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In HeLa cells, the highest increment of c-Fos mRNA content was noted after 6 h of Na+⁄ K+-ATPase inhibition with ouabain that was abolished by actino-mycin D, an inhibitor of RNA synthes

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by activation of the 5¢-promoter containing known

transcriptional elements

Mounsif Haloui1,*, Sebastien Taurin1,2,*, Olga A Akimova1, Deng-Fu Guo1, Johanne Tremblay1, Nickolai O Dulin2, Pavel Hamet1and Sergei N Orlov1

1 Centre de recherche, Centre hospitalier de l’Universite´ de Montre´al (CHUM) ) Technopoˆle ANGUS, Montreal, PQ, Canada

2 Department of Medicine, University of Chicago, Chicago, IL, USA

Previously, we reported that elevation of the

[Na+]i⁄ [K+]i ratio, caused by sustained inhibition of

Na+⁄ K+-ATPase with ouabain or in K+-free

med-ium, inhibits apoptosis in serum-deprived vascular

smooth muscle cells (VSMCs) [1] Subsequently, the

antiapoptotic action of Na+⁄ K+-ATPase inhibition

was also detected in cultured renal proximal tubule

cells [2], freshly isolated rat cerebellar granule cells [3], and endothelial cells from the human umbilical vein [4] and porcine aorta [5] With endothelial cells, we found that Na+⁄ K+-ATPase inhibition blocked apoptosis triggered by3H-induced DNA damage via elevation of [Na+]i rather than attenuation of [K+]i [5] We also noted that in VSMCs, protection against apoptosis

Keywords

c-Fos; expression; intracellular Na+; ouabain;

5¢-UTR

Correspondence

S N Orlov, Centre de recherche,

CHUM ) Technopoˆle ANGUS, 2901, Rachel

est, Montreal, Quebec H1W 4A4, Canada

Fax: +1 514 412 7638

Tel: +1 514 890 8000

E-mail: sergei.n.orlov@umontreal.ca

*These authors contributed equally to this

work

(Received 4 January 2007, revised 25 April

2007, accepted 16 May 2007)

doi:10.1111/j.1742-4658.2007.05885.x

In vascular smooth muscle cells and several other cell types, inhibition of

Na+⁄ K+-ATPase leads to the expression of early response genes, including c-Fos We designed this study to examine whether or not a putative

Na+i⁄ K+

i-sensitive element is located within the c-Fos 5¢-UTR from) 650

to + 103 containing all known response elements activated by ‘classic’ stimuli, such as growth factors and Ca2+

i-raising compounds In HeLa cells, the highest increment of c-Fos mRNA content was noted after 6 h of

Na+⁄ K+-ATPase inhibition with ouabain that was abolished by actino-mycin D, an inhibitor of RNA synthesis c-Fos protein accumulation in ouabain-treated cells correlated with a gain of Na+iand loss of K+i Aug-mented c-Fos expression was also observed under inhibition of Na+⁄ K+ -ATPase in K+-free medium and in the presence of the Na+ ionophore monensin The effect of ouabain on c-Fos expression was sharply attenu-ated under dissipation of the transmembrane Na+ gradient, but was pre-served in the presence of Ca2+ chelators and the extracellular regulated kinase inhibitor PD98059, thus indicating an Na+i-mediated, Ca2+i- and extracellular regulated kinase-independent mechanism of gene expression

In contrast to massive c-Fos expression, we failed to detect any effect of ouabain on accumulation of luciferase driven by the c-Fos 5¢-UTR Negat-ive results were also obtained in ouabain-treated vascular smooth muscle cells and C11 Madin–Darby canine kidney cells possessing augmented c-Fos expression Our results reveal that Na+i-induced c-Fos expression is not mediated by the 5¢-UTR containing transcriptional elements activated

by growth factors and other ‘classic stimuli’

Abbreviations

CRE, Ca2++ cAMP response element; ERK, extracellular regulated kinase; LDH, lactate dehydrogenase; MDCK, Madin–Darby canine kidney; NaRE, Na + response element; SRE, serum response element; VSMC, vascular smooth muscle cells.

