bromodi- phenyl) ether, and the fully brominated diphenyl ether. Chlorinated diphenyl ethers are con- taminants of chlorinated phenols and readily concentrated, for example, by fish. Because of the structural-activity relationships among chlorinated bi- phenyls and chlorinated dioxins, the chlorinated diphenyl ethers were ex- amined. Also, the potency of individual isomers wer,e compared to commercial mixtures of brominated diphenyl ethers. Benzoquinones were examined for effects as inducers. Although they did not qualify in this respect, they were found to have very cumulative toxicity. Benzofurans were very potent inducers of xenobiotic metabolism. Relationship between Induction and Storage Municipal wastewaters contain sev- eral chlorinated and brominated ben- zenes which induce xenobiotic metabo- lism at low doses. Brominated isomers are generally more potent inducers of hepatic microsomal enzymes than chlo- rinated isomers, and the 1,2,4-trihalo- genated compound is a more potent inducer than other isomers. Studies with 1,2,4-trichlorobenzene and 1,2,4-tribromobenzene show these compounds cause enzyme induction, even at low doses. Observations sug- gest storage in body tissues, with slow release after dose termination, thereby prolonging induction of xenobiotic me- tabolism. Numerous studies have shown poly- chlorinated biphenyls induce xenobiotic metabolism. In view of the results with the halogenated benzenes, similar experiments were conducted to deter- mine the length of time PCBs affect xenobiotic metabolism. Esterase Activity Little is known about the ability of halogenated and chlorinated benzenes to alter esterases, except that over 200 pharmacologically active compounds are esters. Therefore hexabromoben- zene was compared to less halogenated benzenes regarding the metabolism of acetanilide, which is biotransformed by both an oxidative reaction and an ester- ase. Hydrolysis of procaine was also studied. Conclusions This study increased in scope and depth as research progressed. The interactions affecting xenobiotic me- tabolism were more complex than origi- nally hypothesized. The more obvious conclusions are stated under subhead- ings; hepatic prophyria, halogenated aromatics, relationship between indue- tion and storage, and esterase activity. Hepatic Porphyria The brominated benzenes did not significantly increase hepatic porphyria. The chlorinated benzenes, other than hexachlorobenzene, had previously been shown to cause minimal increases in liver or urinary porphyrins. Similarly, hexabromobenzene, 1,4-dibromoben- zene, and 1,2,4-tribromobenzene (TBB) caused only small increases in hepatic porphyrins, but did not cause increases in ALA synthetase or in the urinary excretion of porphobilinogen, amino- levulinic acid, or porphyrins. Halogenated Aromatics The trichlorophenols, which in some species are metabolites or contami- nants in halogenated benzenes, were not inducers of xenobiotic metabolism. The brominated diphenyl ethers were potent short-term inducers of xenobi- otic metabolism, as well as potent long- term (90 days) inducers at low doses. Measurements of these ethers in tissue were not made, but it is likely that the. extended period of induction, observable 30 to 60 days after the last dose, was a result of their induction potential and i accumulation in sites such as adipose tissue and liver. ------- Chlorinated diphenyl esters were inferior as inducers of xenobiotic meta- bolism compared to what would be predicted from studies on commercial brominated diphenyl ether mixtures. Diphenyl ether isomers with 2 or 3 chlorines were inactive at the experi- mental doses. However, similar PCBs exhibited low-induction potential. Pen- tabromodiphenyl and