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heat shock cognate 70 kDa; hsc70 members, which actively participate in a number of vital cellular functions such as protein folding, translocation, degradation and the acquisition of ce

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hsc70 chaperone function

Athanasia Salma, Apostolos Tsiapos and Ioannis Lazaridis

Laboratory of General Biology, Medical School, University of Ioannina, Greece

The heat shock protein 70 (hsp70) family of

molecu-lar chaperones consists of stress inducible (e.g hsp70)

and constitutively expressed (e.g heat shock cognate

70 kDa; hsc70) members, which actively participate in

a number of vital cellular functions such as protein

folding, translocation, degradation and the acquisition

of cell thermotolerance [1–4] In order to perform

their functions, the hsp70s cooperate with a wide

range of divergent proteins collectively known as

co-chaperones Among them, the DnaJ family

mem-bers seem to be the major and critical partners in

regulating at least the folding activity of the hsp70

chaperone machine [5]

DnaJ proteins exert their function by binding to

hsc70 and stimulating its ATPase activity ATP

hydro-lysis converts hsc70 from an open to a closed state

with low exchange rates, therefore promoting a cycle

of substrate binding and release [6] In mammals, more

than 20 DnaJ homologues have been reported and

classified into three groups on the basis of their

domain characteristics [7] All members of the DnaJ

family contain the J domain, which is a 70-amino acid sequence structured in four helices with a loop between helices II and III containing the highly conserved tri-peptide HPD, which is necessary for binding to hsc70 [8] The type I DnaJs, in addition to the J domain, contain a Gly⁄ Phe-rich region followed by a stretch of cysteine repeats Type II DnaJs lack the cysteine repeats and type III DnaJs lack both the G⁄ F region and the cysteine repeats Type I and Type II proteins seem to have similar functions and they bind non-native substrates, in contrast to type III proteins which may not bind denatured polypeptides and thus proba-bly function as ‘specialized’ molecular chaperones [9] dj2 is the best characterized type I mammalian DnaJ and it has been defined as the mammalian homologue of the bacterial DnaJ and the yeast Ydj1 [10–12] It is mainly cytosolic and acts as a cochaperone to hsc70 assisting the folding of denatured proteins and facilitat-ing the protein import into the mitochondria [13–15] As

a critical member of the hsc70 chaperone machine, dj2 was found, when overexpressed, to suppress aggregate

Keywords

DnaJ; hsc70; molecular chaperone; protein

folding; T antigen

Correspondence

I Lazaridis, Department of Biology,

Faculty of Medicine, University of Ioannina,

453 32 Ioannina, Greece

Fax: +302 6510 97863

Tel: +302 6510 97752

E-mail: ilazarid@cc.uoi.gr

(Received 2 April 2007, revised 9 July 2007,

accepted 30 July 2007)

doi:10.1111/j.1742-4658.2007.06019.x

Simian virus 40 large T antigen is a J-domain-containing protein with mul-tiple functions Among its numerous activities, T antigen can bind heat shock cognate 70 (hsc70) but the biological significance of this interaction has not been fully understood Here, we show that T antigen can act as an hsc70 co-chaperone enhancing the protein-folding ability of the hsc70 chap-erone machine We also show that T antigen exerts its function in colla-boration with the mammalian homologue of DnaJ Moreover, we show that the participation of T antigen in the hsc70 chaperone machine has cell-type-specific characteristics

Abbreviations

dj2, mammalian homologue of DnaJ; GST, glutathione S-transferase; hsc70, heat shock cognate 70 kDa; hsp, heat shock protein;

mutTAg, mutant TAg; SV40, simian virus 40; TAg, SV40 large T antigen; wtTAg, wild-type TAg.