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was almost completely abolished by inhibitors of RNA

and protein synthesis [6], suggesting the de novo

expression of genes involved in suppression of the cell

death machinery This hypothesis was confirmed by

proteomics-based analysis of soluble proteins from

control and ouabain-treated VSMCs, leading to the

identification of mortalin as an antiapoptotic gene

trig-gered by elevation of the [Na+]i⁄ [K+]iratio [7]

Keeping in mind the increase of total RNA synthesis

seen in ouabain-treated VSMCs [6], we proposed that

the expression of antiapoptotic genes, including

morta-lin, is at least partially mediated by early response

genes [8] This hypothesis was also consistent with

accumulation of early response gene mRNA detected

in cultured renal epithelial cells, fibroblasts,

hepato-cytes, and leukemia and melanoma cell lines, as well as

in freshly isolated cardiomyocytes [9] In VSMCs, 2 h

of incubation with ouabain or K+-free medium led to

a 10-fold increase of immunoreactive c-Fos protein

content, followed by c-Jun expression Importantly,

accumulation of c-Fos mRNA in ouabain-treated

VSMCs correlated with increased [Na+]i and preceded

the loss of K+i[10]

It is well documented that the c-Fos promoter

contains a serum response elements (SRE) and a

Ca2++ cAMP response element (CRE) activated by

[Ca2+] elevation in the cytoplasm and nucleus,

respect-ively [11,12] (Fig 1) These data suggest that c-Fos

expression in Na+i-loaded cells might be mediated by

activation of the Na+⁄ Ca2+exchanger and an increase

in [Ca2+]i However, neither [Ca2+]i nor total

exchangeable Ca2+ content in VSMCs was augmented

by ouabain Moreover, ouabain-induced c-Fos

accu-mulation was preserved in the presence of nicardipine

as well as extracellular and intracellular Ca2+chelators [10] These data allowed us to conclude that c-Fos expression in ouabain-treated VSMCs was mediated

by a novel Na+i-sensitive, Ca2+i-independent trans-cription factor We designed this study to localize the putative Na+response element (NaRE) within the 5¢-UTR containing all known elements involved in the regulation of c-Fos expression

Results The effect of ouabain on c-Fos expression

is cell type-specific Keeping in mind that VSMCs from the rat aorta used

in our previous study [10] possess low transfection efficacy [7], we compared the action of ouabain on cul-tured cells with different origins Figure 2A shows that

5 h of inhibition of Na+⁄ K+-ATPase with ouabain led to an  10-fold elevation of intracellular exchange-able Na+in all types of cells investigated In contrast, the action of ouabain on c-Fos mRNA was cell type-specific, with the highest accumulation in HeLa and C11 Madin-Darby canine kidney (MDCK) cells and a modest rise in HIH 3T3 fibroblasts and C7-MDCK cells; no effect of ouabain on c-Fos expression was observed in H9C2 cells (Fig 2B) To search for NaRE within the 5¢-UTR c-Fos promoter, we tested HeLa cells Side-by-side with the highest increment of c-Fos expression and perfect susceptibility to transfection, the choice of HeLa cells was motivated by the exist-ence of a commercially available activation domain fusion cDNA library from HeLa cells that could be employed for the identification of NaRE-binding

-650 -348 -335 -320 -313 -297 -291 -176 -166 -97 -76 -67 -62 -59 -55 -31 +103

CArG

GGATATTACC

CCATATTAGG

-303 -312

TATA CRE

MLTF/USF GC-rich

direct repeats/

RCE

FAP Ets CArG NF-1 SIE

SRF SRF

NF-1

SP-CREB/

ATF

STAT STAT

SRE

AP-1

wt-SRE

mt-SRE

Fig 1 Structure of c-Fos promoters containing wild-type (wt) and mutated (mt) SRE STAT, signal transducers and activators of transcription (transcription factor family); SIE, sis-inducible element; Ets, E 26 domain; TCF, ternary complex factor, including Elk-1, Net, and Sap-1 tran-scription factors; SRF, serum response factor; CArG, CC-A + T-rich-GG box; AP-1, activator protein-1; FAP, fos-AP-1 binding sequence; RCE, retinoblastoma (Rb) control element; CREB, CRE-binding protein; MLTF ⁄ USF, major late transcription factor ⁄ upstream stimulating factor.

