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Peter Rodemann1 1 Section of Radiobiology and Molecular Environmental Research, Department of Radiotherapy, and 2 Department of Molecular Pathology, University of TuÈbingen, Germany The

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Early growth response-1 gene ( Egr-1 ) promoter induction

Ralph G Meyer1,2, Jan-Heiner KuÈpper2, Reinhard Kandolf2and H Peter Rodemann1

1 Section of Radiobiology and Molecular Environmental Research, Department of Radiotherapy, and 2 Department of Molecular Pathology, University of TuÈbingen, Germany

The promoter of the early growth response gene (Egr-1)

has been described to be activated by ionizing radiation,

and it seems to be clear that this process involves di€erent

mitogen activated protein (MAP) kinases, dependent on

the speci®c cell type examined However, early steps

leading to activation of the corresponding pathways and

thus to overexpression of Egr-1 are not well understood

In this study, deletion mutants of the 5¢ upstream region

of the Egr-1 gene were generated which allowed us to

correlate the radiation±induction of the Egr-1 promoter in

U87 glioma cells to ®ve serum response elements Based on

the data shown, a possible role of two cAMP responsive

elements for radiation-dependent promoter regulation

could be ruled out On the basis of activator/inhibitor

studies applying fetal bovine serum, EGF, PD98059, anisomycin, SB203580, forskolin and wortmannin, it could be demonstrated that in U87 cells the ERK1/2 and potentially SAPK/JNK, but not the p38MAPK/ SAPK2, pathway contribute to the radiation-induction of Egr-1 promoter In addition, it was observed that irradi-ated cells secrete a di€usible factor into the culture media which accounts for the radiation-induced promoter upregulation By blocking growth factor receptor activa-tion with suramin, this e€ect could be completely abolished

Keywords: Egr-1 promoter; growth factor receptor; glio-blastoma cells; ionizing radiation

The immediate early gene Egr-1 (synonyms are NGFI-A,

zif268, TIS8 and krox24) encodes a transcription factor

involved in cell growth and differentiation The DNA

binding domain of this protein with its three zinc-®nger

motifs allows speci®c binding to GC rich recognition

sequences in the promoters of many downstream genes

and thus regulation of their expression Target genes of the

Egr-1 transcription factor are numerous and include growth

factors such as platelet derived growth factor A chain

(PDGF-A [1]), PDGF-B chain [2], basic ®broblast growth

factor (bFGF) [3], cytokines such as TGF-b [4] and other proteins that can be affected

Expression of Egr-1 itself is transiently induced by a variety of extracellular stimuli such as cytokines, growth factors such as FGF-2 [5], hypoxia [6], shear stress on vascular cells caused by blood current [7], tissue injury and physical stress in¯icted by ionizing radiation Publication of the latter ®nding [8] initiated investigations on how the Egr-1 promoter may be employed in cancer gene therapy approaches, controlling ectopic expression of therapeutic genes with the application of X-rays to target tissues [9±13] However, initial steps of the underlying mechanism of the observed radio-induction of Egr-1 expression are not completely understood, although further signal transduc-tion pathways involved in this gene activatransduc-tion are, at least in part, well characterized Functional dissection of the Egr-1 promoter sequence [14±16] revealed in previous studies that

it contains at least ®ve copies [17] of a characteristic transcription factor binding site designated the serum response element (SRE), which is described to be respon-sible for radioinducibility of the gene Due to its consensus sequence CC(A/T)6GG this motif is also known as the ÔCArGÕ element, and represents a combined recognition site for Elk-1, a member of the Ets family which acts as a ternary complex factor (TCF) in concert with other transcription factors, mainly p68/SRF serum response factor [18] The promoter is strongly activated upon binding of Elk-1/SRF transcription factor complexes to CArG elements [19] Complex assembly requires phosphorylation of both SRF and Elk-1 by speci®c kinases which are, at least in the case of Elk-1, in turn dependent on prior activation of mitogen activated protein kinases (MAPK) downstream of different signal transduction pathways At least three differently regulated but partly overlapping kinase cascade pathways

Correspondence to H Peter Rodemann, Section of Radiobiology and

Molecular Environmental Research, Department of Radiation

Oncology, University of TuÈbingen, RoÈntgenweg 11, D-72076

TuÈbingen, Germany Fax: + 49 7071 29 5900,

Tel.: + 49 7071 29 85962,

E-mail: hans-peter.rodemann@uni-tuebingen.de

Abbreviations: Egr-1, early growth response-1 gene; PDGF, platelet

derived growth factor; bFGF, basic ®broblast growth factor; SRE,

serum response element; MAPK, mitogen activated protein kinases;

TCF, ternary complex factor; SAPK, stress activated protein kinases;

Raf, ras-activated factor; ERK, extracellularly regulated kinase; PLC,

phospholipase C; FGF, ®broblast growth factor; AP-1, activated

protein-1; TRE, thiophorbolester responsive element; EgrBS, Egr-1

binding site; CRE, cAMP responsive element; MCS, multiple cloning

site; RSV, Rous sarcoma virus; rhEGF, recombinant human

epider-mal growth factor; PtdIns3-kinase, phosphatidylinositol 3-kinase;

b-Gal, b-galactosidase; PVDF, poly(vinylidene di¯uoride); ECL,

enhanced chemoluminescence; IL, interleukin.