octabromodiphen- yl ether mixtures were more active than 4,4'-dibromodiphenyl ether. The more chlorinated the diphenyl ethers, the better their induction. Curiously, deca- chlorodiphenyl ether treatment caused a shift in the P-450 peak toward 448, but did not induce AHH; although 2,4,5, 3',4-pentachlorodiphenyl ether caused both effects. The degree of substitution and position of these groups were both important to determine the extent and type of induction. The toxicity of benzoquinones was very cumulative. A dose far below that of acute toxicity was lethal when given daily for 17 to 30 days. The reasons for this toxicity were not readily apparent. One possibility considered and discarded as erroneous was the occurrence of methemoglobin formation. Both of the chlorinated dibenzofurans induced benzpyrene hydroxylase activity, but dibenzofuran itself did not. Relationship between Induc- tion and Storage Both TBB and TCB induced hepatic microsomal enzymes for at least 16 days, after ending 7 days of a 1 mmolper kilogram dose per day. Excretion data indicated more TBB than TCB was held in the body. Metabolism of trihalogen- ated benzenes to trihalogenated phe- nols has been demonstrated in rabbits, but these were not inducers of xeno- biotic metabolism in rats. The major metabolites in rats appeared to be mercapturic acid derivatives. Halogenated benzenes were observed in tissues. Increased induction resulting from 4 days of starvation, at 6 days after TBB administration was terminated, suggested TBB was mobilized from fat depots. Phenobarbital treatment imme- diately after halogenated benzene dosing appeared to hasten mobilization, meta- bolism, and excretion of either com- pound. This left smaller amounts in the rat to cause" induction at the time of assay. It was clear that both TBB and TCB were retained in the body and released slowly after administration. On an equi- molar basis, TBB led to higher levels of hepatic enzyme induction. These levels were maintained for longer periods and retained to a greater extent in body tissues. TBB was influenced more by starvation than TCB. Starvation accel- erated excretion of halogenated benzene. For phenobarbital treatment, this effect was inferred from the decrease in enzyme levels, compared to those in non-phenobarbital-induced animals. A similar relationship of time and loss of elevated xenobiotic metabolism was seen for polychlorinated biphenyls. This induction was also increased by starva- tion. Administration of the commercial polychlorinated biphenyl mixture, Aroclor 1254, resulted in increases in xeno- biotic metabolism. This persisted for as long as 4 to 5 months. Esterase Activity Halogenated benzenes induced xeno- biotic metabolism by increasing ester- ase activity. This applied to phenyl acetate, acetanilide, and procaine in- dicating broad induction of oxidative, reductive, conjugative, and esteratic metabolic reactions. The compounds most active in inducing arylesterase activity in the liver were 1,2,4-TCB and 1,2,4-TBB, shown throughout our studies as better inducing isomers. Trihalogenated benzenes decreased the inhibitory effect of malathion on cholinesterase activity in the brain, and to a lesser degree in red blood cells, but not in liver or plasma. It therefore appeared that halogenated benzenes protect against malathion or malaoxon toxicity by increasing the detoxification rate. The trihalogenated benzenes de- creased the inhibitory effect of paraoxon on cholinesterase activity in the brain and liver, but not in plasma or red blood cells. Thus, it appears that the halo- genated benzenes protect against para- oxon and probably parathion toxicity by increasing the detoxification rate of the pesticides. Results Basically, xenobiotic