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formation of androgen receptor and huntingtin caused

by expanded polyglutamine tracts [16,17]

Simian virus 40 (SV40) large T antigen (TAg) is a

multifunctional oncoprotein which is able to induce

transformation in multiple cell types [18] It has been

shown that T antigen can act as a molecular chaperone

because it contains a functional J domain [19] It has

also been shown that the J domain is essential for

T antigen to exert its functions related to

transforma-tion, enhancement of cell division, release of Rb⁄ E2F

complexes and viral DNA replication [20–23] T antigen

was found to bind hsc70 in an ATP-dependent manner

that requires the ATPase activity to be provided by

hsc70 [24] Although the biological significance of the

above binding is not yet clear, the prevailing view states

that upregulation of the hsc70 chaperone machine is

required for several viral functions [25]

In this report, we show that T antigen binds to

hsc70 both directly and indirectly via dj2 We also

show that the above binding is ATP independent and

contributes significantly to the folding activity of the

hsc70 chaperone machine Finally, we show that the

formation of the heterotrimeric complex T antigen–

dj2–hsc70 is cell-type-specific, because it is observed in

cells nonpermissive for SV40 viral lytic infection and

not in cells permissive to lytic infection

Results

In order to investigate the interactions of T antigen

with the hsc70 chaperone machine, we purified hsc70,

dj2 and T antigen wild-type and mutant proteins as

described in Experimental procedures Our efforts to

express the full-length forms of wild-type and mutant

T antigen fused to glutathione S-transferase were not

successful, despite the fact that we tested extensively

both the bacterial and the insect cell expression

systems We believe that the difficulty in purifying full-length GST-tagged T antigen forms was due to the large size of the resulting proteins Therefore, we decided to purify truncated forms of T antigen which included the J domain, the Rb-binding domain and the DNA-binding domain, but lacked the ATPase domain

of the C-terminus Given that the ATPase domain of the T antigen has been shown to be dispensable for hsc70 binding [24], we reasoned that the truncated T-antigen proteins would mimic the function of their full-length counterparts

T antigen binds directly to hsc70 Upon performing GST pull-down experiments, we observed that the wild-type TAg (wtTAg) bound to hsc70 in an ATP-dependent manner with a stoichiome-try of 1 : 1, as reported previously [24] We also con-firmed the inability of the mutTAg protein to bind hsc70, even in the presence of ATP (data not shown)

It is interesting to note that hsp70 exhibited the same characteristics as hsc70, in that it was found to bind wtTAg in an ATP-dependent fashion, but with signifi-cantly reduced affinity (data not shown)

T antigen and dj2 cooperate in binding to hsc70 Having established the assay conditions, we tested whether the presence of a typical hsc70 co-chaperone, namely dj2, interfered or altered the TAg⁄ hsc70-bind-ing characteristics The first findhsc70-bind-ing was that dj2 bound TAg in an ATP-independent manner (Fig 1A, lanes 3 and 4) Although functional dimerization of DnaJs has been reported [31–33], our results clearly indicate that binding between type I and type III DnaJs is possible

in an ATP-independent manner Moreover, it was shown that unlike hsc70, dj2 bound mutTAg indicating

Fig 1 dj2 participation in the TAg ⁄ hsc70 complex Pull-down assays were performed using GST-tagged wtTAg and mutTAg as described in Experimental procedures Lanes 1, 2 and 8 represents purified pro-teins (A) GST–wtTAg was incubated with the indicated proteins in the presence or absence of ATP Bound proteins were detected by SDS ⁄ PAGE, stained with Coo-massie Brilliant Blue (upper), followed by western blotting (IB) (B) The same experi-ment as in (A) was performed using GST– mutTAg instead of GST–wtTAg.

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once again that dj2 and T antigen, although both

J-domain-containing proteins have clearly distinct

hsc70-binding properties (Fig 1B, lanes 3 and 4) The

above data also show that dj2 and hsc70 have different

binding properties to wtTAg and mutTAg Most

importantly, we observed that the presence of dj2

dis-rupted the stoichiometric balance of hsc70⁄ wtTAg

complex reducing the amount of bound hsc70 and

allowing hsc70 to bind wtTAg even in the absence of

ATP (Fig 1A, lanes 5 and 6) Similar results were

obtained when we used mutTAg instead of wtTAg in

our pull-down assays More specifically, we observed

that in the presence of dj2, hsc70 bound mutTAg in an

ATP-independent fashion (Fig 1B, lanes 5 and 6)

