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Comparison of the neuropeptide y receptor in the rat brain and intestine, b

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In addition we have cross-linked radiolabelled NPY to its intestinal receptor, and compared the resulting complexes observed on SDS-polyacrylamide gel electrophoresis with the pattern ob

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Comparison of the Neuropeptide

IAN L TAYLOR, PETER J MANNON, GREGORY G HEINTZ,

Durham, North Carolina 27710

INTRODUCTION

Neuropeptide Y (NPY), together with pancreatic polypeptide (PP) and peptide YY

(PYY), constitute a family of structurally related peptides all of which contain 36 amino

acids and have a similar tertiary structure.'-4 NPY has neurotransmitter and neuromod-

ulator functions in the central, peripheral and enteric nervous Central admin-

istration of NPY increases food intake,s produces hypotension, bradypnea and EEG

synchronization.6 and shifts circadian rhythm^.^ NPY applied to intestinal mucosa

mounted in Ussing chambers inhibits ion transport with an EC,, of 10-30 nM;*." it

inhibits transmural electrical potential and short circuit current, increases mucosal-to-

serosal Na+ and C1- fluxes, and reduces serosal-to-mucosal C1- fluxes.*-" This inhib-

itory action is only demonstrable when NPY is added to the serosal (but not luminal) side

of the intestinal epithelium These observations correlate with the localization of NPY to

intrinsic nerves within the enteric nervous system that end in close proximity to the

laterobasal region of the intestinal epithelial cell

We have used a recently described method that allowed isolation of intestinal serosal

latero-basal membranes (LBM) free from contamination with luminal brush border mem-

branes (BBM), and intracellular endoplasmic reticulum (ER) and Golgi vesiclesi2 to

demonstrate that NPY binds preferentially to the serosal LBM of the enterocyte In

addition we have cross-linked radiolabelled NPY to its intestinal receptor, and compared

the resulting complexes observed on SDS-polyacrylamide gel electrophoresis with the

pattern observed after cross-linking the brain receptor

T h i s project was supported by funds from the Department of Veterans Affairs Dr Toan Nguyen

is the recipient of a FIRST award (DK zyxwvutsrqponmlkjihgfedcbaZYXWVUTSRQPONMLKJIHGFEDCBA40506) and Dr Ian Taylor of a zyxwvutsrqponmlkjihgfedcbaZYXWVUTSRQPONMLKJIHGFEDCBAR01 Grant (DK 38216) from

the National Institutes of Health

bAbbreviations used: NPY: neuropeptide Y; PYY: peptide YY; PP: pancreatic polypeptide; HPLC:

high performance liquid chromatography; ER: endoplasmic reticulum; LBM: laterobasal membranes;

BBM: brush border membranes; HEPES: N-2-hydroxyethylpiperazine-N'-2-ethanesulfonic acid;

BSA: bovine serum albumin; DlT: dithiothreitol; SDS: sodium dodecyl sulfate; PMSF: phenylme-

thylsulfonyl fluoride; DSS: disuccinimido suberate; EDTA: ethylenediaminetetraacetic acid; PAGE:

polyacrylamide gel electrophoresis; lacto-NPY ,: zyxwvutsrqponmlkjihgfedcbaZYXWVUTSRQPONMLKJIHGFEDCBAlactoperoxidase labelled NPY contained in the first

radioactive peak isolated on HPLC; IODO-GEN-NPY,: IOW-GEN labelled NPY contained in the

second radioactive peak isolated on HPLC; B-H-NPY: Bolton-Hunter labelled NPY

48

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TAYLOR zyxwvutsrqponmlkjihgfedcbaZYXWVUTSRQPONMLKJIHGFEDCBAel zyxwvutsrqponmlkjihgfedcbaZYXWVUTSRQPONMLKJIHGFEDCBAal.: NPY RECEPTOR zyxwvutsrqponmlkjihgfedcbaZYXWVUTSRQPONMLKJIHGFEDCBA49