metabolism was induced by chlorinated and brominated benzenes. This induction affects both mixed function oxidases and esterases. Porphyria was not caused by chlori- nated benzenes, except for hexachloro- benzene. Administration of 1,2,4-tribromoben- zene caused a significant increase in liver weight, even at the lowest level of 50 mg/kg in 30 days. An increase m porphyrin content in the liver did not appear until 90 days (Table 1). The Table 1. Dose (mg/kg) 0 50 100 200 0 50 100 200 0 50 100 200 0 50 100 200 Effect of 1,2,4-Tribromobenzene PO on Porphyrin Production and Excre- tion in Female Rats Liver porphyrins Urine porphyrins Liver wt (g) (ng/g) (ng/24 h) 6.46 ± 0.34s 8.94 ±0.56" 8.94 ± 0.56" 9.52 ±0.30° 7.30±0.21a 9.16 ±0.42" 9.96±0.37ti 9.72 ±0.50b 6.44 ± 0.26s 8.97 ± 0.43" 10.07 ± 0. 18* 12.20±0.88C 7.27 ± 0.38* 11.11 ±0.80b 12.71 ±0.84* 15.18 ±0.23C 30 days of administration 526 ± 49* 602 ± 90* 620 ± 66a 471 ±22* 60 days of administration 156 ± 64" 251 ± 75a 285 ± 78a 2.85 ±54* 90 days of administration 468 ± 12* 629 ± 2d° 700 + 17C 711 ±26C 120 days of administration 411 ± 13* 560 ± 33b 646 ± 28b'c 682 ± 45C 2.1 9 ±0.28* 2.29 ±0.69* 2.40 ±0.13* 2.53 ± 0.27* 1.92 ±0.58* 1.61 ±0.21* 1.77 ±0.48* 2.42 ± 0.54* 1.41 ±0.23*'* 1.17 ±0.18* 2.43+0.59" 1 .88 ± 0.35*'" 1.75 ±0.39* 1.81 ±0.42* 2.27 ± 0.56* 2. 13 ± 0.40* cVa/ues with same superscript are not significantly different fp>0.05J. ------- increases were dose dependent, small and very similar to those previously observed with 1,2,4-trichlorobenzene. Animals treated with 200 mg/kg of 1,2,4-tribromobenzene for 120 days were slightly smaller than the controls, but not statistically significant. They were discolored and their ears brown and ragged in appearance. Thus, al- though the animals looked unhealthy, porphyria was not the problem. Hexabromobenzene was not shown to share the extreme porphyrinogenic properties of its chlorinated analog. The less brominated compounds were simi- lar to the chlorinated analogs in being very weak porphyria inducers. Table 2. Effect of Trichlorophenols In Vitro on p-Nitroanisole O-demethylation and EPN Detoxification p-Nitroanisole 0-demethylation0 EPN detoxification0 (fjg p-nitrophenol/ (t*g p-nitrophenol/ Treatment 50 mg/30 min) 50 mg/30 min) Control" 2,3,5-Trichlorophenof1 2,3,6- TrichlorophenoP 2,4,5- TrichlorophenoP 2, 4, 6- TrichlorophenoP 6. 64 ±0.68 0.57 ± 0.21" 2.02 ±0.22" 0.61 ±0.24" 2.33 ± 0. 19" 8.39 ± 0.34 4. 02 ± 0.43d 4.58 ± 1.14" 3.88 ± 0.47" 4.03 ± 1.1 '7" *50 /j( benzene added ^Compound added in 50 /jl benzene to give final concentration of 2.5 x 10'* M. cMean ± S.E. of 4 experiments. ^Significantly different from control (p<0.05). Halogenated Aromatics Chlorinated Phenols— All of the experimentation resulted in an excess of negative data for halogena- ted aromatic induction of xenobiotic metabolism. These compounds did not induce EPN detoxification, NADPH cytochrome c reductase, or cytochrome P-450. Specific compounds, such as 1,2,4-trichlorobenzene and 1,3,5-tri- chlorobenzene, did not depend upon biotransformation to trichlorophenols for induction ability, so they must be regarded as inactive metabolites. In vitro the trichlorophenols were inhibitors of EPN detoxification and p- nitroanisole demethylation (Table 2). For p-nitroanisole demethylation, the inhibition was noncompetitive. The 2,3,5- and 2,4,5-isomers were the most potent. Brominated Diphenyl Ethers— The brominated diphenyl ethers, including the complex commercial mix- tures of pentabromodiphenyl and octa- bromodiphenyl ethers, (Table 3), caused liver enlargement (Table 4). Pentabro- modiphenyl ether gave the largest increase of 64%. A similar pattern was seen with both NADPH cytochrome c reductase and