De®nition: 1 gray (Gy) ˆ 100 rads.

(Received 18 July 2001, revised 26 October 2001, accepted 6 November

2001)

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converge in their activity on the phosphorylation of Elk-1,

including the cascade leading to the activation of stress

activated protein kinases (JNK/SAPK), the ras-activated

factor/extracellularly regulated kinase (Raf/ERK) pathway

and the activation of the p38 MAPK/SAPK2 pathway

Independently of these pathways, protein kinase C (PKC) is

able to phosphorylate Elk-1 directly PKC is activated by

diacylglycerol, which is formed by phospholipase C (PLC)

mediated phosphatidylinositol 4,5-diphosphate cleavage

PLC in turn is activated by binding to intracellular domains

of activated growth factor receptors, e.g the ®broblast

growth factor (FGF) receptor

In addition to SREs the 700-bp full length Egr-1

promoter comprises several kinds of other binding

sites including a JNK/SAPK dependent activated

protein-1/thiophorbolester responsive element (AP-1/TRE)

site, binding sites for Egr-1 itself (EgrBS) and two cAMP

responsive elements (CRE) For gene therapy purposes a

core promoter of 490 bp (nucleotides )425 to +65 relative

to the putative transcription start [9,10], was described to be

suf®cient for radioactivation This includes only the SREs,

Sp1 sites and the two CREs (see Fig 1) Whether or not

CRE sites contribute to radioinducibility of the Egr-1

promoter in normal cells was not clearly demonstrated to

date, although there is evidence that this is the case in

ras-mutated Jurkat cells which exhibit impaired MAP kinase

pathways [20]

In order to investigate the phenomenon of radiation

induction of the human Egr-1 promoter, glioblastoma

cells U87 were transiently transfected with expression

plasmids containing a reporter gene under the control of

wild-type and recombinant versions of the human Egr-1

promoter This system was used to investigate the Egr-1

promoter regulation under different experimental

condi-tions We show that Egr-1 promoter can be induced by a

single dose of 4 Gy The data presented indicate that

radiation induction of the Egr-1 promoter is at least in

part mediated by protein factors secreted by U87 cells

in response to radiation exposure The data are discussed

in the context of the potential use of Egr-1 promoter for

radiation-induced gene therapy strategies in radiation

oncology

M A T E R I A L S A N D M E T H O D S

Cloning of Egr-1 promoter variants

A 780-bp fragment of the human Egr-1 promoter was obtained by double restriction digestion of plasmid pGL/TiS8 [15] with SmaI/HindIII, with overhanging 5¢ ends ®lled up by using T4 DNA polymerase (Roche, Mannheim, Germany) The promoter fragment was then ligated blunt into pCR-Script SK+ (Stratagene) The resulting plasmid pEgr was used for sequencing and as a source of all following promoter variants which were generated by conventional plasmid construction methods using the restriction enzymes depicted in Fig 1 As an exception pD7egr was generated by site directed mutagenesis

of pD5egr (see below) Plasmid pD6egr is similar to pD5egr but contains an additional cluster of SRE/Ets sites in a fragment which was generated by cutting pD3egr with Eco47III/AccIII and polishing the ends of the 207 bp fragment with T4 DNA polymerase All promoter versions were excised from their host plasmids and cloned into pGFL cut with SmaI The resulting plasmids were desig-nated pwtegrGFL, pD1egrGFL, pD2egrGFL, etc

Expression plasmid pGFL is based on pGL3basic (Promega) but the luciferase gene was replaced by an in-frame ®re¯y luciferase/EGFP fusion with the original multiple cloning site (MCS) and the synthetic upstream 5¢ polyadenylation signal which blocks unspeci®c transcrip-tion activatranscrip-tion The presence of EGFP as part of the luciferase gene allows additional comparison of transfection ef®ciencies in parallel cultures Physical properties of the novel GFL protein were investigated in several sets of plasmid transfection experiments which showed, that in the fusion protein luciferase activity was constantly lowered to

 70% of the unfused luciferase gene Also, EGFP ¯uores-cence was decreased to an estimated  65±70% of free EGFP Extensive tests, including complete sets of experi-ments described in this study were performed in order to ensure that there was no alteration of promoter behaviour

in corresponding luciferase/luciferase±EGFP vectors (data not shown) All cloning steps were controlled and veri®ed by restriction analysis

Fig 1 The human Egr-1 promoter and its regulatory elements as cloned into pwtegrGFL As a key region the sequence from nucleotides )136 to )56 is shown in detail, comprising two serum response elements (SRE) ¯anked by two cAMP responsive elements (CRE) Other binding sites are located upstream of SRE 1±3, namely three Sp1 binding sites, two recognition sequences for the Egr-1 gene product itself (EgrBS) and an AP1 binding site.