METHODS

Chemicals and Reagents zyxwvutsrqponmlkjihgfedcbaZYXWVUTSRQPONMLKJIHGFEDCBA

Synthetic NPY, PYY and PP were urchased from Peninsula Laboratories (Belmont,

gland Nuclear (specific activity 2200 Cilrnmol) For some experiments one or more of the

five tyrosines in NPY was radioiodinated using lactoperoxida~e'~ or IODO-GEN, l 4 and

the resulting radiolabelled species purified on high performance chromatogra h

from Amersham C o p (Arlington Heights, IL), polyacrylamide gel electrophoresis re-

agents from Bio-Rad (Richmond, CA) and molecular weight standards for gel electro-

phoresis from Pharmacia (Pistcataway, NJ) Triton-X-100 was from J.T Baker (Phil-

lipsburg, NJ), and all the protease inhibitors (antipain, chymostatin, pepstatin, leupeptin

phenylmethylsufonyl fluoride (PMSF), ovomucoid trypsin inhibitor, bacitracin, aproti-

nin) were from Sigma The crosslinking agent disuccinimido suberate (DSS) was pur-

chased from Pierce (Rockford, IL) X-ray film (XAR-2) was from Eastman Kodak (Roch-

B

Intestinal Cell Membrane Fraclionatton

Membranes were prepared from intestinal epithelial cells dissociated from the jejunum

and ileum of fasted male Sprague Dawley rats (-300 gm) using previously described

methods.', Protease inhibitors were added during cell dissociation (2.5 kg/d each of

antipain, chymostatin, pepstatin, leupeptin, ovomucoid trypsin inhibitor, and 1 mM

PMSF) and during the first homogenization (25 kglml each of antipain, chymostatin,

pepstatin, leupeptin, ovomucoid trypsin inhibitor, and 1 mM PMSF) Differential cen-

trifugation was used to yield a pellet (P,) that contained mostly ER-Golgi and LBM;

precipitation of ER-Golgi with 8 mM CaCI, combined with differential centrifugation

yielded a pellet (P,) that contained mostly LBM and BBM The membrane populations

contained in P, and P, were subsequently separated by centrifugation (85,000 x g for

14-16 hr) in linear sorbitol gradients (25-606 w/v) Fractions (2 ml) were collected from

the top of the gradient and assayed for protein (Coomassie blue dye binding using reagents

obtained from Bio-Rad), marker enzymes (aryl esterase for ER-Golgi; K-stimulated phos-

phatase for LBM; sucrase for BBM), and for NPY binding In other experiments, all the

membranes contained in the whole homogenate were subjected to calcium precipitation to

increase the yield of LBM

Binding of NPY to Membrane Fractions

Aliquots (200 pl) of the gradient fractions derived from the P, pellet were incubated

for I hr at room temperature with trace amounts (10-50 pM) of labelled NPY dissolved

in 800 p1 of 10 mM NaH,PO,-K,HPO,, 0.2 TIUlml aprotinin, 0.5% bovine serum

albumin (BSA), 0.05% bacitracin, pH 7.0 When NPY was labelled with lactoperoxidase

or iodogen, Triton X-100 was added to the incubation buffer at a final concentration of

0.006% to minimize the nonspecific binding of labelled peptide to the polypropylene

assay tubes At the end of the incubation period, the membrane-bound ligand was sep-

arated by centrifugation at 27,500 x g for 30 min at 4°C Total radioactivity at the

beginning of the experiment and in the membrane pellet was determined and specific

binding corrected for nonspecific binding (number of apparently bound counts observed

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50 zyxwvutsrqponmlkjihgfedcbaZYXWVUTSRQPONMLKJIHGFEDCBAANNALS NEW zyxwvutsrqponmlkjihgfedcbaZYXWVUTSRQPONMLKJIHGFEDCBAYORK ACADEMY OF SCIENCES zyxwvutsrqponmlkjihgfedcbaZYXWVUTSRQPONMLKJIHGFEDCBA

in the presence of 1 pM unlabelled NPY.) Scatchard analysis was performed using the