cytochrome P-450 using pentabromodiphenyl ether.The effect of pentabromodiphenyl ether was greater than that of octabromodiphenyl ether, which was equal to bis(p-bromodiphenyl) ether. Decabromodiphenyl ether was without effect. This was similar to the poor induction properties of fully bromi- nated benzene. When a series of enzyme activities were determined, pentabromodiphenyl ether and octobromodiphenyl ether Table 3. Composition of Bromodiphenyl Ethers Mol wt Percent of bromodiphenyl Compound 02 4 Diphenyl ether 98 Bis (p-bromophenyl) ether * Pentabromodiphenyl ether 24. 6 Octabromodiphenyl ether Decabromodiphenyl ether 5 6 58.1 13.3 1.1 8.5 7 8 2.6 0.3 45.1 30.7 con- glom- erate 9 10 M"' "" 170 328 0.2 0.8 564 13.0 1.6 766 " 959 "Reagent grade. "High purity. Table 4. Effect of Bromodiphenyl Ethers on Liver wt./Body wt., NADPH Cyto- chrome c Reductase and Cytochrome P-450 Cytochrome c reductase, nmol Treatment" Control Diphenyl ether Bis (p-bromophenyl) ether Pentabromodiphenyl ether Octabromodiphenyl ether Decabromodiphenyl ether Liver wt. inn" Body wt. 3.80 ± 0.1 2C 4.03 ± 0. 13C'" 4.48 ±0.1 2** 6.25 ± 0.25' 5.54 ± 0.259 4.75 ±0.10' Cyto. c reduced/ min/mg protein* 151 ± 26C 134 ± 25° 238 ± /3d* 315 ±20' 281 ± 34''' 175± 5C" Cytochrome P-450 nmol/mg protein* 0.79 ± O.O5C 0.71 ±0.04° 1.61 ± 0.09" 2.56 ±0.1 7* 1.86 ±0.14" 0.91 ± 0.05° '0.1 mmol/kg/day for 14 days po. Controls received corn oil. tiMean ± S.E. for 4 rats. °~a Values with the same superscript are not significantly different from one another (p >0.05). were the more potent inducers, giving large increases in both EPN detoxifica- tion and p-nitroanisole demethylation (Table 5). They were the only compounds which caused increased conjugation of naphthol. Benzo(a)pyrene hydroxylase was increased only by pentabromo- diphenyl ether. Administration of 6.25, 12.5 or 25 /ymol/kg daily of the pentabromo- diphenyl ether and octabromodiphenyl ether over a 90-day period resulted in large increases in EPN detoxification, p- nitroanisole demethylation, and cyto- chrome P-450 (Table 6). Pentabromo- diphenyl ether did not cause large ------- Table 5. Effect of BromodiphenylEthers on EPNDetoxification, p-Nitroanisole Demethylation, Benzo(a)pyreneHydroxylase, and UDP-Glucuronyltransferase p-Nitroanisole UDP-Glucuronyl- Treatment* EPN detoxification, fjg p-nitrophenol/ 50 mg/30 min° demethylation, jjg p-nitrophenol/ 50 mg/30 min° transferase, nmol napthol/ mg protein/min* Benzola)pyrene hydroxylase, nmol/mg protein/10 min* Control Diphenyl ether Bis (p-bromophenyl) ether Pentabromodiphenyl ether Octabromodiphenyl ether Decabromodiphenyl ether 6.60 ± 1.1 2C 11.08± 1.72" 10.42± 1.24c'a 15.98 ± 1.22* 16.30 ± i.ir 7.10 ±0.85° 6.33 ±0.7 8^ 5.68 ± 0.85° 9.25±0.75a 43.81 ± 1.93e 17.84 ±0.41' 8.68 ± 1.06c'a 6.23 ± 1.25C 5.76±0.73C 7.65 ± 1.12c'a 10.87 ± 1.74a 10.36 ± 1.14a 5.97 ±0.98C 6.79±0.54C 4.44±0.55C 4.86±0.74C 11.01 ± 1.07a 6.01 ± 1.06C 5.52 ± 0.61C aO. 1 mmol/kg/day for 14 days po. Controls received corn oil. *Mean ± S.E. of 4 rats except: 3 rats in pentabromodiphenyl ether group in liver wt./bodywt. and glucuronyltransferase and 2 for that group in benzo(a)pyrene hydroxylase. c~'Values with the same superscript are not significantly different from one another (p >0.05). Table 6. Effect of Pentabromodiphenyl Ether and Octabromodiphenyl Ether on EPN Detoxification, p-Nitroanisole Demethylation, Cytochrome c Reductase Activity, and Cytochrome P-450 Content p-Nitroanisole Cytochrome c Dose EPN detoxification, demethylation, reductase, nmol fjmol/kg/day tig p-nitrophenol/ fjg p-nitrophenol/ Cyto. c reduced/ Cytochrome P-450 for 90 days 50 mg/30 min 50 mg/30 min min/mg protein nmol/mg protein 0 9.6±0.3a 6.25 17.7 ±0.5* 12.5 2/.5±0.6c 25 26.5 ±0.7* 0 9.7±0.5a 6.25 21.3 ±1.1" 12.5 26.9 ±2.2* 25 37.1 ±2.0C Pentabromodiphenyl ether 7.6 ±0.1a 25.6 ± 1.2* 34.6 ± 1.1C 50.1 ± 1.3d Octabromodiphenyl ether 10.0 ± 0.4a 20.9 ± 1.8* 27.3 ± J.3C 38.4 ± 1.9* 88 ± 6* 117± 9* 120 ± 5b 138 ± 7* 171 ± 11a 197 ± 9a 196 ± 18a 208 ± 11a 0.60 ± 0.04a 1.02 ±0.06* 1.1 6 ±0.07* 1.1 4 ±0.07* 1.04 ±0.10" 1.56 ± 0. 