These findings led us to hypothesize that dj2 binds

T antigen in an ATP independent manner and the

resulting heterodimer complexes with hsc70 via dj2

To verify this hypothesis we proceeded in a

pull-down experimental scheme in which wtTAg was

sequentially incubated with hsc70 and dj2 As shown

in Fig 2, formation of the dj2⁄ TAg complex prior to

hsc70 addition resulted in the recruitment of increased

amounts of hsc70 to the glutathione Sepharose-bound

GST–wtTAg (compare lanes 1 and 2) Densitometry

analysis revealed that there is a 2–2.5-fold increase in

the amount of hsc70 collected in the Tag⁄ dj2 complex

In contrast, addition of dj2 to the already formed

hsc70⁄ TAg complex decreased the amount of bound

hsc70 by 50% (compare lanes 1 and 3) Once again the

absence of ATP in the binding reactions did not

influ-ence hsc70 recruitment to the dj2⁄ TAg complex,

confirming our conclusion that the participation of the

T antigen in this complex is mainly mediated by dj2 The reduced amounts of hsc70 bound to TAg prior to dj2 addition (lanes 1 and 5) are probably due to the fact that the binding affinity of dj2 to hsc70 is stron-ger The possibility of an antagonistic effect between dj2 and TAg for hsc70 binding cannot be excluded, but the finding that formation of the dj2⁄ TAg complex recruits more hsc70 (compare lanes 1, 3 and 5 with lanes 2, 4 and 6) indicates that the order of inter-actions is important for the final composition of the complex

T antigen enhances the folding activity of the hsc70 chaperone machine

Because one of the main functions of the dj2⁄ hsc70 chaperone complex is the folding of denatured or par-tially folded proteins [29] we investigated the involve-ment of T antigen in the above process Therefore,

we performed luciferase-refolding experiments and observed that indeed T antigen facilitated hsc70 and dj2 in recovering of activity for denatured luciferase (Fig 3) We also found that T antigen can act as an hsc70 co-chaperone, albeit with much reduced activity when compared with dj2 However, we observed that the presence of wtTAg significantly enhanced the fold-ing activity of the dj2⁄ hsc70 chaperone machine This was verified by the finding that the maximal refolding

of luciferase achieved by the hsc70⁄ dj2 dimer, was fur-ther increased with the addition of wtTAg Impor-tantly, the mutTAg had no effect on the function of hsc70 alone or hsc70 with dj2 suggesting that the effect

of wtTAg is dependent on its co-chaperone activity

Fig 2 dj2 recruits increased amounts of hsc70 to the

heterotrimer-ic complex Pull-down experiments were performed using GST–

wtTAg and in the assay mixture hsc70, dj2 and ATP were added

sequentially as indicated The composition of the complexes

formed was analysed by SDS ⁄ PAGE followed by Coomassie

Bril-liant Blue staining.

Fig 3 wtTAg enhances the folding activity of the hsc70 ⁄ dj2 chap-erone pair Refolding assays were performed as described and luciferase activity was monitored at several time points ranging from 0 to 60 min This diagram depicts values taken after 60 min incubation with the indicated proteins and expressed as percentage

of the native luciferase activity.

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The ATP independence of the heterotrimeric