EBDA/LIGAND program (originally written by P J Munson and D Rodbard and mod-

Cross-Linking of NPY to Intestinal Membranes

Membrane fractions were pooled according to their enzyme markers, washed twice,

NaCl, 0.5 mM EDTA, 5 mM histidine-imidazole, pH 7.4 The membrane pools were

frozen in liquid nitrogen, and stored at -70°C Binding studies were performed as in the

prior section except that 100 pg of membrane protein was used for each assay The

membrane pellet obtained after allowing radiolabelled NPY to bind was washed (centrif-

ugation at 27,500 x g for 30 min) and finely resuspended with a 25 gauge needle in 1 ml

of 60 mM HEPES, pH 7.5 Cross-linking was initiated by the addition of 10 p1 of 20 mM

DSS dissolved in dimethyl sulfoxide (final concentration -0.2 mM), and the membranes

were then incubated for 15 min at 4°C on a rotary shaker The crosslinking was stopped

by the addition of 2 ml of cold 60 mM HEPES, 60 mM ammonium acetate, pH 7.5 The

membranes were centrifuged at 27,500 x g for 30 min and washed with 62.5 mM

Tris-HC1, pH 6.8, prior to SDS polyacrylamide gel electrophoresis

Prepamlion zyxwvutsrqponmlkjihgfedcbaZYXWVUTSRQPONMLKJIHGFEDCBAof Bm‘n Membranes, NPY Binding, and Cross-Linking

Male Sprague-Dawley rats (200-250 g) were anesthetized with intraperitoneal pen-

tobarbital, decapitated and the brains rapidly removed The cerebellum and white matter

were dissected away from the cortex, and the cortex then homogenized with a glass-

on-glass Dounce homogenizer (6 passes pestle B, 10 passes pestle A) in 10 ml of ice-cold

“Buffer A” (137 mM NaCl, 2.68 mM KCl, 2.05 mM MgCl,, 1 mM EDTA, 0.1 mM

PMSF, 0.1% bacitracin, 0.1% glucose, 0.2 TIU/ml aprotinin and 20 mM HEPES, pH

7.4) The homogenate was brought to a volume of 30 ml with “Buffer A” and centrifuged

at 14.000 x g and 4°C for 15 min The resulting pellet was washed and resuspended in a

final volume of 4.5 ml buffer A Binding and cross-linking experiments were performed

using the same methods described above for the intestinal membrane except that binding

was performed in “buffer A” supplemented with 0.005% Triton X-100 and 0.2% BSA

and cross-linking was performed with 1 mM DSS

SDS-Polyacrykuni& Gel Electrophoresis and Autoradiogmphy

Cross-linked membrane pellets were resuspended in 150 p1 of a solubilization buffer

containing 2% SDS, 10% w/v glycerol, 1 mM EDTA, 10 mM DlT, bromphenol blue and

pyronin Y as dye indicators, and 0.0625 M Tris-HC1, pH 6.8; D l T was omitted when

using DSP Following incubation in a shaking water bath at 37°C for 30 min, the resulting

membrane suspension, or the solubilized material contained in the supernatant after

centrifugation at 18,000 x g and 22°C for 5 minutes was studied by 10% polyacrylamide

gel electrophoresis and autoradiography as outlined by Nguyen et a1.’5v16 In some ex-

periments, radioactive bands were cut from the dried gels using the autoradiogram as a

template and counted directly

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TAYLOR zyxwvutsrqponmlkjihgfedcbaZYXWVUTSRQPONMLKJIHGFEDCBAef zyxwvutsrqponmlkjihgfedcbaZYXWVUTSRQPONMLKJIHGFEDCBAal.: NPY RECEPTOR

RESULTS zyxwvutsrqponmlkjihgfedcbaZYXWVUTSRQPONMLKJIHGFEDCBA51 zyxwvutsrqponmlkjihgfedcbaZYXWVUTSRQPONMLKJIHGFEDCBA

