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Tiêu đề Olfactory receptor signaling is regulated by the post-synaptic density 95, Drosophila discs large, zona-occludens 1 (PDZ) scaffold multi-PDZ domain protein 1
Tác giả Ruth Dooley, Sabrina Baumgart, Sebastian Rasche, Hanns Hatt, Eva M. Neuhaus
Trường học NeuroScience Research Center, Charité Universitätsmedizin Berlin
Chuyên ngành Neuroscience
Thể loại Journal article
Năm xuất bản 2009
Thành phố Berlin
Định dạng
Số trang 12
Dung lượng 563,63 KB

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Neuhaus3 1 Molecular Medicine Lab RCSI, Education & Research Centre Smurfit Building, Beaumont Hospital, Dublin, Republic of Ireland 2 Department of Cell Physiology, Ruhr University Boch

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post-synaptic density 95, Drosophila discs large,

zona-occludens 1 (PDZ) scaffold multi-PDZ domain

protein 1

Ruth Dooley1,2,*, Sabrina Baumgart2,*, Sebastian Rasche1, Hanns Hatt1and Eva M Neuhaus3

1 Molecular Medicine Lab RCSI, Education & Research Centre Smurfit Building, Beaumont Hospital, Dublin, Republic of Ireland

2 Department of Cell Physiology, Ruhr University Bochum, Germany

3 NeuroScience Research Center, Charite´, Universita¨tsmedizin Berlin, Germany

Keywords

MUPP1; olfactory neuron; olfactory

receptor; PDZ protein; signal transduction

Correspondence

E M Neuhaus, NeuroScience Research

Center, Charite´, Universita¨tsmedizin Berlin,

10117 Berlin, Germany

Fax: +49 30 450 539 970

Tel: +49 30 450 539 702

E-mail: eva.neuhaus@charite.de

*These authors contributed equally to this

work

(Received 9 September 2009, revised 6

October 2009, accepted 12 October 2009)

doi:10.1111/j.1742-4658.2009.07435.x

The unique ability of mammals to detect and discriminate between thou-sands of different odorant molecules is governed by the diverse array of olfactory receptors expressed by olfactory sensory neurons in the nasal epithelium Olfactory receptors consist of seven transmembrane domain G protein-coupled receptors and comprise the largest gene superfamily in the mammalian genome We found that approximately 30% of olfactory receptors possess a classical post-synaptic density 95, Drosophila discs large, zona-occludens 1 (PDZ) domain binding motif in their C-termini PDZ domains have been established as sites for protein–protein inter-action and play a central role in organizing diverse cell signaling assem-blies In the present study, we show that multi-PDZ domain protein 1 (MUPP1) is expressed in the apical compartment of olfactory sensory neurons Furthermore, on heterologous co-expression with olfactory sen-sory neurons, MUPP1 was shown to translocate to the plasma mem-brane We found direct interaction of PDZ domains 1 + 2 of MUPP1 with the C-terminus of olfactory receptors in vitro Moreover, the odor-ant-elicited calcium response of OR2AG1 showed a prolonged decay in MUPP1 small interfering RNA-treated cells We have therefore elucidated the first building blocks of the putative ‘olfactosome’, brought together

by the scaffolding protein MUPP1, a possible central nucleator of the olfactory response

Structured digital abstract

l MINT-7290305 : OR2AG1 (uniprotkb: Q9H205 ) physically interacts ( MI:0915 ) with MUPP1 (uniprotkb: O75970 ) by anti tag coimmunoprecipitation ( MI:0007 )

l MINT-7289999 , MINT-7290250 , MINT-7290063 , MINT-7290110 : OR2AG1 (uni-protkb: Q9H205 ) binds ( MI:0407 ) to MUPP1 (uniprotkb: O75970 ) by peptide array ( MI:0081 )

l MINT-7290162 : mOR283-1 (uniprotkb: Q9D3U9 ) binds ( MI:0407 ) to MUPP1 (uni-protkb: O75970 ) by peptide array ( MI:0081 )

l MINT-7290128 : mOR-EG (uniprotkb: Q920P2 ) binds ( MI:0407 ) to MUPP1 (uni-protkb: O75970 ) by peptide array ( MI:0081 )

Abbreviations

CamKII, calcium ⁄ calmodulin-dependent protein kinase II; GABA B , c-aminobutyric acid receptor B; GFP, green fluorescent protein; GST, glutathione S-transferase; HRP, horseradish peroxidase; INAD, inactivation no after potential D; MUPP1, multi-PDZ domain protein 1; OMP, olfactory marker protein; OR, olfactory receptor; OSN, olfactory sensory neuron; PDZ, post-synaptic density 95, Drosophila discs large, zona-occludens 1; RNAi, RNA interference; siRNA, small interfering RNA.