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Site-directed mutagenesis

Plasmid pD7egrGFL was generated by exchange of ®ve

nucleotides in CRE2 (nucleotides )71 to )58) from

ACGTC to CTCAT by site directed mutagenesis using a

kit (Stratagene) The primer sequence (5¢)3¢) was CCCA

TATATGCCATGTCTCATCACGACGGAGGCGG

Successful mutagenesis was con®rmed by sequence analysis

The de®ciency of this altered sequence to bind CREB was

previously published [18]

As a positive control a well characterized Rous Sarcoma

Virus (RSV) promoter, excised from pAdRSVbgal, was

inserted into pGFL, resulting in pRSVGFL and sequenced

This promoter stems from rous sarcoma virus, strain

Schmidt±Ruppin (EMBL database accession no L29198)

Cell culture and transfection procedures/irradiation

of transfected cells

Human U87 glioma cells were kept in DMEM (Gibco),

supplemented with 10% fetal bovine serum (Gibco), under

standard cell culture conditions (5% CO2, 37 °C)

FuGene (Boehringer Mannheim) transfections were

performed according to instructions of the manufacturer

Transfection ef®ciencies were determined by transfection of

plasmid pCMVb (Clontech) into U87 cells; 48 h after

transfection cells were stained for b-galactosidase (b-Gal)

activity using the b-Gal staining kit purchased from

Invitrogen

Routine luciferase activity measurement procedures were

performed according to the following procedure Cells were

plated at a density of 105cells per 35 mm dish and allowed

to attach for 24 h FuGene transfections were performed by

using 900 ng pDxEgrGFL per cell culture dish pCMVb

(100 ng; Clontech) was added to each culture dish for

internal control of transfection ef®ciency Negative controls

were performed by transfecting promoterless pGFL as well

as pRSVGFL constructs in parallel As tested by pilot

experiments, cotransfection of pCMVb did not in¯uence

basal Egr-1 or RSV promoter activity signi®cantly

Twenty-four hours after transfection, cells were exposed to a single

dose of 4 Gy of ionizing radiation generated by a linear

accelerator (Mevatron 6MeV, LINAC) as described

else-where [20,21]

Cells were harvested 48 h after irradiation and assayed

for luciferase activity In experiments using speci®c effectors

of Egr-1 promoter activity these factors/substances were

added 6 h prior to cell harvest (i.e after 42 h)

Inhibitor and activator studies

Speci®c activators and inhibitors to signal transduction

pathways, except for fetal bovine serum, were obtained

from Calbiochem and dissolved to the following working

solutions

Fetal bovine serum fetal bovine serum (Gibco Life

Technologies) was added to a ®nal concentration of 30%

in the culture medium serving as a positive control for

ERK1/2 activation

Recombinant human epidermal growth factor

(rhE-GF) Stock solutions at a concentration of 100 lgámL)1

in an aqueous solution of 0.3% BSA with 10 mMacetic acid were added to the culture media at a ®nal concentration of

100 ngámL)1 rhEGF was used as a positive control for the immediate early activation of the Egr-1 promoter by activated Ras-dependent pathways

PD98059 This was added as a 50-mM solution in dimethylsulfoxide to the media making a ®nal concentration

of 100 lM This compound is a potent inhibitor of MEK1 (IC50 ˆ 5±10 lM) and to a lesser extent of MEK2 [22,23], two upstream protein kinases which activate ERK1/2 Anisomycin This was dissolved in dimethylsulfoxide (10 mgámL)1) and immediately added to the culture media

at a ®nal concentration of 50 lM Anisomycin (from Streptomyces griseolus) activates p38MAPK/SAPK2 and SAPK/JNK and served as a positive control in this study It

is also an inhibitor of protein expression at the translational level

SB203580 This was added as a 1-mMworking solution in dimethylsulfoxide to the cells to a ®nal concentration of

10 lM It was used to inhibit p38MAPK/SAPK2 activity Forskolin This was prepared as a 10-mM stock solution

in dimethylsulfoxide and directly added to the culture medium to make a ®nal concentration of 10 lM Being a strong and speci®c activator of adenylate cyclase, forsko-lin induces increased levels of cAMP in treated cells This

in turn activates cAMP-dependent protein kinase A (PKA) which phosphorylates CREB and other target proteins

Wortmannin A 1 mMstock solution in dimethylsulfoxide was further diluted 1 : 100 in NaCl/Pi and ®nally added

as a 10-lMworking solution with a ®nal concentration in the media of 100 nM As a speci®c inhibitor of phosphat-idylinositol 3-kinase (PtdIns3-kinase, IC50 ˆ 5 nM) wort-mannin allows us to investigate downstream signalling of the PtdIns3 pathway and dependent activation events Suramin Suramin (Sigma, St Louis, MO, USA) was added

as an aqueous 30 mMstock to the media to make a ®nal concentration of 300 lM This substance interferes with the recognition of several growth factors by their membrane receptors and, in addition, disrupts the interaction of growth factor receptors with corresponding adenylate cyclase activating G-proteins

For control conditions, cells were treated with equal amounts of the corresponding solvent (e.g dimethylsulf-oxide)

Cell lysis and quanti®cation of reporter gene activities Cell monolayers were scraped off with a rubber policeman

in 100 lL of reporter lysis buffer (Promega), transferred to 1.5 mL reaction tubes, centrifuged (13 000 g for 60 s) in a conventional bench-top centrifuge and kept on ice until measurements of luciferase activity, b-Gal activity and protein content which were performed from the same cell aliquots

Protein content was estimated using Bradford's reagent (Biorad), b-Gal activity was measured by employing a