Binding of NPY to Pooled Membrane Fractions zyxwvutsrqponmlkjihgfedcbaZYXWVUTSRQPONMLKJIHGFEDCBA

exhibited dependence upon time and the amount of membrane protein added In contrast

the nonspecific binding to BBM observed in the presence of 10 pM NPY was actually

higher than the total binding in the absence of unlabelled NPY Half-maximal inhibition

of labelled NPY binding to LBM was observed with 20-50 nM unlabelled NPY Scat-

(K, 15 nM, B,,, 30 p m o l e h g of membrane protein) and a two-binding-site model (K,

5.3 nM, B,,, 4 pmolehg of membrane protein [Site I]; K, 29 nM, B,, 36 pmole/mg

of membrane protein [Site 21)

When NPY was radiolabeled with lactoperoxidase or IODO-GEN and purified by

HPLC, at least 3 major peaks corresponding to different sites of iodination were observed

(NPY has 5 tyrosine residues that can potentially be iodinated) Sheikh er af l4 previously

demonstrated that, following IODO-GEN radioiodination, NPY contained in the first

radioactive peak (IODO-GEN-NPY ,) on HPLC was monoiodinated at tyrosine residue 1;

NPY contained in the second radioactive peak (IODO-GEN-NPY,) was monoiodinated at

tyrosine residue 36; and NPY contained in the third major peak or radioactivity (IODO-

GEN-NPY,) was iodinated at both positions 1 and 36

We determined whether the preferential binding of radiolabeled NPY to LBM was

dependent on site of iodination of the ligand IODO-GEN-NPY , bound well to LBM

(11% of the initial amount of NPY added specifically bound to 100 p g of membrane

protein) but poorly to BBM (1% specific binding to 100 p g of membrane protein) In

contrast, IODO-GEN-NPY, and IODO-GEN-NPY, both bound well to LBM (20-25%

specific binding to 100 pg of membrane protein), but also BBM (8-10% of the initial

amount of NPY bound specifically to 100 pg of membrane protein) The lactoperoxidase-

labeled NPY obtained from the first peak of radioactivity observed on HPLC (lacto-

NPY was assessed in the same manner The specific binding of NPY , to LBM and BBM

(75 pg of membrane protein) was respectively 14.8% 2 1.3% and 1.3% ? 0.1% of the

initial amount of radioactive NPY I added Since IODO-GEN-NPY, and IODO-GEN-

NPY, are both radioiodinated at position 36, it is possible that this is the common feature

that allows demonstration of ligand binding to BBM

Assessment of Label Degradation

As mentioned above, NPY radioiodinated either at the fourth lysine residue using the

Bolton-Hunter agent (B-H-NPY,) or at the first tyrosine residue (NPY,) using either

IODO-GEN or lactoperoxidase binds specifically to LBM but not to BBM On the other

hand, NPY radioiodinated at the carboxyl terminal tyrosine residue in position 36

(NPY,,) while still exhibiting preferential binding to LBM also exhibited specific binding

to BBM This observation raises the possibility that there are receptors on the BBM which

are only readily demonstrable with NPY labelled at the carboxyl terminus and not with

amino-terminal labelled NPY (NPY,) When the putative NPY receptors were identified

by cross-linking to radiolabelled NPY no receptor species unique to NPY,, was

identified l 6 It is possible that the binding reflects contamination of BBM with LBM

However, the degree of binding observed with the carboxyl terminal labelled tracers

makes this unlikely Since BBM contain proteases, preferential degradation of NPY , and

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52 zyxwvutsrqponmlkjihgfedcbaZYXWVUTSRQPONMLKJIHGFEDCBAANNALS NEW YORK ACADEMY OF SCIENCES zyxwvutsrqponmlkjihgfedcbaZYXWVUTSRQPONMLKJIHGFEDCBA

FIGURE 1 Time and temperature depen- dence of Bolton-Hunter-NPY degradation by BBM B-H-NPY was incubated with BBM (20

pg of membrane protein) for the times noted on the abscissa After the incubation was com- pleted, the suspension was centrifuged at 27,500 x g for 30 min The degree of degrada- tion of the unbound radiolabeled NPY con- tained in the supernatant was assessed by 10%