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Detection of an odorant is initiated by activation of

a fraction of many hundreds of G protein-coupled

odorant receptors (ORs) expressed in olfactory

sen-sory neurons (OSNs) of the mammalian olfactory

epithelium [1] Signal transduction begins when an

odorant molecule binds to an OR, resulting in the

activation of adenylyl cyclase type III [2] via the

olfactory G protein Gaolf [3] cAMP then binds to a

cyclic nucleotide-gated channel [4–7], allowing it to

conduct cations such as Na+⁄ Ca2+ The calcium

ions then bind to a calcium-gated chloride channel

[8], further depolarizing the cell How these diverse

signaling molecules find each other in the complex

and densely-packed environment of the cell, avoiding

cross-talk with other signaling pathways, in order to

ensure the rapidity and specificity of signaling,

remains an unanswered question The idea of the

existence of an ‘olfactosome’, or highly ordered

multi-component protein network involving the

olfac-tory signal transducing molecules, has been

previ-ously discussed [9–11]; however, until now, no

concrete evidence has been provided Scaffolding

net-works have been investigated in detail in the visual

system of Drosophila melanogaster, where inactivation

no after potential D (INAD), made up of five

post-synaptic density 95, Drosophila discs large,

zona-occludens 1 (PDZ) domains, has the ability to bind

to various molecules in the signal transduction

cas-cade, thereby bringing them into close proximity and

ensuring a rapid and specific signal transduction

[9,12]

PDZ domains are modular protein–protein

interac-tion domains, which are amongst the most abundant

protein interaction domains in organisms from bacteria

to mammals, and have been implicated in various

pro-cesses, including clustering, targeting and routing of

their binding partners [13–15] PDZ target specificity is

usually dependent on the extreme carboxyl-terminal

amino acid sequence of the interacting protein;

how-ever, for some ligands, residues as far back as the)10

position may influence binding energy [16]

Peptide-binding preferences of PDZ domains led to their

division into three discrete functional classes [16], which may not be as strict as initially anticipated because predictions of PDZ domain–peptide interac-tions were recently shown to be evenly distributed throughout selectivity space [17]

The multi-PDZ domain protein 1 (MUPP1) is com-posed of thirteen PDZ domains, each diverse with respect to its amino acid sequence It was first identi-fied through a yeast two-hybrid screening as an interaction partner of the C-terminus of 5-hydroxy-tryptamine receptor type 2C [18] Subsequently, many diverse interaction partners of MUPP1 have been characterized, including G-protein coupled c-aminobu-tyric acid receptor B (GABAB) [19] and the calcium⁄ calmodulin-dependent protein kinase II (Cam-KII) [20] In the present study, we introduce ORs as novel interaction partners of MUPP1

Results MUPP1 is expressed at the sites of olfactory signal transduction

ORs are expressed on the ciliary membranes of OSNs, the first point of contact of the sensory cell with incoming odorant molecules To investigate whether a receptor centered multi-component protein network might exist, we tested for the expression of PDZ scaffolding proteins in the olfactory epithelium using RT-PCR (Fig 1A) We detected robust expression of MUPP1 and weak expression of ZO-1, but could not detect Patj, Erbin or DLG-2 Because MUPP1 mRNA was highly abundant, we examined the expression of the protein by western blotting Upon fractionation of the olfactory epithelium [21], we found MUPP1 to be present to a greater extent in the cilia-enriched fraction compared to the remaining cell fractions (Fig 1B) Using olfactory marker protein (OMP)-green fluo-rescent protein (GFP) transgenic mice, expressing GFP

in every mature olfactory sensory neuron [22], we investigated the cellular localization of MUPP1 in the olfactory epithelium and found MUPP1 to be

l MINT-7290219 : hOR3A1 (uniprotkb: P47881 ) binds ( MI:0407 ) to MUPP1 (uni-protkb: O75970 ) by peptide array ( MI:0081 )

l MINT-7290191 : hOR1D2 (uniprotkb: P34982 ) binds ( MI:0407 ) to MUPP1 (uni-protkb: O75970 ) by peptide array ( MI:0081 )

l MINT-7289922 : AC3 (uniprotkb: Q8VHH7 ) and MUPP1 (uniprotkb: O75970 ) colocalize ( MI:0403 ) by fluorescence microscopy ( MI:0416 )

l MINT-7289933 , MINT-7289954 , MINT-7289978 : OR2AG1 (uniprotkb: Q9H205 ) binds ( MI:0407 ) to MUPP1 (uniprotkb: O75970 ) by pull down ( MI:0096 )

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expressed in the apical part of OSNs, mainly in the

cilia layer (Fig 1C) Double immunolabeling showed

co-localization with adenylyl cyclase 3, a central

mole-cule in the olfactory signal transduction cascade in the

cilia of OSNs (Fig 1C, D)