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commercial kit (Invitrogen) Luciferase activity was

deter-mined with a kit from Promega and measured in a

luminometer (Berthold); measured values were normalized

to speci®c b-Gal activity Egr-1 promoter stimulation by

ionizing radiation or chemical compounds was performed

only for the three major promoter mutant plasmids

pD1egrGFL, pD5egrGFL and pD7EgrGFL All

transfec-tion experiments were performed in triplicates and

repro-duced at least three times

Immunoblotting and detection of activated protein

factors with phospho-speci®c antibodies

For Western blot analyses cells were cultured in 60 mm

dishes under normal cell culture conditions Treatment with

speci®c inhibitors or exposure to a single dose of 4 Gy of

c-irradiation were performed as described above Thirty

minutes after treatment with activators or inhibitors or

radiation exposure, cells were washed twice with NaCl/Pi,

SDS sample buffer was added and cells scraped off the plate

and subjected to denaturing SDS/PAGE Proteins were

subsequently blotted to a poly(vinylidene di¯uoride)

(PVDF) membrane and detected using phosphospeci®c or

phosphorylation-state-independent antibodies according to

the recommendations of the manufacturer (Cell Signaling

Technology, New England Biolabs) As secondary

antibod-ies, monoclonal horseradish coupled anti-(rabbit Ig) Ig or

anti-(mouse Ig) Ig was used allowing identi®cation of

protein bands using enhanced chemoluminescence (ECL)

detection For detection of site-speci®c phosphorylated

target proteins, i.e ERK1/2 (T202/Y204), SAPK/JNK

(T183/Y185), p38MAPK/SAPK2 (T180/Y182), ATF-2

(T71), c-Jun (S73) and CREB (S133) phosphospeci®c rabbit

polyclonal Ig was applied

Phosphorylation-state-indepen-dent polyclonal antibodies were used to detect total Egr-1, ATF-2 and c-Jun protein

R E S U L T S

Basal activity of Egr-1 promoter variants Basal activities of cloned variants of the Egr-1 promoter were analyzed by measuring the luciferase reporter gene activity Transfection experiments with pwtegrGFL showed that basal activity of the wild-type Egr-1 promoter construct was roughly 10±12% of the activity displayed by a control RSV promoter

As demonstrated in Fig 2, the relative activity of promoter variant pD1egrGFL (nucleotides )474 to +12) did not differ signi®cantly from that of the wild-type promoter construct pwtegrGFL (nucleotides )720 to +12) These data indicate that regulatory promoter ele-ments upstream of nucleotide )474 do not contribute signi®cantly to basal promoter activity under the conditions applied In contrast however, deletion of nucleotides )259 to )126 which results in promoter construct pD3egrGFL led to

a small but signi®cant increase in relative basal luciferase activity (110.5 ‹ 2.3% of control activity, P < 0.05) A similar, but more pronounced, effect was observed with promoter variant pD5egrGFL also lacking nucleotides )259

to )126 but, as compared to pD3egrGFL, additionally missing the sequence )474 to +12 This promoter variant presented a signi®cantly( p < 0.005) enhanced relative basal activity of 137.1 ‹ 5.7% These data indicated, that dele-tion of the CRE1 site and of the putative Sp1 recognidele-tion site results in an upregulation of basal Egr-1 promoter activity Insertion of an additional cluster of two SRE/Ets binding sites (nucleotides )474 to )265) into pD5egrGFL resulting

Fig 2 Basal activity of Egr-1 promoter variants in U87 glioma cells Deletion mutants of the human Egr-1 promoter were generated in order to con®ne the radio-induction e€ect of the promoter to speci®c transcription factor binding sites For comparison of promoter activity in a noninduced state, resulting promoter variants D1egr, D2egr, D3egr, D4egr, D5egr, D6egr and D7egr were cloned into pGFL, carrying an in-frame fusion of EGFP and ®re¯y luciferase (termed GFL) and transfected into U87 cells Luciferase activities under normal cell culture conditions were considered as basal promoter activities, which were compared to wild-type Egr-1 promoter activity.

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in the variant pD6egrGFL, led to a further but, as compared

to pD5egrGFL, nonsigni®cant increase in basal promoter

activity (158 ‹ 9.1%)