TCA precipitation (30 min at 4°C)

0 , I ( I , I

Time (min)

BH-NPY zyxwvutsrqponmlkjihgfedcbaZYXWVUTSRQPONMLKJIHGFEDCBArelative to NPY,, could account for the apparent differential binding of the

different radioligands to BBM

To address this question, NPY label degradation was assessed by monitoring either the

fraction of radiolabelled NPY that did not precipitate with 10% TCA or the fraction which

could not be rebound to LBM In the latter experiments, Bolton-Hunter labelled NPY was

incubated for 1 hr at 22"C, either in the absence of membranes or in the presence of 70

pg of either LBM or BBM At the end of the incubation period, the radiolabelled NPY

that was not bound to the membranes was recovered after centrifugation (27,500 x g for

30 min) and allowed to rebind to LBM, in the presence or absence of 1 p M unlabelled

NPY The specific binding of BH-NPY to LBM was determined as the difference in the

amount of radiolabelled NPY bound in the absence or presence of excess unlabelled NPY

Compared to the control preincubation without membrane, preincubation with LBM did

not alter specific binding to LBM in the second incubation (1 1.5% after preincubation

with LBM or without membranes) In contrast, after 1 hr preincubation of BH-NPY with

BBM, the subsequent specific rebinding to LBM was only 27% of control (specific

binding of 3%) In a similar fashion, after an incubation with BBM, the unbound BH-

NPY showed a 60% decrease in TCA precipitability (from 87% to 36%) Degradation of

BH-NPY by BBM was time and temperature dependent (FIG 1)

We next determined whether there was differential degradation of NPY, and NPY,,

by BBM by examining degradation of different forms of IODO-GEN radiolabelled NPY

(FIG 2A) After 30 min incubations of label peaks at 22°C with 40 p g BBM, q e

percentages of unbound radiolabelled NPY that could be TCA-precipitated was 51% for

ison, the corresponding percentages for LBM were 8 9 8 , 9 6 8 and 94% respectively The

greater degradation of NPY, by BBM was little altered by the addition of an excess

amount (1 pM) of unlabelled NPY Similar results were obtained when the different

forms of lactoperoxidase-labelled NPY (FIG 2B) were studied Thus, after incubation

with 50 p g membranes, the fractions of lactoperoxidase-radiolabelled NPY that could be

TCA-precipitated was 87% (peak 1) and 95% (peak 2) after a preincubation with LBM,

and 40% and 82% after a preincubation with BBM This finding correlates well with the

50% loss in the expected rebinding ability of NPY , to LBM after preincubation with

BBM

In the next series of experiments, we attempted to minimize enzymatic degradation of

NPY Even with shorter incubations at 4°C in the presence of a combination of protease

inhibitors (1 mM of phenylmethylsulfonylfluoride and 0.0125 mglml each of pepstatin,

chymostatin, antipain, leupeptin, trypsin inhibitor), degradation of NPY , was not fully

peak 1 (NPY,), 92% for peak 2 (NPY,,), and 90% for zyxwvutsrqponmlkjihgfedcbaZYXWVUTSRQPONMLKJIHGFEDCBApeak 3 (NPY, a 36) By COmpX-

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TAYLOR zyxwvutsrqponmlkjihgfedcbaZYXWVUTSRQPONMLKJIHGFEDCBAet zyxwvutsrqponmlkjihgfedcbaZYXWVUTSRQPONMLKJIHGFEDCBAd.: NPY RECEPTOR zyxwvutsrqponmlkjihgfedcbaZYXWVUTSRQPONMLKJIHGFEDCBA53 zyxwvutsrqponmlkjihgfedcbaZYXWVUTSRQPONMLKJIHGFEDCBA