13b 1.27 ± 0. 16at> 1.46 ±0.09* Values with same superscript are not significantly different from one another (p > 0.05). increases in NADPH Cytochrome c re- ductase, nor did Octabromodiphenyl ether even at the highest dose level. When administered for 90 days, even the lowest dose of pentabromodiphenyl ether (0.78 /umol/kg daily) caused in- creases in EPN detoxification, p-nitro- anisole demethylation, NADPH cyto- chrome c reductase, and cytochrome P- 450 (Table 7). For EPN detoxification andp-nitroanisole demethylation, there was a clear-cut dose response relation- ship. Chlorinated Diphenyl Ethers— Chlorinated isomers proved to be poor inducers of xenobiotic metabolism when compared to the very potent induction ability of the polybrominated diphenyl ethers. Only two of the isomers caused increases in aryl hydrocarbon hydroxylase, 3,4,2,4-tetrachlorodiphenyl ether and 2,4,5,3',4'-pentachloro- diphenyl ether. When microsomal NADPH cytochrome c reductase activity was measured, only decachlorodiphenyl ether caused an increase. This compound caused the largest increase in cytochrome P-450 content. Small but significant eleva- tions were also observed in rats treated with both 2,4,5,2',4',- and 2,4,5,3',4'- pentachlorodiphenyl ether. Dibenzofurans— Dibenzof uran and its chlorinated deri- vatives did not increase EPN detoxifica- tion or NADPH cytochrome c reductase. Benzypyrene hydroxylase activity was induced by both chlorinated dibenzo- furans, but not by the parent compound. Both chlorinated dibenzofurans increased cytochrome P-450 content, although the increase was not statistically signifi- cant with the 2,8-dichloro isomer. Both also caused a shift to 448.2 nm for the peak of cytochrome P-450 absorbance. These factors strongly support the contention that the compounds are inducers of the 3-methylcholanthrene type. Relationship between Storage and Induction Halogenated Benzenes— Due to the large difference in molecu- lar weight of the halogenated benzenes tested previously they were compared on a molar basis. A dose of 1 mmol/kg/ day for 7 days was used in all studies. This dose caused a high level of induction on day 1 after the 7 days with both TBB and TCB (Figures 1 and 2). EPN detoxifi- cation levels were approximately twice as high as control values 16 days after ------- the last dose of TBB, suggesting induc- tion may have occurred beyond day 16 of recovery. The decline in induction was slower with TBB than TCB. Duration of Induction by PCB and Influence of Starvation— The results of Aroclor 1254 adminis- tration were as expected. EPN detoxifi- cation andp-nitroanisole demethylation were elevated four- and ten-fold, respec- tively, 1 day after the last (14th) dose. Measurements of microsomal NADPH cytochrome c reductase and cytochrome P-450 revealed similar results. Cyto- chrome P-450 increases were observed for the first 71 days, due to Aroclor alone, before returning to control levels at later time periods. Changes in NADPH cytochrome c reductase, although not as large, followed a similar time course. Esterase Activity Acetanilide and Procaine Esterase— Halogenated benzenes induced the metabolism of acetanilide and procaine by increasing esterase activity. This was true of the less halogenated benzenes, as well as hexachlorobenzene. These compounds were broad inducers of oxidative, reductive, conjugative, and esteratic