Trang 3

protein(s) involved in [Na+]i sensing, engaging the

yeast two-hybrid system

Ouabain-induced c-Fos accumulation is abolished

by inhibition of RNA synthesis

Figure 3A shows that c-Fos mRNA expression in

qui-escent HeLa cells was below the detection limit and

was time-dependently increased after 1 h of ouabain

addition The inclusion of 1 lgÆmL)1of actinomycin D

decreased RNA synthesis by 95–98% (data not

presen-ted), and completely abolished ouabain-induced c-Fos

mRNA accumulation (Fig 3B) Neither ouabain nor

actinomycin affected survival of HeLa cells, as

indica-ted by a low number of trypan blue-positive cells and

a lactate dehydrogenase (LDH) release assay (Table 1)

c-Fos expression in ouabain-treated HeLa cells

is mediated by [Na+]ielevation

Side-by-side with elevation of the [Na+]i⁄ [K+]i ratio,

interaction of ouabain and other cardiotonic steroids

with the Na+⁄ K+-ATPase a-subunit triggers diverse

Na+i-independent signals [8,13,14] Ouabain targets

other than Na+⁄ K+-ATPase also cannot be excluded

To examine these hypotheses, we adopted several approaches First, we compared the actions of ouabain

on c-Fos expression in control and K+-free media Figure 4 shows that, similarly to the effect of ouabain,

Na+⁄ K+-ATPase inhibition in K+-free media resulted

in an approximately seven-fold elevation of intracellu-lar Na+ content and a 12-fold increase of c-Fos protein Importantly, the effect of ouabain on c-Fos

-Serum - - + - - + - - + - - + - - +

A

B

0 200 400 600

0 200 400 600

0 200 400 600

0 200 400 600

0 200 400

600

ouabain control

+, nmol/mg protein

Fig 2 Effect of ouabain on intracellular exchangeable Na+(A) and c-Fos mRNA (B) in different cell types Serum-deprived cells were incuba-ted for 5 h in DMEM ± 10 l M (HeLa, C7-MDCK and C11-MDCK cells) or 3 m M (NIH 3T3 and H9C2 cells) ouabain In some of the experi-ments, 10% fetal bovine serum was added for 20 min as a positive control The means ± SE from experiments performed in triplicate are shown.

(hr) 0 0.5 1 3 6 12

A

B

Fig 3 c-Fos mRNA expression in HeLa cells (A) Kinetics of c-Fos mRNA accumulation in serum-deprived cells incubated in DMEM containing 10 l M ouabain (B) c-Fos mRNA in HeLa cells after 6 h

of incubation in DMEM ± 10 l M ouabain and 1 lgÆmL)1 actino-mycin D (Act-D).

Trang 4

expression was abolished in K+-free medium Second,

we compared the dose-dependent action of ouabain on

intracellular monovalent cation content and c-Fos

expression This experiment revealed that c-Fos

accu-mulation in ouabain-treated cells positively and

negat-ively correlated with the gain of Na+iand loss of K+i,

respectively (Fig 5) Third, we treated cells with

monensin, an ionophore providing electroneutral

Na+⁄ H+exchange At a concentration of 1 lgÆmL)1,

this compound did not affect [K+]i but increased

[Na+]i and c-Fos content two- to three-fold (Table 2)

The modest impact of monensin on [Na+]i as

com-pared to ouabain was probably caused by the negative

resting membrane potential () 50 mV) [15], which

limits the accumulation of charge-balancing anions,

such as Cl– and HCO3 Elevation of monensin

con-centration up to 10 lgÆmL)1 attenuated cell survival,

as indicated by the accumulation of trypan

blue-posit-ive cells and augmented LDH release (Table 1) Fourth, as predicted, equimolar substitution of 80% of extracellular Na+ by N-methyl-d-glucamine sharply attenuated the action of ouabain on Na+i content (Fig 4A) In this medium, ouabain increased c-Fos content only two- to three-fold (Fig 4B) Viewed col-lectively, these data strongly indicate that c-Fos expres-sion in ouabain-treated HeLa cells is caused by inhibition of Na+⁄ K+-ATPase-mediated ion fluxes and elevation of [Na+]i