Interaction of PDZ domains 1 + 2 of MUPP1 with

OR2AG1 in vitro

PDZ domain interactions have been well characterized

and modes of binding have been grouped into three

main classes of PDZ binding motifs, occurring at the

C-terminus of the interacting proteins [16] We scanned

the human olfactory receptor repertoire for putative

binding motifs and discovered them in the extreme

C-termini of approximately 30% of human ORs, with

examples from each of the three classes being outlined

to date (7% Class I, 12% Class II and 10% Class III;

Fig 2A) Intriguingly, this suggested that a subset of

ORs could have the ability to interact with PDZ

domains of MUPP1

We performed co-immunoprecipitation experiments

to verify the ability of ORs containing a PDZ interac-tion motif to bind to MUPP1 Hana3A cells were transfected with HA-OR2AG1 These cells express members of the RTP and REEP family, which com-prise molecular chaperones known to promote the expression of ORs [23] Antibodies to the HA tag were used to co-immunoprecipitate MUPP1, as shown by a band of 220 kDa in western blots (Fig 2B, precipitation: a-HA), whereas no MUPP1 immuno-reactivity could be observed in precipitates of nontransfected cells (Fig 2B, control) These results indicated an interaction between OR2AG1 and MUPP1 in the recombinant expression system

MUPP1 is made up entirely of thirteen different PDZ domains, each being diverse in sequence We set out to determine which of these PDZ domains were involved in the molecular interaction with ORs We created a glutathione S-transferase (GST) fusion pep-tide of the C-terminus of OR2AG1 and in vitro trans-lated the PDZ domains of MUPP1, in pairs (1 + 2,

A

C

D

B

Fig 1 MUPP1 expression in olfactory

sen-sory neurons (A) Expression of mRNA of

different PDZ scaffolding proteins in the

olfactory epithelium by RT-PCR *Weak

band for ZO-1 (B) Fractional preparation of

whole olfactory epithelium shows MUPP1,

at 220 kDa, enriched in the cilia fraction (1)

compared to the remaining cell fractions

(2–4); a Coomassie-stained gel is shown as

a loading control (C) MUPP1 is co-localized

with adenylyl cyclase 3 in the apical layer of

the olfactory epithelium

Immunohistochemi-cal staining of 14 lm cryosections of

OMP-GFP mouse olfactory epithelium using

specific antibodies against MUPP1 (green)

and adenylyl cyclase 3 (red) Overlay shows

mature OSNs in blue White arrow denotes

the apical layer Scale bars = 50 lm (D).

Higher magnification image of MUPP1 ⁄

ade-nylyl cyclase 3 stained olfactory epithelium.

The arrow shows MUPP1 expression in cilia

and in dendritic knobs Scale bar = 5 lm.

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3 + 4, etc.) (Fig 2C) Interaction assays were then

carried out by incubating different pairs of PDZ

domains as in vitro translation products with OR2AG1

C-terminus GST fusion peptides A specific binding of

PDZ domains 1 + 2 was determined via western

blot-ting, whereas, for example, in vitro translated PDZ

domains 3 + 4 did not have the ability to bind to the

C-terminus of OR2AG1 (Fig 2D) None of the PDZ

domains could bind to GST alone We then tested

binding of single PDZ domains 1 + 2, and found that

both could bind to the OR C-terminus (Fig 2D)

Next, we investigated the ability of PDZ domains

1 + 2 to bind to receptor C-termini of 15 amino

acids in length, which were spotted on microarrays

The arrays were probed four times with PDZ

domains 1 + 2 fused to the HA tag for subsequent

analysis of binding by antibody incubation and chemiluminescence detection (Fig 2E) Interactions were analyzed in every experiment with positive (HA tag spotted directly) and negative (FLAG tag spotted directly and A1⁄ A2) control spots Interactions that yielded robust interactions of PDZ domains 1 + 2 with the olfactory receptors hOR2AG1 (S-T-L), mOR283-1 (A-T-V) and hOR3A1 (S-L-A), which all contain PDZ domain binding motifs in their C-ter-mini, were scored as array positives (Fig 2E) hOR1D2 and mOR-EG, which are olfactory receptors that do not contain classical PDZ interaction motifs

in their C-termini, also showed positive interactions but, in the case of hOR1D2, only in two out of four experiments Other olfactory receptors, such as mOR167-4, mOR199-1, M71, M72 and mOR241-1

A

C

B

Fig 2 The C-terminus of OR2AG1 interacts with MUPP1 in vitro (A) Pie chart illustrating the abundance of classical PDZ motifs in human