TAg–dj2–hsc70 complex formation is cell type

specific

The in vitro binding data raised the question of how

T antigen, dj2 and hsc70 may interact in the cellular

context In order to investigate these interactions we

chose two transformed cell lines, namely Cos7 and

SVTT1, which constitutively express T antigen but

dif-fer in that the Cos7 cells are permissive for SV40 lytic

infection, whereas the SVTT1 are not Cell extracts

were immunoprecipitated with an anti-TAg coupled to

protein G beads (as described in Experimental

proce-dures) and the immunoprecipitates were analysed for

the presence of TAg, dj2 and hsc70 In accordance with

previous findings [30], we detected the formation of

the hsc70⁄ TAg complex only in nonpermissive cells

(Fig 4B, +ATP) The amount of hsc70 bound to TAg

was quantitated as 50% of the input We also detected

the presence of dj2 in the immunoprecipitates of both

cell types in the presence of ATP and our quantification

measurements showed that 15–20% of the input was

retained in the complex However, to our surprise, we

found that in the absence of an ATP regeneration

sys-tem, both dj2 and hsc70 were not able to associate with

T antigen in the extracts of non permissive cells

(Fig 4B, –ATP) In contrast under the same conditions

the association of T antigen with dj2 persisted in

per-missive cells (Fig 4A, ±ATP) in accordance with our

in vitro findings that this binding is ATP independent

Collectively, the above results led us to conclude that

the interactions between T antigen, dj2 and hsc70 are

cell-type dependent

Discussion

Although the ability of T antigen to bind hsc70 was

extensively studied, the exact mechanism by which this

binding contributes to the T-antigen-mediated cellular transformation remains elusive [34,35] However, a model has been suggested according to which the J-domain-dependent association of T antigen with hsc70 stimulates chaperone activity, which in turn releases E2F from its pRb complex allowing the ‘free’ E2F to transactivate the genes required for cell prolif-eration [20,22,36] Our results, without disputing the above model, indicate that T antigen might not exert its hsc70-related functions alone but in combination with dj2, a classical hsc70 co-chaperone This sugges-tion is based on our findings that, in vitro, T antigen associates with dj2 in an ATP-independent manner and this binding persists even in the presence of hsc70 (Fig 1A) As a result, T antigen is recruited to the hsc70 chaperone complex via dj2 Therefore, the pres-ence of T antigen allows hsc70 to utilize yet another J-domain-containing protein and enhance its chaperon-ing function It is interestchaperon-ing to note that even a mutated form of T antigen unable to bind hsc70 can

be recruited to the complex via dj2 (Fig 1B)

Our interpretation of the above data is that besides the formation of the expected dj2⁄ hsc70 (dimer : monomer) complexes, the presence of T anti-gen leads to the formation of novel heterotrimeric complex comprising of monomeric forms of TAg⁄ dj2⁄ hsc70 The formation of these complexes does not exclude the possibility of direct binding between

T antigen and hsc70 On the contrary, given the abun-dance of hsc70, one can envisage the presence of all three types of complex in the cellular context This interpretation is supported by the finding that associa-tion of T antigen with dj2 prior to the addiassocia-tion of hsc70 leads to the recruitment of increased amounts of hsc70 to the complex In contrast, addition of dj2 to the already formed TAg⁄ hsc70 dimer does not increase the levels of hsc70 present in the complex, indicating that probably dj2 associates with hsc70 in a separate

A

Fig 4 Cell-type-specific interaction of T antigen with hsc70 Immunoprecipitations of Cos7 cell extracts (A), SVTT1 extracts (B), and NIH 3T3 transfected with mutTAg extracts, as a control (C), were performed using an anti-(T antigen) serum column Bound proteins were detected

by western blotting The presence or absence of ATP regeneration system in the lysates is indicated FL, analysis of the flow through mate-rial; ctrl, the control IgG-protein G beads; Inp, the whole cellular lysate (10% of total).

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complex which does not include T antigen