metabolic reactions. Esterases and Pesticide Toxicity The 1,4-dihalogenated benzenes and hexabromobenzene had little effect on the lethality of malathion. Both trihalo- genated benzenes increased the LD50 values, which indicated a decrease in lethality. The trihalogenated benzenes also decreased the toxicity of the active metabolite of malathion, malaoxon, approximately two-fold. Even greater protection against lethality was demon- strated with parathion. The effect of the trihalogenated ben- zenes on cholinesterase activity in the brain, liver, plasma, and red blood cells was measured, since toxicity of the organophosphates is related to inhibition of cholinesterase. Malathion caused a decrease in cholinesterase activity in the brains of control mice, but not in those treated with 1,2,4-trichlorobenzene. The decreases were similar between control and treated groups in other tissues. Similarly, 1,2,4-tribromobenzene treatment prevented the decrease in brain cholinesterase following malathion treatment, and slightly decreased the malathion effect on red blood cells. Measurement of carboxylesterase activity with malathion as the substrate revealed that 1,4-dichlorobenzene, 1,2,4-trichlorobenzene, hexachloroben- zene, 1,4»dibromobenzene, 1,2,4-tri- bromobenzene, and hexabromobenzene all increased carboxylesterase activity in the liver. A similar trend was seen in plasma. The trihalogenated benzenes caused the largest increases in activity. Paraoxon dearylation was examined since halogenated benzenes might pro- tect against paraoxon toxicity by increas- ing its metabolism. Plasma esterase was not altered by 1,4-dihalogenated or hexahalogenated isomers. Trihalogenated isomers actually decreased this activity. As expected, there was little activity in either control or treated animals in the 105,000 x g liver supernatant. Microso- mal esterase activity was increased by 1,2,4-trichlorobenzene, hexachloroben- zene, and hexabromobenzene, but was inhibited by 1,4-dibromobenzene and 1,2,4-tribromobenzene. However, the mixed function oxidase dearylation in liver microsomes was increased eightfold by 1,2,4-tribromobenzene and to a lesser extent by 1,4-dichlorobenzene, hexachlorobenzene and 1,2,4-trichloro- benzene. Arylesterase— None of the halogenated benzenes tested caused any increase in serum arylesterase activity. These compounds included 1,2,4-trichlorobenzene, 1,3,5- trichlorobenzene, hexachlorobenzene, 1,2,4-tribromobenzene, 1,3,5-tribromo- benzene, and hexabromobenzene. In- creased activity was observed in the liver after 1,2,4-trichlorobenzene, hexa- chlorobenzene, 1,2,4-tribromobenzene, and 1,3,5-tribromobenzene. The com- pounds, therefore, associated through- out this research project as the better Table 7. Effect of Pentabromodiphenyl Ether on EPN Detoxification, p-Nitroanisole Demethylation, NADPH Cytochrome c Reductase, and Cytochrome P-450 p-Nitroanisole NADPH Cytochrome Dose EPN detoxification, demethylation, c reductase, nmol fjmol/kg/day i*g p-nitrophenol /jg p-nitrophenol Cyto. c reduced for 90 days 50 mg/30 min 50 mg/30 min min/mg protein Cytochrome P-450, nmol/mg protein 0 0.78 1.56 3.13 0 0.78 1.56 3.13 0 0.78 1.56 3.13 A dministration 5.8 ±0.1* 5.5 ±0.4* 165 ±10* 8.1 ±0.2* 9.7 ±0.6" 215 ±13* 8.9 ±0.3* 72.2 ±0.8° 194 ± 27a'b 11.4±0.6C 16.9 ±0.4" 209 ±14*'* Administration plus a 30-day recovery period 6.0 ±0.2* 5.5 ±0.4* 128 ± 9* 7.2 ± 0.2* 7.5 ± 0.3* 138 ± 7a'b 7.4 ± 0.5* 7.9 ± 0.4* 138 ± 8a'b 9.1 ±0.2C 10.7±0.9C 152 ± 6b Administration plus a 60-day recovery period 6.3 ± 0.3* 3.6 ± 0.3* 155 ± 9* 6.4 ± 0.3* 3.8 ± 0.2* 162 ± 14* 7.7 ±0.3* 4.6 ±1.0* 148± 7* 7.5 ±0.4* 5.6 ±0.3° 772± 8" 7.05 ± 0.02* 1.41 ±0.07* 1.26 ±0.06* 1.25 ±0.09* 0.80 ± 0.07* 0.87 ± 0.04* 0.96 ± 0. 