OR C-termini (B) MUPP1 was immunoprecipitated in HA-OR2AG1 expressing Hana3A cells using a-HA antibodies, detection was performed with a-MUPP1 (*MUPP1) and a control was performed with identical amounts of nontransfected cell lysates from Hana3A cells The blot shown is representative of three independent immunoprecipitation experiments (C) Western blot using HA-specific antibodies showing the

in vitro translation products of PDZ domain pairwise constructs Three nonspecific bands appear at 170, 70 and 30 kDa Specific bands at the correct molecular weights are outlined (white asterisk) (D) PDZ domains 1 + 2 both interact with OR2AG1_GST in vitro Interaction assay using in vitro translated PDZ domains 1 + 2, PDZ domains 3 + 4, PDZ domain 1 and PDZ domain 2 with GST alone or C-terminus OR2AG1_GST The blots shown are representative of four independent experiments for each interaction assay described (E) Peptide micro-array with C-termini of different receptors incubated with PDZ domains 1 + 2 fused to HA; chemiluminescence detection on film after incu-bation with a-HA antibodies and HRP-coupled secondary antibodies The array shown is representative of four independent experiments; peptide sequences for spots A1–A12 (row 1), A13–A24 (row 2) and B1 (FLAG tag) and B2 (HA tag, positive control) are listed in Table S1 A1 and A2 serve as negative controls.

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and mGluR2, as well as the olfactory cyclic

nucleo-tide-gated ion channel subunit A2, did not show any

interaction with the PDZ domains investigated

We furthermore investigated the binding

determi-nants in the C-terminus of hOR2AG1 by spotting

pep-tides that correspond to mutated or shortened receptor

C-termini Truncation of the last amino acids

abol-ished binding of the C-terminus of hOR2AG1 to PDZ

domains 1 + 2 hOR2AG1 constructs where the last

four amino acids H-S-T-L were mutated to H-A-T-A

[OR2AG1_deltaPDZ(A)] still bound to PDZ domains

1 + 2, whereas mutation to H-W-T-W

[OR2AG1_del-taPDZ(W)] completely abolished binding (Fig 2E)

MUPP1 shows plasma membrane localization

upon co-expression of ORs

MUPP1 is a cytosolic protein, and MUPP1-GFP,

simi-lar to endogenous MUPP1, shows a homogenous,

predominantly cytosolic distribution when expressed

in Hana3A cells (Fig 3A) Interestingly, when

co-expressed with hOR2AG1, MUPP1 exhibited a

lar-gely plasma membrane expression in a subset of cells,

forming clusters at the cell surface (Fig 2A, B) Approximately 5% of transfected cells exhibited this translocation effect of MUPP1-GFP This apparently low proportion of cells reflects the notoriously low expression rate of olfactory receptors in heterologous systems and the relatively high amount of cells express-ing MUPP1-GFP However, the results obtained in the present study correlate with various studies showing a similar proportion of transiently transfected cells responding to odorant in ratiometric calcium imaging experiments [24–26] This alteration in the subcellular distribution of MUPP1 upon co-expression with ORs supported the finding of a physical association between MUPP1 and ORs in the heterologous expression system

We hypothesized that, by deleting the components

of the PDZ binding motif, we could disrupt MUPP1 translocation Truncation of the receptor from the final eight amino acids (amino acids 309–316) did result in

a clear abrogation of the association, as outlined by the predominantly cytosolic localization of MUPP1-GFP (Fig 3A) We then investigated the in vitro bind-ing properties of the truncated C-terminal mutant of OR2AG1 by creating a GST fusion construct The

A

Fig 3 MUPP1 plasma membrane translocation on co-expression of odorant receptors (A) MUPP1-GFP expressed alone in Hana3A cells exhibits a diffuse cytosolic expression Co-transfection of OR2AG1 with MUPP1-GFP leads to a predominant plasma membrane expression

of GFP with clustering apparent Truncation of OR2AG1 from the final eight amino acids leads to a cytosolic expression of MUPP1-GFP; at least five independent experiments were performed for each condition (B) Higher magnification of the plasma membrane of the cells shown in (A) (C) In vitro interaction properties of truncated hOR2AG1 C-terminus Western blot showing HA-PDZ1 + 2 probed with 2AG1-GST and trunc8-GST, at 55 kDa, using a-HA antibodies The experiment was repeated three times with similar results being obtained (D) Co-expression of hOR1D2 and hOR3A1 also resulted in translocation of MUPP1-GFP to the plasma membrane; at least five independent experiments were performed for each receptor Scale bars = 20 lm.

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C-terminal mutant peptide was incubated with PDZ

domains 1 + 2 of MUPP1 and failed to interact with

truncated mutant (Fig 3C)

Consistent with this observation is the fact that other olfactory receptors showing interactions with PDZ domains 1 + 2 (hOR1D2, hOR3A1) also caused