Interest-ingly, the increased amounts of hsc70 required by the

TAg⁄ dj2 heterodimer do not seem to be affected by

the presence of ATP, indicating once more that the

ATP-independent dj2 binding to hsc70 is the driving

force for the creation of the heterotrimeric complex

(Fig 2) Therefore, based on our results, we believe

that T antigen can bind hsc70 in two distinctly

differ-ent ways First, it can bind directly in an

ATP-depen-dent fashion, and second, it can bind indirectly via dj2

in an ATP-independent manner

The functional significance of our findings was

investigated by monitoring the chaperone-folding

activity of the detected complexes Indeed, we found

that the presence of T antigen enhanced the ability of

the hsc70⁄ dj2 chaperone pair to refold denatured

lucif-erase We believe that this increased folding activity

was due to the function of the newly formed

heterotrimeric complex (TAg⁄ dj2 ⁄ hsc70) In contrast,

the presence of the mutated form of T antigen was

not able to change the folding activity of the hsc70⁄ dj2

chaperones In other words, despite the fact that the

trimeric complex mutTAg⁄ dj2 ⁄ hsc70 can be clearly

formed (Fig 1B), mutTAg is unable to further

enhance luciferase folding, probably due to its inability

to stimulate the hsc70 ATPase activity This last

assumption is supported by the finding that although

wtTAg can act as a weak hsc70 cochaperone, mutTAg

seem to be unable to positively contribute to the

enhancement of the hsc70 folding activity Collectively,

we concluded that T antigen facilitates the hsc70

chaperone machine by enhancing its folding function

In order to detect the existence of the described

complexes in vivo, we performed immunoprecipitations

with an anti-(T antigen) serum in cellular extracts of

Cos7 and SVTT1 cells As shown in Fig 4, our

approach was quite effective in that our antibody

col-umn depleted most of the T antigen from the cell

lysates As expected, based on our previous data [30],

formation of the TAg⁄ hsc70 complex was observed

only in nonpermissive cells, reinforcing our suggestion

that this binding has cell-type-specific characteristics

Moreover, we detected the presence of dj2 in both the

TAg⁄ hsc70 complex (nonpermissive cells) and in the

T antigen immunoprecipitate (permissive cells)

How-ever, to our surprise, we observed that in the absence

of ATP the dj2 and hsc70 did not associate with TAg

in SVTT1 cells, in contrast to the Cos7

immuno-precipitates where the binding of T antigen to dj2

persisted (Fig 4) Given that the dj2⁄ TAg binding is

ATP independent, as shown above, we suspect that

the activation of an additional, yet unidentified,

cellular factor is responsible for the cell type specific

dissociation of the heterotrimeric complex in the absence of ATP or conversely enabling dj2 to bind TAg in Cos7 cells Overall, our data using cellular extracts clearly suggest the existence of a cell type specific organization of the hsc70 chaperone machine, which is probably related to the T antigen J-domain-mediated viral functions

Experimental procedures

Cell lines

The Cos7 and SVTT1 (NIH 3T3 cells expressing wtTAg) cell lines established from monkey or mouse embryos, respectively, were maintained in minimal essential medium supplemented with 10% fetal bovine serum at 37C in a humidified 5% CO2 atmosphere Sf9 insect cells were grown in Sf900II medium (Gibco, Invitrogen, Carlsbad, CA) containing 10% fetal bovine serum at 27C and used for the production of baculoviruses

Cloning, expression and purification of recombinant proteins

The pQE-32-Mydj2 construct [13] was used to overexpress Mydj2–6·His in Escherichia coli SG13009 Briefly, over-night cultures of E coli carrying the pQE-32-Mydj2 plasmid were diluted 10-fold and cultured for 1 h After isopropyl thio-b-d-galactoside induction (1 mm) for 2 h at

37C, cells were collected by brief centrifugation at 6000 g using an Avanti J-25 centrifuge with JA-14 rotor (Beckman Coulter, Fullerton, CA) and cell lysates were prepared by sonication The recombinant protein was purified using a

Ni⁄ nitrilotriacetic acid column and imidazole elution (50 ± 250 mm) as described by the manufacturers (Qiagen, Valencia, CA)

The SV40 large T antigen was subcloned from pSG5-T (a generous gift from J A DeCaprio, Harvard Medical School, MA) into the BamH1 site of pGEX-4T-1 (AMRAD)

to create the pGEX-4T-1–wtTAg construct The resulting plasmid was digested with EcoR1 and HindII, treated with Klenow and religated to create the pGEX-4T-1–wtTAg282 construct which was used to express the first 282 amino acid residues of the wild-type T antigen The mutated form

of T antigen was subcloned from pSG5-T-H42Q (a gener-ous gift from J A DeCaprio) to pGEM and subsequently inserted to the EcoR1 and Sal1 sites of pGEX-4T-1 The resulting plasmid was digested with Not1 and HindIII, blunt ended with Klenow and religated to create the pGEX-4T-1–mutTAg268, which was used to express the first 268 amino acid residues of T antigen with a single amino acid substitution (H42Q) The described constructs, named GST–wtTAg and GST–mutTAg, respectively, were expressed in BL21(DE3) bacterial cells and the corresponding

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proteins were purified from lysates according to standard

procedures [26]

Baculovirus expressed His6·-tagged hsc70 and hsp70

were prepared according to Bac-To-Bac baculovirus

expres-sion system procedure (Invitrogen)