18* 0.90 ± 0. 13* 0.82 ± 0.07* 0.85 ±0.1 2a 0.85 ± 0.06* 0.82 ± 0.06* a-d For each time period, values with same superscript are not significantly different from one another (p > 0.05). ------- 500 400 o 300 § 200 ;oo 0 * * fS Days after— Last Dose 6 11 16 EPN Detoxification 1 6 11 16 p-Nitroaniso/e Demethylation 6 11 1t Cytochrome c Reductase 6 11 16 Cytochrome P-450 Figure 1. Decline with time in rats receiving TBB(1 mmol/kg/day for 7 days po. Asterisk indicates values significantly different from controls IP 0.05). Average control values: EPN detoxification, 5.9 ±0.2 (jg p-nitrophenol/50 mg/30min; p-nitroanisole demethylation, 5.1 + 0.3 (jgp-nitrophenol/SOmg/30 min; NADPH-cytochrome c reductase, 118±6 nmol cytochrome c reduced/min/ml protein; P-450. 0.85 + 0.07 nmol/mg protein. inducing isomers, were also the most active in inducing arylesterase activity in the liver. Recommendations The results of these studies support our earlier findings that many of the halogenated aromatic compounds are capable of altering the metabolism of foreign organic compounds. These reactions'include the mixed function oxidases, conjugative enzymes, and esterases. A critical area in need of additional research is the relationship of storage to prolonged induction. In our studies on halogenated ben- zenes and PCBs, the period of increased xenobiotic metabolism lasted far beyond the period of administration of the com- pounds. The halogenated benzenes were able to correlate this activity with storage, especially in adipose tissue. This is also suggested, but not proven, for PCBs. More studies on PCBs and brominated diphenyl ethers*are needed. The chlorinated benzofurans were found to be inducers, supporting pre- vious findings. The chlorinated benzo- quinones did not prove to be inducers, but did show highly cumulative toxicity. The reasons for this are not known, but are evidently not related to methemoglo- bin formation or liver damage. The dramatic nature of this cumulative toxicity indicates subsequent study is needed to ascertain the mechanism involved. The brominated diphenyl esters were among the most potent inducers tested in our laboratory. Little is known about their pharmacokinetic properties or effects, other than those associated with xenobiotic metabolism. Additional studies are needed to quantify the tissue distribution, metabolism, and rate of elimination. These complex mixtures of isomers need to be identified to ascertain the active ones causing the induction process. ------- 500 400 300 § 0) 0. 200 700 fc i A Days after— Last Dose 1 6 11 16 EPN Detoxification 1 11 16 p-Nitroaniso/e Demethylation 1 6 11 16 Cytochrome c Reductase 6 11 16 Cytochrome P-450 Figure 2. Decline with time in rats receiving TCB. Average control values: EPN detoxification, 6.3 ±0.4 fjg/50 mg/30 min; p-nitroanisole demethylation. 5.1 ± 0.2/jg/50 mg/30 min; NADPH-cytochrome c reductase, 118 + 6 nmol/min/mg; P-450, 0.85 + 0.07 nmol/mg. Gary P. Carlson is with the Department of Pharmacology and Toxicology, Purdue University, West Lafayette, IN 47907. Merrel Robinson is the EPA Project Officer (see below}. The complete report, entitled "Effects of Halogenated Aromatic Compounds on the Metabolism of Foreign Organic Compounds," (Order No. PB81 -152 522; Cost: $9.50, subject to change) will be available only from: National Technical Information Service 5285 Port Royal Road Springfield, VA 22161 Telephone: 703-487-4650 The EPA Project Officer can be contacted at: Health Effects Research Laboratory U.S. Environmental Protection Agency Cincinnati, OH 45268 i US GOVERNMENT PRINTING OFFICE 1981-757-064/031Z ------- •of - CTT Ui 71 Cft o -1 -~ -> -4 ar o -< i >r (o : n < I! p = 1J 3 3 a a to O) oo CO O W- cn 6 O I'll I ------- |