Removal of this cluster of SRE/Ets bindings sites, as

performed in pD2egrGFL and pD4egrGFL, always led to a

dramatic decrease of basal promoter performance to

11.1 ‹ 0.5% (pD2egrGFL) and 10.5 ‹ 0.3%

(pD4egr-GFL) of wild-type promoter activity

Site directed mutagenesis of CRE2 in pD5Egr resulted

in promoter variant pD7Egr, which contains only the SRE

and Ets binding sites of the wild-type promoter

pD7egr-GFL presented a signi®cantly (P < 0.005) reduced

pro-moter activity which was 61.5 ‹ 2.8% of the wild-type

promoter

Immunoblotting of U87 cell lysates followed by

detec-tion of activated ERK1/2 with phosphospeci®c ERK1/2

(T202/Y204) antibodies demonstrated detectable amounts

of activated ERK1/2 already formed under normal cell

culture conditions Relatively high concentrations of

phos-phorylated CREB (S133) and ATF-1 were detected,

whereas there appeared to be no detectable amounts of

activated ATF-2 nor SAPK/JNK

Effect of serum, rhEGF and ionizing radiation

on promoter activity

To analyse the effect of fetal bovine serum and human

recombinant EGF on Egr-1 promoter activity the promoter

variants D1egr, D5egr and D7egr were used Increasing the

concentration of fetal bovine serum in the culture medium

to 30% resulted in an ef®cient induction of all three

promoter plasmids tested (pD1egrGFL pD5egrGFL and

pD7egrGFL) within a 6-h interval of application As shown

in Fig 3 the corresponding luciferase activity increased to

157.3 ‹ 12.6% (pD1egrGFL), 149.2 ‹ 13.4%

(pD5egr-GFL), or 206.6 ‹ 33.1% (pD7egr(pD5egr-GFL), respectively, as

compared to wild-type activity

Treatment of U87 cells carrying these promoter

con-structs with 10 ngámL)1rhEGF resulted in a pronounced

stimulation of promoter activities to 205.5 ‹ 18.8% in pD1egrGFL transfectants, to 151.9 ‹ 11.4% in pD5egr-GFL transfectants and to 211.5 ‹ 22.4% to pD7egrpD5egr-GFL transfectants as compared to cells transfected with the wild-type promoter construct (Fig 3)

As indicated by time kinetic experiments, increased levels

of ®re¯y luciferase activity due to the exposure of pwtegrGFL-, pD1egrGFL-, pD5egrGFL-, and pD7eg-rGFL-transfected U87 cells to a single dose of 4Gy of ionizing irradiation could be observed to be maximal after 40±48 h post IR (data not shown) As compared

to sham-irradiated controls luciferase activities measured

48 h post IR were increased signi®cantly to 133.7 ‹ 4.3% for pD1egrGFL-, 119.1 ‹ 5.0% for pD5egrGFL and 138.7 ‹ 4.2% for pD7egrGFL-transfected U87 cells (all

P << 0.005)

Protein kinase inhibitor/activator studies

As shown in Fig 3, a 6-h treatment of U87 cells transfected with the three Egr-1 promoter mutants with PD98059 (100 lM), a speci®c inhibitor of MEK1, decreased relative luciferase activities by about 20±30%

as compared to wild-type control levels (pD1egrGFL: 82.6 ‹ 3.5%; pD5egrGFL: 67.6 ‹ 4.8%; pD7egrGFL: 72.0 ‹ 4.7%)

Under the same treatment conditions anisomycin, a speci®c activator of p38MAPK/SAPK and SAPK/JNK, did not alter the luciferase activity of pD1egrGFL (relative activity: 103.3 ‹ 6.8%) and pD7egrGFL (relative activity: 106.5 ‹ 19.8%) as compared to wild-type controls How-ever, anisomycin resulted in a signi®cant (P < 0.005) inhibition of the pD5egrGFL luciferase activity by about 26% (relative activity: 74 ‹ 2.1%) Treatment with SB203580, which is a potent inhibitor of p38MAPK/SAPK, resulted in a pronounced promoter activation of pD1eg-rGFL (131.7 ‹ 9.5%, P < 0.005) and pD7egpD1eg-rGFL (124.2 ‹ 12.3%) In contrast to these results a signi®cant decrease in luciferase activity by about 27% could be

Fig 3 D1egr, D5egr and D7egr promoter activities as a function of inhibitors/activators of speci®c signal transduction pathways U87 cells were transfected with reporter gene constructs containing an in-frame EGFP±luciferase gene under the control of modi®ed Egr-1 promoters (see Fig 1) using FuGene transfection reagent (Roche, Mannheim, Germany) Forty-two hours after the start of transfection cells were treated with chemical e€ectors as indicated Cells were further incubated for 6 h and assayed for luciferase activity 48 h post transfection Irradiated cells were exposed to

a single dose of 4 Gy of ionizing radiation 16 h after the start of transfection and luciferase activity was determined 48 h postirradiation Cotransfected plasmid pCMVbGal (Clontech) was used as an internal control of transfection eciency in all samples Data represent the mean ‹

SE from three to six experiments performed in triplicates.

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observed in pD5egrGFL-transfected cells (relative activity:

73.1 ‹ 6.6%; P < 0.005) (Fig 3)

Treatment with 10 lM forskolin, a speci®c activator of

adenylate cyclase, did not signi®cantly alter the promoter

activity in cells transfected with the luciferase reporter

constructs pD1egrGFL and pD7egrGFL, but led to a slight,

but signi®cant decrease to 84.2 ‹ 8.9% (P < 0.05) of

relative activity in cells transfected with pD5egrGFL

(Fig 3)

For all three promoter variants tested, treatment of the

transfected cells with wortmannin, a speci®c inhibitor of

PtdIns3 kinase, resulted in a measurable downregulation,

which ranged between 10% and 17% (pD1egrGFL:

84.0 ‹ 6.8%; pD5egrGFL: 82.9 ‹ 15.3%; pD7egrGFL:

90.8% ‹ 4.1%) within a 6-h interval

In order to analyse, whether factors produced and

secreted in response to radiation exposure may alter the

activity levels of the promoter variant construct pD7egrGFL

in transfected cells, a cross feeding experiment as described

in Materials and methods was performed When culture

media from irradiated was fed to nonirradiated cells

transfected with promoter variant pD7egrGFL the luciferase

activity was increased to approximately the same level

(130.6 ‹ 4.8%) as in irradiated cells (132 ‹ 10.2%)