Evidence of Ca2- and extracellular regulated kinase (ERK)-independent signaling

The presence of CRE in the c-Fos promoter (Fig 1) sug-gests that in cells with highly active Na+⁄ Ca2+ exchange, ouabain and other [Na+]i-raising stimuli can trigger c-Fos expression via elevation of [Ca2+]i To test this hypothesis, we treated HeLa cells with ouabain in the absence of extracellular Ca2+ and in the presence

of the intracellular Ca2+ chelator 1,2-bis(O-amino-phenoxy)ethane-N,N,N¢,N¢-tetraacetic acid (BAPTA)

As predicted, the procedure almost completely abolished

an increase of [Ca2+]i triggered by inhibition of endo-plasmic reticulum Ca2+-ATPase with thapsigargin or

by activation of Ca2+ signaling with the P2Y agonist ATP (data not shown) However, neither Ca2+-free medium nor BAPTA abolished c-Fos expression trig-gered by ouabain (Fig 6) In recent studies, we docu-mented that addition of the extracellular Ca2+chelator EGTA leads to a four-fold increase in Na+influx, prob-ably due to heightened passive permeability of the plasma membrane [16] This observation provides an

Table 1 Effect of ouabain, monensin and actinomycin D on survival

of HeLa cells Cells were incubated in DMEM with compounds

indicated in the left column for 6 h Total cell number and LDH

con-tent were taken as 100% The means ± SE from experiments

per-formed in quadruplicate are shown.

Additions

Number of trypan blue-positive cells (%)

LDH release (%)

A

K +

o , mM

Na +

o , mM

5.4 140.1

0 145.5

5.4 30.4

0 200 400 600 800 1000

+ , %

control ouabain

0 200 400 600 800 1000 1200 1400

B

5.4 140.1

0 145.5

5.4 30.4

Fig 4 Effect of 10 l M ouabain on intracellular Na+(A) and immunoreactive c-Fos (B) after 6 h of incubation of HeLa cells in control, K+-free

or Na + -depleted medium Na +

i and immunoreactive c-Fos content in control medium without ouabain was taken as 100% Means ± SE obtained from experiments performed in quadruplicate are shown Control medium contained (m M ) NaCl, 109.4; KCl, 5.4; CaCl 2 , 1.8; MgSO 4 , 0.8; NaHCO 3 , 29.8; NaH 2 PO 4 , 0.9; Hepes, 8.4; glucose, 5; and vitamins and amino acids at concentrations indicated for DMEM recipes In

K + -free medium, KCl was substituted by NaCl; in Na + -depleted medium, NaCl was substituted by N-methyl- D -glucamine.

Trang 5

explanation for the modest rise of c-Fos seen in

EGTA-treated cells in the absence of ouabain (Fig 6)

During the last decade, several research teams have

reported that, side-by-side with elevation of the

[Na+]i⁄ [K+]i ratio, exposure to ouabain results in the

transient activation of ERK1⁄ 2 via Ras ⁄ Raf-mediated

signaling [13,14,17] ERK-mediated signaling was also

demonstrated in studies of c-Fos expression triggered

by growth factors [11,12] Considering this, we

exam-ined the effect of ouabain on phosphorylated ERK1⁄ 2

content and the effect of the ERK kinase inhibitor

PD98059 on c-Fos expression evoked by ouabain

Figure 7 shows that 2 h of incubation of HeLa cells

with 3 lm ouabain did not affect ERK1⁄ 2

phosphory-lation As predicted, c-Fos expression evoked by serum was sharply attenuated in the presence of PD98059 However, this compound did not alter c-Fos expression

in ouabain-treated cells

Ouabain does not affect F-luc expression driven

by the c-Fos promoter

To examine whether or not augmented c-Fos expres-sion in ouabain-treated cells is mediated by NaRE within the 5¢-UTR containing all known transcrip-tional elements, we deployed the firefly luciferase gene (F-luc) as a reporter gene and the Renilla luciferase gene (R-luc) driven by the herpes simplex virus thymi-dine kinase promoter as a negative control Figure 8 shows that the addition of serum to F-luc- and R-luc-transfected HeLa cells augmented the F-luc⁄ R-luc ratio by three-fold, confirming the responsiveness of our construct to ‘classic stimuli’ In contrast to serum,