A

C

B

Fig 4 Functional role of MUPP1 in OR signaling (A) Western blot showing MUPP1 expression in Hana3A cells (control) compared to 48 and 72 h after siRNA (exon5) transfection (B) Representative ratiometric calcium imaging responses of transiently transfected Hana3A cells [siRNA(1)]; the arrow represents the beginning of application of amylbutyrate, lasting for 10 s (C) Western blot showing MUPP1 expression

in Hana3A cells (control) compared to scrambled siRNA, siRNA against exon 5 of MUPP1 and siRNA against exon 45 of MUPP1, 72 h after transfection (D) Bar chart showing the rise time (10–90%) of Hana3A cells responding to amylbutyrate, transfected with OR2AG1 (ctrl) (n = 15) or siRNA(exon5)-treated Hana3A cells transfected with OR2AG1 (RNAi) (n = 15) (E) Time of decay from 90% of peak amplitude to 10% of average baseline (n = 15) for each condition and the percentage of cell responses decaying to basal levels within the time-frames outlined Cell responses not decaying within the time-frame of experiment were included in the > 20 s section; n = 15 for control, n = 27 for RNAi(exon5) (F) Bar chart showing the rise time (10–90%) for siRNA(exon45) transfected Hana3A cells; n = 12 for control, n = 12 for RNAi(exon45) (G) Bar chart showing the time of decay (90–10%) and percentages of cell responses for siRNA(exon45) transfected Hana3A cells; n = 12 for control, n = 12 for RNAi(exon45) (H) Bar chart showing the rise time (10–90%) for Hana3A cells transfected with scrambled siRNA (I) Bar chart showing the time of decay (90–10%) and percentages of cell responses for scrambled siRNA transfected Hana3A cells Error bars show the SEM **P < 0.01, ***P < 0.001.

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MUPP1-GFP translocation to the plasma membrane

in the Hana3A cells (Fig 3D)

MUPP1 controls the duration of Ca2+signaling

mediated by recombinant ORs

To determine whether MUPP1 has the ability to

regulate OR function, we investigated the role of this

scaffolding protein in hOR2AG1-mediated Ca2+

mobilization by performing ratiometric Ca2+ imaging

in Hana3A cells These cells express MUPP1

endoge-nously and, by reducing the amount of MUPP1 by

RNA interference, we aimed to investigate the

func-tionality of the interaction between MUPP1 and

hOR2AG1 Transfection of small interfering RNA

(siRNA) against Mupp1 led to an almost complete

knockdown of the MUPP1 protein, as shown by wes-tern blotting (Fig 4A) Next, we monitored the response of transiently transfected OR2AG1 to its spe-cific odorant ligand, amylbutyrate [24] via ratiometric calcium imaging in siRNA-treated cells (Fig 4B) When MUPP1 was largely absent, the OR-elicited response exhibited a similar rise time to that of the control cells, 5.54 ± 0.87 s for RNA interference (RNAi) compared to 4.27 ± 0.65 s for the control (Fig 4B, C) However, the response failed to decay within the normal average time-frame in siRNA-trea-ted cells (19.3 ± 2.9 s) compared to the control cells (7.2 ± 2.1 s) (Fig 4B, D) Using another siRNA directed against an alternative exon of Mupp1, similar results were obtained The rise time of the OR-elicited response was similar to that of the control cells

Fig 5 Interaction of MUPP1 with OR2AG1 is important for controlled signal decay (A) Immunocytochemistry (a-HA antibody) showing sta-ble expression of MUPP1-PDZ1 + 2-HA in Hana3A cells Scale bar = 20 lm (B) Representative ratiometric calcium imaging traces for Hana3A cells (control) and MUPP1-PDZ1 + 2-HA cells (1 + 2) transiently transfected with OR2AG1 Arrows denote amylbutyrate application (C) Bar chart showing the rise time (10–90%) for Hana3A cells stably expressing MUPP1-PDZ1 + 2-HA, transiently transfected with OR2AG1; n = 13 for control, n = 24 for PDZ domains 1 + 2 (D) Decay of response (90–10%) (n = 13 for control, n = 24 for PDZ domains

1 + 2) and the percentage of responses to amylbutyrate decaying to basal levels within the given time-frames (E) Transient expression of a truncated version of OR2AG1 missing the last eight amino acids (trunc8) Bar chart showing the rise time (10–90%) for Hana3A cells expressing the truncated receptor (n = 12 for control, n = 17 for OR2AG1-trunc8) (F) Decay of response (90–10%) (n = 12 for control,

n = 17 for OR2AG1-trunc8) and the percentage of responses to amylbutyrate decaying to basal levels within the given time-frames Error bars show the SEM **P < 0.01, ***P < 0.001.

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(Fig 4C), although the decay was prolonged

signifi-cantly (Fig 4D) Cells transfected with a scrambled

version of the siRNA did not show any significant

differences in the kinetics of the OR-elicited

Ca2+ response compared to nontransfected cells

(Fig 4E, F)

Interaction with MUPP1 is important for

controlling OR-mediated Ca2+signaling

Because PDZ domains 1 + 2 interact with MUPP1

(Fig 2), we generated a cell line over-expressing these

two PDZ domains (Fig 5A) Interestingly, the

pro-longed signal decay observed in the siRNA

experi-ments was mirrored in the OR-dependent responses of

Hana3A cells stably over-expressing PDZ domains

1 + 2 of MUPP1 (Fig 5B) When monitoring the

response of transiently transfected OR2AG1 to

amy-lbutyrate, we found that the OR-elicited response did

not decay within the normal average time-frame in

cells over-expressing PDZ domains 1 + 2 (26.2 ±

1.8 s) compared to control cells (10.2 ± 1.9 s)