Levels of activity in the irradiated cells did not decrease

signi®cantly after addition of control medium for up to 6 h,

indicating a longer lasting secretion of activator molecules

or growth factors Adding suramin, a potent inhibitor of

growth factor receptor±ligand binding, to the culture

medium of irradiated cells or nonirradiated cells fed with

medium from irradiated cells the stimulatory effect on

luciferase activity of promoter variant plasmid pD7egrGFL

could completely be abolished (87.49 ‹ 10.15%, 0 Gy and

84.89 ‹ 11.87%, 4 Gy, Fig 4)

Western-blot analyses For the interpretation of the regulatory function of the different Egr-1 promoter elements and the role of speci®c signal transduction pathways in activating the Egr-1 pro-moter with and without radiation exposure Western blot analyses of untransfected cells for different target proteins and their phosporylation status were performed Therefore, protein extracts from the same set of cells used for the analyses of luciferase activity under different treatment conditions with serum, rhEGF and ionizing radiation as well as inhibitors or activators of speci®c protein kinases were used

Fetal bovine serum treatment After treatment with 30% fetal bovine serum increased ERK1/2 phosphorylation was shown by immunoblot analysis (Fig 5) This could account for the promoter induction shown in Fig 3 While there was slight activation of c-Jun (S73), ATF-2 phosphorylation did not seem to be affected by elevated fetal bovine serum concentration (Fig 5)

RhEGF-treatment Treatment with 10 ngámL)1 rhEGF resulted in the strongest phosphorylation and activation of ERK1/2 (T202/Y204) (Fig 5), re¯ecting the highest Egr-1 promoter induction as shown for all mutants tested (Fig 3) Immunoblots incubated with phospho-speci®c antibodies revealed increased levels of phosphorylated CREB and ATF-1 (S133), SAPK/JNK (T183/Y185) as well as upre-gulation at the translational level and activation of ATF-2 (T71) and c-Jun (S73) An increase in p38MAPK/SAPK2 (T180/Y182) activation was not observed

Radiation exposure After exposure to ionizing radiation, phosphorylated SAPK/JNK was detectable, but to a much lesser degree than it was observed after rhEGF treatment (Fig 5) Activation of p38MAPK/SAPK2 could not be detected and ERK1/2 phosphorylation was slightly lower than in control samples As a result, there were only low amounts of phosphorylated CREB (S133); however, the level of phosphorylated ATF-1 remained unchanged as compared to controls Furthermore, radiation exposure resulted in high amounts of activated ATF-2 and c-Jun As

it could be demonstrated using speci®c phosphorylation-independent antibodies as controls for ATF-2 (T71) and c-Jun (S73) levels the expression of both proteins was strongly upregulated

PD98059 As illustrated in Fig 5, PD98059 as an inhibitor

of MEK1, clearly prevented activation of MEK1 (IC50 ˆ 5±10 lM) As ERK1 and ERK2 are activated

by MEK1, treatment of U87 cells with 100 lM PD98059 speci®cally abolished the phosphorylation of ERK1/2 without affecting the activity status of ATF-1, ATF-2, SAPK/JNK, and c-Jun

Anisomycin Exposure of U87 cells to 10 lM anisomycin did not result in marked changes in phosphorylation status of ERK1/2 The amount of phospho-SAPK/JNK (T183/Y185) and especially of phospho-p38MAPK/SAPK2 (T180/Y182) were strongly increased (Fig 5) This activa-tion coincided with high levels of phosphorylated CREB, ATF-1 and ATF-2; however, phosphorylation or activation

Fig 4 Suramin inhibits radiation-induced Egr-1 promoter activation.

After transient transfection with plasmid pD7egr, U87 cells were

irra-diated (4 Gy) and incubated without subsequent exchange of culture

media (Control) After 42 h, media were removed from irradiated cells

and replaced by media from parallel, unirradiated, transfected cells

(A2) The unirradiated cultures, in turn, received media from

corre-sponding irradiated cultures (A1) The addition of culture media from

irradiated cells led to an increase in luciferase activity in the

unirradi-ated cells (A1) up to the level reached by irradiunirradi-ated cells (control cells

and A2) Addition of 300 l M suramin abolished the e€ect (B1, B2).

Cells were harvested after a total time interval of 48 h and luciferase

activities were determined Data represent the mean ‹ SE from three

independent experiments performed at least in triplicates.