6 h of exposure to ouabain did not affect the F-luc⁄ R-luc ratio in HeLa cells or in C11-MDCK cells; a sharp increase of c-Fos expression was seen in the pres-ence of this compound (Figs 2–5) The lack of signifi-cant action of ouabain on the F-luc⁄ R-luc ratio was also documented in HeLa cells transfected with F-luc driven by the c-Fos promoter region from ) 1264 to

0.03 0.1 0.3 1 10

ouabain, M

A

B

+, c-Fos

20 40 60 80 100

0 200 400 600 800 1000 1200

ouabain, µM

c-Fos

Na+ i

K+ i

Fig 5 (A) Representative western blot showing the effects of ouabain and monensin on c-Fos content in HeLa cells (B) Dose-dependent effect of ouabain on intracellular Na + , K + and c-Fos content Cells were incubated for 6 h in DMEM with or without ouabain and monensin.

Na +

i , K +

i and c-Fos content in the absence of ouabain and monensin was taken as 100% The means ± SE from experiments performed in triplicate (Na+i , K+i ) or three independent experiments (c-Fos) are shown.

Table 2 Effect of monensin on intracellular Na + and K + content

and c-Fos expression in HeLa cells Cells were incubated in DMEM

with or without monensin for 6 h The means ± SE from

experi-ments performed in quadruplicate (ion content) or three

independ-ent experimindepend-ents (c-Fos expression) are shown Immunoreactive

c-Fos content in the absence of monensin was taken as 100%.

Control Monensin, 1 lgÆmL)1

Na +

i [nmolÆ(mg protein))1] 67 ± 24 201 ± 33

K+i [nmolÆ(mg protein))1] 1873 ± 102 1904 ± 211

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+ 103 (Table 3) Negative results were also obtained

with VSMCs from the rat aorta (Fig 8) expressing

Na+⁄ K+-ATPase with low affinity for cardiotonic

steroids and showing  10-fold elevation of

immuno-reactive c-Fos content after 4–6 h of incubation with

1 mm ouabain [10]

Role of SRE

Previously, we demonstrated that Na+⁄ K+-ATPase

inhibition in VSMCs did not affect luciferase

expres-sion driven by CRE, but evoked a two-fold decrease in

luciferase expression driven by SRE [10] To

investi-gate the impact of SRE on the negative results

obtained in the study of F-luc expression in

ouabain-treated cells, we explored F-luc expression driven by

the c-Fos 5¢-UTR containing mutated SRE (Fig 1)

Figure 9 shows that the F-luc⁄ R-luc ratio was

increased by three-fold in HeLa cells transfected with

F-luc driven by the mutated c-Fos promoter, and was

only slightly affected by the combined addition of epi-dermal and insulin-like growth factors This observa-tion is consistent with the sharp elevaobserva-tion of baseline expression of human c-Fos lacking SRE in stably transfected mouse NIH 3T3 cells that was insensitive

to the addition of serum [18] Similar to the situation with wild-type c-Fos, ouabain did not affect luciferase expression driven by the mutated c-Fos promoter in the absence or the presence of growth factors

Discussion Our results reveal that, similar to the situation in VSMCs [10], c-Fos accumulation in ouabain-treated HeLa cells is triggered by Na+⁄ K+-ATPase inhibi-tion and occurs via elevainhibi-tion of [Na+]i This conclu-sion is supported by several observations: (a) similar

to the effects of ouabain, massive c-Fos accumula-tion was seen under Na+⁄ K+-ATPase inhibition in