Pull-down assays

GST fusion proteins (3 lg; wtTAg, mutTAg) or GST alone,

were incubated for 30 min at room temperature with 30 lL

of glutathione–agarose beads and ‘blocked’ in 1% fish

gela-tin in assay buffer (150 mm NaCl, 20 mm Tris⁄ HCl pH 7.5,

2 mm MgCl2, 250 mm sucrose, 1% Triton X-100, 0.1 mm

EGTA, 1 mm phenylmethanesulfonyl fluoride, 1 mm DTT)

After washing three times with the same buffer, the beads

were combined with equal amounts of purified His–hsc70

and⁄ or His–dj2 and further incubated for 1 h at room

tem-perature in the presence or absence of ATP regeneration

buffer (1 mm ATP, 30 mm creatine phosphate, 0.25 mg

phosphokinase per mL, 2 mm MgCl2, 1 mm dithiothreitol)

The beads were washed six times with assay buffer, before

eluting the bound proteins with hot Laemmli buffer [27]

Western blots were performed using the following

anti-bodies: T antigen-specific mAb PAb419, which have been

produced by hybridoma cells Hsc70-specific antibody

(SPA-815, StressGen), Hsp70-specific antibody (SPA-810,

StressGen) and Dj2-specific antibody (HDJ-2⁄ DNAJ Ab-1,

NeoMarkers) Quantitation of the pulled down proteins

was performed using the quantity one densitometry

software provided by Bio-Rad Inc (Hercules, CA)

Immunoprecipitation

Whole-cell extracts were prepared from COS and SVTT1

cells in lysis buffer containing 150 mm NaCl, 20 mm

Tris⁄ HCl pH 7.5, 2 mm MgCl2, 250 mm sucrose, 1%NP40,

0.1 mm EGTA, 1 mm phenylmethanesulfonyl fluoride,

1 mm dithiothreitol and 1 lgÆmL)1each of protease

inhibi-tors aprotinin, leupeptin and pepstatin The extracts were

centrifuged at 13 000 g for 15 min using a Sigma 1-14

microcentrifuge with 12094 rotor (Sigma-Aldrich, Munich,

Germany), precleared with 20 lL of IgG–protein G (3 lg)

for 30 min at room temperature and then incubated with

20 lL of anti-TAg–protein G beads (40 lg of anti-TAg

serum) or with 20 lL IgG–protein G beads (40 lg of

anti-[mouse IgG] serum) overnight at 4C, in the presence or

absence of ATP regeneration buffer The antibodies were

covalently coupled to the beads using DMP (Pierce,

Rock-ford, IL) as a cross-linker After incubation, the beads were

washed three times with lysis buffer Proteins present in the

immune complexes were eluted with lysis buffer

supple-mented with 1 m NaCl The eluates were trichloroacetic

acid precipitated and the pellets were resuspended in 30 lL

Laemmli buffer for subsequent analysis by SDS⁄ PAGE and

western blotting

Luciferase assays

Luciferase activity was measured as described [28] with minor modifications Briefly, 1 mg luciferase (Promega, Madison, WI) was chemically denatured by diluting 3-fold in buffer containing guanidinium-HCl (6 m) 25 mm Hepes (pH 7.6), 50 mm KC1, 5 mm MgCl2 and 1 mm dithiothreitol for 40 min at room temperature Refolding reactions were performed in 125 lL volumes by diluting denatured luciferase (1 lL) into refolding buffer contain-ing 25 mm Hepes (pH 7.6), 50 mm KC1, 5 mm MgCl2, purified chaperones, and ATP regeneration buffer The samples were incubated at 30C and at the indicated times, 1 lL of each reaction was diluted into 60 lL of luciferase assay mixture (Promega) Activity was measured using a luminometer (Junior LB9509 EG & G Berthold, Bad Wildbad, Germany) Native luciferase activity was measured after first diluting the stock solution threefold into refolding buffer and then diluting 125-fold into the same buffer All activities were calculated as a percent of the native luciferase activity and all data points are the average of at least two replicates

Acknowledgements

We thank M Cheetham and H.H Kampinga for critically reading the manuscript We also thank

Dr P Kouklis for helpful advice This work was sup-ported by grants from the EU (QLRT-1999, #30720) and the Greek Ministry of Education (Hrakleitos)

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