Trang 7

of c-Jun (S73) was only marginal By using a pan-c-Jun

antibody, which recognizes c-Jun independently of its

phosphorylation status, a partial phosphorylation of the

c-Jun protein, presumably in position S63, could be

demonstrated

SB203580 As control cells, grown under standard

conditions, presented basically no phosphorylated

p38MAPK/SAPK2, no alterations of the phosphorylation

pro®le was to be expected by treating the cells with the

p38MAP-kinase inhibitor SB203580 However, potentially

as side-effects which have also been described in the recent

literature, SB203580 caused strong activation of ERK1/2

(T202/Y204) via activation of Raf1 [24±26] and inhibition of

CREB/ATF1 activation as shown in immunoblots at a

concentration of 10 lM

In this context it remains to be addressed in more detail

whether the profound promoter activation of pD1egrGFL

and pD7egrGFL shown in Fig 3 is related to the Western

blotting results

Forskolin While forskolin had no effect on the

phospho-rylation of SAPK/JNK, p38MAPK/SAPK2, ATF-2 or

c-Jun, a marked increase in phospho-CREB (S133) levels

could be observed (Fig 5) As CREB phosphorylation is a

cAMP-dependent reaction [27], this observation proves

functionality of the drug As shown in Fig 5 in agreement

with results from others [28] forskolin abolished ERK1/2 phosphorylation in U87 cells The extent of inhibition was comparable to that shown above for PD98059

Wortmannin As a consequence of wortmannin treatment

no activation of SAPK/JNK or p38MAPK/SAPK2 was observable and the amounts of phosphorylated ERK1/2 were slightly diminished Additionally no effect on ATF-2 phoshorylation or expression could be observed; however, reduced levels of activated CREB, ATF-1 and c-Jun were present after treatment with wortmannin, whereas no phosphorylated c-Jun could be detected

D I S C U S S I O N

One of the main aims of this work was to investigate mechanisms of radiation induction of the human Egr-1 promoter and its potential use for radiation induced gene therapy as recently reported [9,29] While it is ®rmly established, that the Egr-1 promoter is effectively and quickly activated by growth factors, such as EGF, bFGF and other serum compounds [5,30,31], mechanisms leading

to induction by radiation are by far less well understood Most likely both, growth factor and radiation stimuli ultimately lead to the binding of SRF and TCF/Elk-1 to SREs which are recognized as overlapping CArG/Ets binding sites forming the core promoter [14±17] By the

Fig 5 Immunoblot analyses of activated protein factors in U87 cells using polyclonal phosphospeci®c antibodies U87 cells were subjected to various treatments with chemical compounds for a time interval of 30 min and then lysed Cells exposed to 4 Gy of ionizing radiation were incubated for

30 min prior to harvest Lysates were resolved by SDS/PAGE and subsequent immunoblotting with polyclonal rabbit antisera directed speci®cally against the phosphorylated proteins indicated (phosphorylated amino-acid residues are given in brackets) Phosphorylation-state-independent rabbit polyclonal antibodies recognized total Egr-1, ATF-2 and c-Jun protein.

Trang 8

stepwise removal all other known regulatory elements from

the 5¢ upstream region of the wild-type Egr-1-promoter,

such as CREs as well as AP1-, Egr-1- and Sp1- binding sites,

we were able to provide additional evidence supporting the

prevailing view that these binding sites are suf®cient to

maintain responsiveness of the Egr-1 promoter to EGF and

ionizing radiation

In general, the radiation-dependent Egr-1 promoter

upregulation in U87 glioma cells observed in the present

study was weak but signi®cant A single dose of 4 Gy

upregulated the promoter variant pD7egrGFL by a factor of

1.4 (p < 0.05) Similar data of induction of the Egr-1

promoter by ionizing radiation have been reported recently

[29] Using synthetic promoter constructs consisting merely

of repetitive SRE consensus sequences Marples et al [29]

described an upregulation of Egr-1 by a factor of 1.5±2.5

after radiation exposure of U87 cells

Based on literature data [32] it could be expected that

stimulation with EGF results in the phosphorylation and

thus binding of TCF/Elk-1 to SRE through activation of the

MAP kinases ERK1/2 or SAPK/JNK or both However, in

our hands strong activation of p38MAPK/SAPK2 was not

observed in U87 cells except after anisomycin treatment

Immunoblot analyses showed activation of ERK1/2 after

stimulation of U87 cells with fetal bovine serum, EGF and

SB203580 but not after exposure to ionizing radiation This

data indicate that ERK1/2 and SAPK/JNK pathways may

be activated apart from each other Both, SAPK/JNK and

ERK1/2, are activated upon growth factors binding to

their receptors However, signal transduction leading to

JNK/SAPK activation is known to be mainly triggered by

ultraviolet light (UV-C) [34±36], ionizing radiation

(reviewed in [37]), proin¯ammatory cytokines [30,31] and

DNA damaging agents [37], whereas the Raf/ERK pathway

is preferentially activated upon binding of growth factors to

receptor tyrosine kinases ([18] and many others)

While there is some overlap of both pathways our data

based on EGF treatment and protein kinase inhibitor

studies suggest a clear preference of the ERK1/2 pathway

after binding of EGF to its receptor, whereas ionizing

radiation seems to favour SAPK/JNK activation as

dem-onstrated by the pronounced c-Jun activation observed by

Western blot analyses As a clear immediate early reaction

after exposure to ionizing radiation a strong increase in

c-Jun activation and expression was apparent Although in

our study no evidence has been obtained that Egr-1

immediate early gene induction could be observed 30 min

after exposure to ionizing radiation, Liu et al [38] reported

that exposure of serum-depleted, quiescent U87 cells

presented a slight induction of Egr-1 2 h after exposure to

UVC

Forskolin inhibited ERK1/2 phosphorylation under

normal cell culture conditions, but had no signi®cant effect

on Egr-1 promoter activity in our experimental setup As it

has also been reported by others [28] as a speci®c side-effect

of forskolin this compound abolished ERK1/2

phosphory-lation in the U87 cells used in the present study Therefore,

this ®nding supports the view, that Egr-1 promoter activity

is not strictly dependent on ERK1/2 activity, but may in

part be regulated by the SAPK/JNK [39,40] or the PKC

pathway Furthermore, in the present study we were able to

show that binding of EGF to its receptor led to strong Egr-1

expression U87 cells transfected with Egr-1 reporter

constructs On the other hand, expression of ATF-2 and c-Jun was not signi®cantly affected after EGF treatment of these cells, but strongly induced after exposure to ionizing radiation The fact that ATF-2 and c-Jun were phospho-rylated to a great extent due to the radiation exposure, provides good evidence for the activation of an intact SAPK/JNK pathway, as this is the major kinase activating the two transcription factors [35,41]