(Fig 5D) As in siRNA-treated cells, the rise time after

odorant stimulation was almost indistinguishable in

cells over-expressing PDZ domains 1 + 2 (4.87 ±

0.2 s) compared to control cells (4.71 ± 0.69 s)

(Fig 5C) In summary, when the interaction between

MUPP1 and OR2AG1 is inhibited by over-expressing

the interacting PDZ domains, the resulting response of

OR2AG1 to odorant is modified in that the rapid

decay of signal is impaired

We finally examined the effect of deletion of the

components of the PDZ binding motif on the

signal-ing properties of the receptor in Ca2+ imaging

experiments Truncation of the receptor from the

final eight amino acids (amino acids 309–316)

resulted in a prolonged signal decay, similar to that

observed in the siRNA experiments and in the cells

over-expressing PDZ domains 1 + 2, whereas the

rise time of the signals was again not affected

(Fig 5E, F)

Discussion

Until now, the involvement of PDZ domain

scaffold-ing proteins in olfactory signal transduction has gone

unstudied It has previously been suggested that such

scaffolding networks or ‘olfactosomes’ may exist [9,10]

but, to date, no evidence for this phenomenon has

been outlined In the present study, we have uncovered

a PDZ protein as a novel interaction partner of

olfac-tory receptors and have elucidated the molecular

details of this interaction

The primary source of olfactory signaling and the sites of expression of ORs are the ciliary structures of the OSNs Interestingly, we found MUPP1 to be pre-dominantly expressed in the apical compartment of OSNs and enriched in the cilia fraction of a prepara-tion of whole murine olfactory epithelium We hypoth-esize that MUPP1, through its multivalent capabilities, could play a key role as a central nucleator of olfac-tory signal transduction With its thirteen PDZ domains, each diverse in its amino acid sequence, MUPP1 holds great potential for organizing signal transduction molecules into defined protein networks and thereby regulating signaling events

MUPP1 has previously been found to interact with

a diverse array of molecules, including G protein-cou-pled receptors such as the 5-hydroxytryptamine recep-tor type 2C [18,27] and the GABAB receptor [19] We postulated that MUPP1 could directly interact with the olfactory receptor itself We scanned the entire human olfactory receptor repertoire and discovered that up to 30% of receptors contain putative PDZ binding motifs in their C-termini, following the previ-ously outlined rules of binding [16] PDZ domains

1 + 2 of MUPP1 indeed showed direct interaction with OR C-terminal petides Moreover, upon co-expression of ORs containing classical PDZ bind-ing motifs in their C-termini, MUPP1-GFP exhibited

a translocation from the cytosol to the plasma mem-brane in the heterologous expression system, suggest-ing a physical association between both proteins within the cell We found this translocation to be dependent on the final amino acids of the receptor protein Similar to the other PDZ domain interactions that have been shown to be abolished by mutating amino acids at position 0 and )2 from the termi-nus [16], we found that binding of the hOR2AG1 C-terminus to PDZ domains 1 + 2 did not occur when positions 0 and )2 were mutated to tryptophans, which are not present in the PDZ binding motifs of other membrane proteins [17] We also found interac-tion of PDZ domains 1 + 2 with ORs showing no classical PDZ binding motifs, indicating that the understanding of the exact molecular rules of OR PDZ interaction will require further analysis Previous work with other proteins has already indicated that it

is highly likely that a large number of PDZ domain interactions will not fit into the confined class defini-tions and that PDZ domains may have been opti-mized across the proteome in order to minimize cross-reactivity [17]

We observed that a reduction of MUPP1 resulted in

a significant increase in the duration of Ca2+responses evoked by the activation of recombinantly expressed

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hOR2AG1 Similarly, over-expression of the