NPY I to BBM could be demonstrated, suggesting that degradation accounts at least in

degradation (shorter incubations at 4°C) resulted in decreased specific binding of all

labels, including NPY,,, we cannot assess with certainty whether the lack of NPY,

binding to BBM was due entirely to degradation In any case, regardless of the radiolabel

used, NPY bound less well to BBM than to LBM, suggesting that degradation will not

entirely account for the preferential binding of NPY to LBM Since only the radioactivity

of the radiolabeled NPY is monitored, we cannot determine if regions of the molecule

other than those containing the labelled tyrosine residue undergo degradation However,

these results provide evidence that there is preferential degradation of the amino terminus

Cross-Linking the NPY Receptor in Intestine and Brain

Intestine

Lacto-NPY I was cross-linked to its LBM receptor using DSS and the resulting NPY-

NPY-receptor complexes, which were cross-linked in the absence of the reducing agent

DTT (FIG 3; lane 3) migrated as a major radioactive band with an Mr of 52,000-59,000

and as a minor band with an Mr of 42,000-44,OOO (the ranges reflect the apparent

molecular weights estimated using the top and bottom of each band, and are derived from

eight separate experiments) Radioactivity at the top of the lane represents aggregated

material larger than 220 kDa (the size of the largest molecular weight marker, femtin); the

FIGURE 2 Differential degradation of radio- labeled NPY by intestinal LBM and BBM:

NPY was radiolabeled with either IODO-GEN

or lactoperoxidase and the different peaks ob- tained from HPLC purification incubated with

LBM or BBM at 22°C When the incubation was completed, the suspension was centrifuged

at 27,500 x g for 30 min The degree of deg- radation of the unbound radiolabeled NPY con- tained in the supernatant was assessed by 10%

TCA precipitation (30 min at 4°C) (A) IODO-

GEN radiolabelled NPY incubation for 30 min with 40 pg of membrane protein; (B) lactoper- oxidase radiolabeled NPY, incubation for 60

min with 50 pg of membrane protein

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activity at the front of the gel is thought to reflect radiolabelled NPY that was bound, but

not cross-linked to the membranes, which then became dissociated during SDS treatment

to SDS-PAGE (lane 1) minimally affected the migration of the 52-59-kDA band but

FIGURE 3 Size difference between intestinal and brain NPY-receptor complexes Intestinal lat-

erobasal membranes (37.5 kg of membrane protein) or crude brain membranes (370 pg membrane

protein) were incubated with trace amounts of lactoperoxidase radioiodinated NF'Y in the presence or

absence of unlabeled 10 pM NPY The NPY-receptor complexes were next cross-linked using 0.2

mM (intestinal) or 1 mM (brain) of DSS and analyzed subsequently by SDS 10% polyacrylamide gel

electrophoresis in the presence or absence of the reducing agent D" The resulting radioautograph

is shown On the zyxwvutsrqponmlkjihgfedcbaZYXWVUTSRQPONMLKJIHGFEDCBA1eB of the radioautograph, the positions of the molecular weight standards and the

bands corresponding to the intestinal (b) or brain (+) NPY receptors are shown

shifted the position of the 42-44 kDa species to Mr 37-39 kDa This later change may

reflect intramolecular disulfide bonding within the 42-44 kDa species or disulfide bond-

ing between a 37-39 kDa binding subunit and a small 5 kDa subunit Additional faint

bands at Mr -75,000-90,000 and -1lO,OOO-l20,OOO were also revealed; these addi-

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TAYLOR zyxwvutsrqponmlkjihgfedcbaZYXWVUTSRQPONMLKJIHGFEDCBAef zyxwvutsrqponmlkjihgfedcbaZYXWVUTSRQPONMLKJIHGFEDCBAal.: NPY RECEPTOR zyxwvutsrqponmlkjihgfedcbaZYXWVUTSRQPONMLKJIHGFEDCBA55 zyxwvutsrqponmlkjihgfedcbaZYXWVUTSRQPONMLKJIHGFEDCBA

tional bands reflect specific binding of NPY in that they were inhibited in the presence of

1 FM unlabelled NPY

Brain

When radioactive NPY was cross-linked to the brain receptor with DSS, two radio-

active bands were seen (FIG 3: lane 6) which migrated at approximately 62 kDa (range