Secretion of bFGF and interleukin-1a (IL-1a) has been reported after UV-irradiation of HeLa or normal ®broblast cells [42] This phenomenon may help to transmit a radiation-induced signal to nonirradiated cells Moreover

it may establish an obligatory growth factor loop on the producer cell, both leading to expression of immediate early genes, e.g c-Jun, via the activation of SAPK/JNK [42,43] Growth factor-mediated early step in radiation-induced cell signaling could be inhibited either by speci®c antibodies directed against bFGF or IL-1a as well as by preincubation with suramin [42,43] These results although obtained after irradiating cells with UV light are in perfect agreement with the immunoblot analyses and suramin inhibition experi-ments presented in our study indicating an auto- and/or paracrine growth factor dependency of Egr-1 promoter activation by ionizing radiation However, in contrast to the immediate-early expression observed for c-Jun, radiation-induction of Egr-1 seems to be a rather slow, long-lasting and potentially SAPK/JNK independent phenomenon which may involve additional, so far unknown, mecha-nisms Based on data reported by Woloschak et al [44] it is very likely, that activation of protein kinase C (PKC) adds

to the phosphorylation of Elk-1 and therefore to the induction of Egr-1 expression in response to radiation exposure With respect to these results and our own data it can be assumed, however, that growth factor release from irradiated cells unequivocally contributes to radiation-mediated Egr-1 expression via the ERK1/2 or the PKC pathway However, how the secretion into the media is triggered still remains an open question and needs to be investigated further

As a second aspect of Egr-1 gene regulation, our data indicate a strong impact of CRE sites on basal promoter activity This suggests, that the wild-type promoter in U87 glioma cells is in part also dependent on the phosphoryla-tion state of CREB, ATF-1, ATF-2 and c-Jun proteins As reported by Van Dam et al [39], activation of ATF-2 upon genotoxic stress is mediated preferentially by SAPK/JNK, leading to the induction of c-Jun expression According to our data, the SAPK/JNK pathway transmits at least part of Egr-1 radiation-induction The CRE sites may thus be involved in the radiation-dependent Egr-1 expression Indeed, stress induced activation of Egr-1 gene expression via promoter-CRE sites has been described for ras-mutated Jurkat cells which present an impaired Ras/Raf/ERK pathway [20] However, under the experimental conditions applied in this investigation, a speci®c radiation-dependent regulation of CRE sites was not observed

As indicated by the deletion of CRE2 in the pD7egrGFL mutant, this element positively regulates Egr-1 promoter activity (see Fig 2) Inhibition of p38MAPK/SAPK2 dependent activation of these proteins may therefore account for the low pD5egrGFL promoter activity after SB203580 incubation This promoter construct contains only one CRE2 element Deletion of CRE1 as performed in

Trang 9

pD5egrGFL revealed its role as a negative regulatory

element, which is in line with previously published work

[15,46] The presence of both, an activating CRE2 and an

inhibitory CRE1 in pD1egrGFL may therefore neutralize

the effects of SB203580 on CREB/ATF1 phosphorylation

Thus, in pD1egrGFL and pD7egrGFL transfected U87 cells

SB203580 induces increased luciferase activity merely due to

ERK1/2 activation

Taken together in the present study we provide evidence

for the radiation-induction of the Egr-1 promoter and the

regulatory signal transduction pathways involved in this

activation While no evidence for activation of the

p38MAPK/SAPK2 pathway exist from our data, other

pathways involving ERK1/2 and potentially SAPK/JNK

seem to be primarily involved in the initial signal from the

receptor protein to the Egr-1 promoter Most interestingly,

however, a bFGF-like factor released by irradiated cells

contributes markedly to the radiation-induction of the

Egr-1 promoter via upstream SRE elements Closer insight into

the very early events of Egr-1 gene induction and

identi®-cation of the secreted factor will be useful for further

successful utilization of the Egr-1 promoter in combined

radiation-inducible gene therapy approaches as well as for

the understanding of stress-dependent regulation of cell

growth in general

A C K N O W L E D G E M E N T S

Vector pAdRSVbgal was a kind gift from Dr JuÈrgen Kleinschmidt,

Deutsches Krebsforschungszentrum Heidelberg Thanks also to

Kathleen M Sakamoto, University of California, Los Angeles, for

permission to use plasmid pGL/TiS8 This work was supported by a

grant from the Deutsche Forschungsgemeinschaft (Ro527/3-1,2) and

the Dr Mildred Scheel Stiftung (10-1503-KuÈ I).

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