OR-inter-acting PDZ domains 1 + 2 of MUPP1 also resulted in

odorant-evoked Ca2+ responses that persisted longer

than those in control cells When over-expressed, PDZ

domains 1 + 2 may bind to the C-terminus of

hOR2AG1, thus having a blocking effect on the

bind-ing of the less abundant endogenous MUPP1 A

trun-cated receptor no longer containing a PDZ motif in

the C-terminus showed the same effect of prolonged

signal duration Thus, all of the experiments revealed

that the association of hOR2AG1 with MUPP1

regu-lates signal duration To a certain extent, the impaired

signal desensitization resembles the effect of the

absence of the multi-PDZ domain protein INAD in

the Drosophila visual signal transduction cascade Flies

lacking INAD exhibit a profound reduction of the

light response [28] Interestingly, INAD is also

required for normal deactivation of visual signaling by

positioning eye protein kinase C in close proximity to

TRP to facilitate its phosphorylation, ultimately

result-ing in deactivation of the channel [12,29,30] On the

other hand, in contrast to the findings of the present

study, MUPP1 was shown to prolong the duration of

GABABreceptor signaling and increase the stability of

the receptor [19] However, we must note that the

situ-ation in the recombinant expression system is different

from that in the olfactory neurons, where alternative

binding partners of MUPP1 presumably exist It is

therefore possible that MUPP1 could exhibit

alterna-tive effects on the dynamics of calcium responses

induced by ORs in the neurons compared to those

induced by heterologously expressed ORs The

observed effects can therefore only be taken as proof

of the functional significance of the observed

interac-tion Further studies are necessary to shed light on the

function of this interaction in the in vivo situation

By influencing the duration of the Ca2+ signal of

ORs in the cilia of the sensory neurons, MUPP1 could

have a strong influence on the olfactory signaling

path-way An interesting interaction partner of MUPP1

out-lined to date is CamKII, which is known to play an

important role in olfactory adaptation [20] By

phos-phorylation of adenylyl cyclase 3 in OSNs, CamKII

provides an important mechanism for the attenuation

of odorant-stimulated cAMP increases [31]

Alterna-tively, because different pathways, such as those

involving phosphoinositide 3-kinase [32], are ultimately

engaged after OR stimulation, MUPP1 may control

OR activity by acting as a scaffold to link different

signaling pathways

In conclusion, we have outlined a novel aspect of the

olfactory signal transduction cascade by uncovering a

previously unknown interaction partner of olfactory

receptors and a putative regulator of signaling processes in OSNs It is tempting to speculate that a so-called ‘olfactosome’ exists in the cilia of olfactory sensory neurons, organizing the vast array of signaling molecules and ensuring the specificity of signaling How exactly MUPP1 could carry out such an impor-tant task remains to be elucidated, although the answer may lie in the remaining and as yet unidentified interac-tion partners of MUPP1 in the olfactory sensory cell

Experimental procedures DNA constructs and primers

pCDNA3_MUPP1-GFP and in vitro translation tandem PDZ domain constructs in vector pBAT were provided

by H Lu¨bbert (Ruhr-University, Bochum, Germany) pCDNA3_OR2AG1 was cloned as described previously [33] C-terminal mutant constructs of OR2AG1 [^PDZ_ pCDNA3 (S314A, L316A), trunc4_pCDNA3 (amino acids 313–316) and trunc8_pCDNA3 (amino acids 309–316)], were obtained by PCR using varying 3¢ primers and pCDNA3_OR2AG1 as a template GST fusion constructs

of the C-terminus of OR2AG1, and mutant thereof (trunc8) were created by cloning the region between amino acids

293 and 316 from the receptor into pGEX-3X vector (Amersham Pharmacia Biotech, Piscataway, NJ, USA), using varying reverse primers PDZ domains 1 + 2 were cloned using pBAT_1 + 2_HA as a template The stable cell line construct, pCMV⁄ Bsd_PDZ1 + 2_HA, was cloned using pCDNA3_MUPP1-GFP as a template All constructs were verified by sequencing For RT-PCR, mRNA was extracted from adult mouse olfactory epithelium, and the primers were used were: 5¢-CAAAACGCTCTACAGGC TCC-3¢, 5¢-GAAGAGCTGGACAGAGGTGG-3¢ (ZO-1), 5¢-TTATGGGCCACCGGATATTA-3¢, 5¢-GGAGAGTCA CTGAAGGCTGG-3¢ (DLG-2), 5¢-AAGCTAAGAGGCA CGGAACA-3¢, 5¢-TCCTTATTGCCAGCGAGACT-3¢ (Patj), 5¢-TTGCAGACGGAAGAGGTTCT-3¢, 5¢-GGCCACTT TCAGCATCAAAT-3¢ (Erbin), 5¢-GCGGATCCGCAT GTTGGAAACCATAGAC-3¢ and 5¢-GCGAATTCGA CATTTTTAGTGAGTTCCAC-3¢ (MUPP1)

Antibodies

Primary antibodies used were: anti-adenylyl cyclase 3, rab-bit polyclonal (Santa Cruz Biotechnology, Santa Cruz, CA, USA), directly labeled using DyLight549 Microscale Antibody Labeling Kit (Pierce, Rockford, IL, USA); anti-MUPP1, rabbit polyclonal (provided by H Lu¨bbert, Ruhr-University); anti-GFP, rabbit polyclonal (#ab290-50; Abcam, Cambridge, MA, USA); a-HA antibody, mouse monoclonal (#H9658; Sigma, St Louis, MO, USA) Second-ary antibodies used were goat anti-rabbit Alexa546nm

Trang 10

(Molecular Probes, Carlsbad, CA, USA) and horseradish

peroxidase (HRP) coupled goat mouse and goat

anti-rabbit IgGs (Bio-Rad, Hercules, CA, USA)

Cell culture and transfection

All tissue culture media and related reagents were purchased

from Invitrogen (Carlsbad, CA, USA) Hana3A cells [23]