60-64) and 39 kDa (range 36-39) In contrast to the intestinal receptor the addition of 10

mM D l T did not appreciably alter the migration pattern of either band (lane 5 )

DISCUSSION

NPY is localized to the intrinsic nerves of the small intestine, and may be released

and specific receptors located on the serosal side of the intestinal epithelial cell is a

necessary prerequisite for this biologic action Using a membrane preparation technique

that allows fractionation of LBM free of ER-Golgi, we have demonstrated that NPY,

radiolabelled with the Bolton-Hunter agent or at tyrosine 1 (with IODO-GEN and lac-

toperoxidase) binds exclusively to intestinal LBM l 6 This finding is consistent with the

observation that NPY will only inhibit secretion when applied to the serosal surface of

mucosal strips mounted in Ussing chambers In competitive inhibition studies, unlabelled

of the intestinal receptor was not as high as the values previously described for the brain

and kidney NPY receptors, 14*'7-19 or for a PYY-preferring receptor described on crude

intestinal membranes." This 4- to 5-fold lower affinity may be partially due to the small

degree of ligand degradation by laterobasal membranes Alternatively, the low affinity

could reflect greater receptor degradation during the 2-day-long intestinal membrane

fractionation, which might occur despite the addition of protease inhibitors at the begin-

ning of the procedure However, it should be noted that this lower K, is still within the

range of the EC,, (10-30 nM) estimated for the biologic effects of NPY on the

intestine.'-' '

We have identified two tentative candidates for the LBM NPY receptor after cross-

linking the receptor followed by analysis on SDS-PAGE under reducing conditions: a

major 52-59 kDA band and a minor 37-39 kDa band In the absence of DTT, the 37-39

kDa band migrates as a 42-44 kDa species This finding suggests the presence of di-

sulfide bonding within the receptor itself or between a 37-39 kDa binding subunit and a

separate -5-kDa subunit IODO-GEN-NPY,, IODO-GEN-NPY,, and lacto-NPY, cross-

linking to LBM with DSS revealed additional faint bands at 75-90 kDa and 110-120

kDa l 6 These faint bands were also seen with DSP cross-linking of lacto-NPY,, and as

such they do not appear to be specific for IODO-GEN-NPY, or lacto-NPY, Since these

bands were faint and inconsistent, we have had difficulty in further analyzing their

relationships to the 52-59 kDa- and 37-39/4244 kDa species Since both the 52-59 and

37-39 kDa species have the same affinity for NPY, we speculate that the smaller product

is derived as a result of degradation from the larger species

While Inui et al." reported the molecular weight for the NPYlPYY receptor in the

brain to be of 50 kDa, we demonstrated two candidate species for the brain NPY receptor,

with Mr's of 62,000 and 39,000.23 The slight difference in size between the intestinal

52-59 kDa species and the brain 62 kDa species was confirmed when the cross-linked

NPY-receptor complexes from these two different tissues were analyzed together on the

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56 zyxwvutsrqponmlkjihgfedcbaZYXWVUTSRQPONMLKJIHGFEDCBAANNALS NEW YORK ACADEMY OF SCIENCES zyxwvutsrqponmlkjihgfedcbaZYXWVUTSRQPONMLKJIHGFEDCBA

same gel (FIG 3) Another difference between intestine and brain is that the smaller

species in the intestine [37-39/42-44 kDa] is sensitive to reducing agents while the brain

39 kDa species is not Alternate methodologies (e.g., immunologic mapping, receptor

purification and amino acid analysis or receptor cloning) will be required to determine

whether these slight differences reflect distinct structures, or artifactual modifications of

the receptor secondary to enzymatic degradation of the larger species (75-90 kDa or

115-120 kDa)

IODO-GEN-NPY, and IODO-GEN-NPY, bound equally well to the brain NPY

BBM derived from enterocytes The binding of IODO-GEN-NPY, and IODO-GEN-

NPY, coupled with the lack of binding of IODO-GEN-NPY , to brush border membranes

is intriguing IODO-GEN-NPY , is iodinated at tyrosine residue 1, IODO-GEN-NPY, is

iodinated at tyrosine residue 36, and IODO-GEN-NPY, is iodinated at both tyrosine

residues 1 and 36 The differential binding of the different labels to LBM and BBM could

reflect two classes of NPY receptors: a class localized to LBM which can bind B-H-NPY

and NPY radioiodinated at the tyrosine residue 1, and an additional class localized to

BBM (and possibly LBM) which only recognizes NPY radioiodinated at position 36

However, in our cross-linking experiments, we have been unable to provide structural

evidence for distinct NPY receptors which can only bind NPY radiolabelled at position

36 It is conceivable that binding of NPY to BBM reflects contamination with LBM

However, the magnitude of binding of NPY,, labels to BBM makes this unlikely as BBM

would have to be heavily contaminated Our studies in differential degradation of different

label species by LBM and BBM suggest the presence in BBM of an enzyme(s) that

cleaves the amino terminus of NPY thereby removing the label in the Tyr, position and

the Bolton-Hunter label

In summary, we have localized receptors for NPY to the serosal laterobasal membrane

of the intestinal epithelial cell By covalently cross-linking NPY to its receptor, we have

demonstrated two main molecular species of the receptor with molecular sizes of 48-55

kDa (52-59 kDa minus molecular weight of NPY) and 33-37 kDa While NPY iodinated

at Tyrosine, is extensively degraded by BBM we have observed that NPY iodinated at

Tyrosine,, will bind to BBM

SUMMARY

Neuropeptide Y (NPY) is widely distributed in the central and peripheral nervous

systems where it serves neuromodulator and neurotransmitter functions NPY is contained

within intrinsic nerves of the small intestine and can be demonstrated to inhibit intestinal

secretion when added to the serosal side of intestine mucosa mounted in Ussing chambers

When injected centrally it has potent effects on food intake, blood pressure, sexual

activity and circadian rhythms Using NPY radiolabeled with iodogen, lactoperoxidase,

or the Bolton-Hunter reagent, we have localized high-affinity NPY receptors on brain

membranes and on the serosal laterobasal membranes of the rat intestinal epithelial cell

We have demonstrated that enzymatic degradation may limit the ability to demonstrate

NPY binding to brush border membranes In other experiments NPY was cross-linked to

its receptors in brain and intestine using disuccinimido suberate and the resulting com-

plexes analyzed on SDS polyacrylamide gel electrophoresis followed by radioautography

We identified two main NPY receptor species in the intestine with molecular sizes of

52-59 kDa and 37-39 kDa The 37-39 kDa species may possess a disulfide bond which

gives the receptor a fixed conformation, or it may be composed of two subunits (37-39

kDa and -5 kDa subunits) This conclusion is based on the different migration of the

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TAYLOR zyxwvutsrqponmlkjihgfedcbaZYXWVUTSRQPONMLKJIHGFEDCBAet zyxwvutsrqponmlkjihgfedcbaZYXWVUTSRQPONMLKJIHGFEDCBAul.: NPY RECEPTOR zyxwvutsrqponmlkjihgfedcbaZYXWVUTSRQPONMLKJIHGFEDCBA57 zyxwvutsrqponmlkjihgfedcbaZYXWVUTSRQPONMLKJIHGFEDCBA

smaller band in the presence of the reducing agent, dithiothreitol The intestinal NPY

receptor exhibits differences from the rat brain receptor previously characterized by us

using similar techniques The brain receptor has a molecular weight of approximately 58

exposure to dithiothreitol The localization of NPY receptors on laterobasal membranes

and brain membranes is consistent with previous anatomic and physiologic findings The

different characteristics of each receptor type provides physical evidence of receptor

heterogeneity However, it is possible that the greater enzymatic degradation observed in

intestinal membranes might explain the differences in receptor sizes in the two organs

ACKNOWLEDGMENT

The authors are indebted to Dr Steven R Vigna for his help with the radioiodination

of NPY

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