(provided by H Matsunami, Duke University Medical

Cen-ter, Durham, NC, USA), were maintained in DMEM plus

10% fetal bovine serum and 1% penicillin⁄ streptomycin, at

37C and 5% CO2, and transfections were carried out using

a standard calcium phosphate precipitation technique

MUPP1-GFP and OR plasmid DNAs were transfected in a

ratio of 1 : 10, with approximately 2 lg of total DNA per

dish All images were acquired using a Zeiss LSM 510 Meta

confocal microscope (Carl Zeiss, Oberkochen, Germany)

Hana3A cells were stably transfected with pCMV⁄ Bsd

plas-mid (Invitrogen) containing tandem PDZ domains 1 + 2

along with an HA tag Positive clones were selected for

using blasticidin (10 lgÆmL)1) and stable transfection was

confirmed by immunocytochemistry

Cell membrane preparation and western blotting

The olfactory epithelium of CD1 mice was fractionated by

mechanical agitation as described previously [21] Equal

amounts of protein from each fraction were loaded on an

SDS gel and subjected to immunoblotting on

poly(vinyli-dene difluoride) membrane (Millipore, Billerica, MA, USA)

and Coomassie staining Detection was performed using the

ECL western blotting detection system (GE Healthcare,

Milwaukee, WI, USA) For co-immunoprecipitation,

Hana3A cells were transfected with OR2AG1-HA and

MUPP1_pCDNA3 or untransfected The nucleus-free cell

lysates were incubated with biotinylated a-HA antibody

and precipitated protein collected using Dynabeads

(Invi-trogen) and DynaMag (Invi(Invi-trogen) Any interaction was

detected using MUPP1 antibodies

Immunohistochemistry

Mice were raised and maintained according to

governmen-tal and institutional care instructions

Immunohistochemis-try was carried out on 14 lm horizontal sections, and

fluorescence images were obtained with a confocal

micro-scope (Zeiss LSM 510 Meta) with ·40 objective Control

experiments in the absence of any primary antibody

revealed a very low level of background staining For

odor-ant exposure experiments, OMP-GFP mice were exposed to

a mixture of 100 different odorant molecules (Henkel

KGaA, Du¨sseldorf, Germany) for specified amounts of

time Control mice were housed in a separate room free

from artificial odorant stimulation All mice were held in

standard cages at room temperature Each cage was sur-rounded by a Perspex chamber with ventilation suction to maintain a constant air-flow

GST fusion peptides and in vitro interaction assays

The C-terminal region of OR2AG1 was found to lie between amino acids 293 and 316, as predicted by tmhmm, a trans-membrane helices prediction program based on a hidden Markov model [34] OR2AG1 C-terminus GST fusion teins and mutant construct thereof (trunc8-GST) were pro-duced in Escherichia coli XL1 blue and purified on glutathione sepharose beads (Becton-Dickinson Biosciences, Franklin Lakes, NJ, USA) PDZ domains were in vitro trans-lated using the TNTT3 Coupled Reticulocyte Lysate Sys-tem (Promega, Madison, WI, USA) Interaction assays were carried out by incubating 10 lL of in vitro translation prod-uct with 50 lL of GST fusion peptide bead slurry for 2 h at

4C with gentle shaking After a series of washing steps using Buffer S (20 mm Hepes, 100 mm KCl, 0.5 mm EDTA, 1 mm dithiothreitol, pH 7.9), specific interactions were assessed via immunoblotting GST alone was used as a negative control

Peptide microarray

CelluSpots Peptide Arrays (Intavis AG, Cologne, Germany) were blocked for 2 h at room temperature with 5% skimmed milk in NaCl⁄ Tris ⁄ Tween The arrays were incubated with a PDZ1 + 2_HA fusion protein (produced

as described in E coli) overnight at 4C CelluSpots were incubated with the a-HA antibody for 4 h at room temper-ature Detection was performed with HRP coupled second-ary antibody and using ECL western blotting detection reagent (GE Healthcare)

Mupp1 siRNA

Pre-synthesized and tested Mupp1 siRNA (identification 1

#107246 and 2 #216971) and a custom designed scrambled version of Mupp1 (CUGACUGUGUAUCGAACGGtt) were purchased from Ambion (Austin, TX, USA) siRNA was transfected 72 h prior to calcium imaging using Lipo-fectamine 2000 (Invitrogen), in serum-free medium (Opti-Mem; Invitrogen) Forty-eight hours prior to calcium imaging, 2 lg of OR2AG1 plasmid DNA were transfected per dish using ExGen 500 transfection reagent (Fermentas, Glen Burnie, MD, USA) Medium was exchanged for fresh DMEM 24 h post-transfection

Ratiometric Ca2+imaging in heterologous cells

Stably⁄ transiently transfected Hana3A cells were incubated with 7.5 lm FURA-2 AM (Invitrogen) Ratiometric

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