K+-free medium (Fig 4); (b) by comparing dose-dependencies of the effect of ouabain on [Na+]i,

p42~P p44~P

0 15 30 60 90 120 (min)

A

B

0 200 400 600 800 1000 1200

1400

C

control ouabain serum

control PD98059

c-Fos

-ouabain serum PD98059

-+

+

-+ -+

-+

-+ +

Fig 7 Ouabain-induced c-Fos expression in HeLa cells: role of ERK (A) ERK1 (p42) and ERK2 (p44) phosphorylation in control cells and in cells treated with 3 l M ouabain for up to 2 h (B, C) Effect of the ERK kinase inhibitor PD98059 on c-Fos expression in control cells and in cells treated for 30 min with 5% fetal bovine serum or for 6 h with 3 l M ouabain PD98059, 20 l M , was added 20 min before serum and ouabain c-Fos content in the absence of any compounds was taken as 100% The means ± SE from three inde-pendent experiments are shown.

-+

-+ +

-+

-+ -+

-+ +

+ -+ +

ouabain

CaCl2

EGTA

BAPTA

A

B

0

2

4

6

8

10

12

14

16

18

Fig 6 Effect of Ca 2+ chelators on c-Fos accumulation in

ouabain-treated HeLa cells (A) Representative western blot showing the

effect of extracellular (EGTA) and intracellular (BAPTA) Ca 2+

chela-tors on c-Fos expression in control and ouabain-treated cells (B)

Immunoreactive c-Fos content in the absence and presence of

oua-bain, EGTA and BAPTA Cells were treated with 10 l M ouabain in

control and Ca 2+ -free media for 6 h In Ca 2+ -free medium, CaCl2

was substituted with 0.1 m M EGTA For complete composition of

the DMEM-like medium, see legend to Fig 4 BAPTA-AM was

added in Ca 2+ -free medium at a concentration of 20 l M for 30 min

before ouabain c-Fos content in the absence of ouabain and Ca 2+

chelators was taken as 1.0 The means ± SE from three

independ-ent experimindepend-ents are shown.

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[K+]i and immunoreactive c-Fos content (Fig 5), we

demonstrated that c-Fos expression is correlated with

elevation of the [Na+]i⁄ [K+]i ratio; (c) both c-Fos

accumulation and Na+i elevation in ouabain-treated

cells were sharply attenuated in Na+-depleted medium

(Fig 4); and (d) c-Fos content was increased two- to

three-fold in monensin-treated HeLa cells manifesting a

three-fold elevation of [Na+]i (Table 2) Importantly,

about the same increase of [Na+]i seen in cells treated

with 0.1 lm ouabain resulted in a five- to six-fold

eleva-tion of c-Fos content (Fig 5B) It should be underlined,

however, that in contrast to the effects of ouabain, elevation of [Na+]i in monensin-treated cells was not accompanied by loss of [K+]i (Table 2) This finding allows us to speculate that high [K+]iprotects the signal transduction machinery from its activation by Na+i, probably by competing for the same binding sites within

Na+

i-sensing molecules

The presence of CRE in the c-Fos promoter (Fig 1) suggests that an increase of [Na+]i can evoke c-Fos expression via Na+⁄ Ca2+ exchange activation and [Ca2+]i elevation However, neither Ca2+-free medium nor the intracellular Ca2+ chelator BAPTA affected c-Fos expression in ouabain-treated cells (Fig 6) These results indicate that c-Fos expression is caused by activation of the Na+i-mediated, Ca2+i -independent signaling pathway It should be noted that the signaling pathways triggered by ouabain are concentration-dependent and cell type-specific Thus,

in rat cardiomyocytes, c-Fos expression triggered by a modest concentration of ouabain was completely abolished by BAPTA [19], which contrasts with the negative results obtained in BAPTA-loaded VSMCs [10] and HeLa cells (Fig 6) treated with high doses

of ouabain In rat cardiomyocytes [20–23], canine VSMCs [24] and human endothelial cells [25], ouabain

Table 3 Effect of ouabain and serum on the ratio of firefly

lucif-erase (F-luc) and Renilla luciflucif-erase (R-luc) luminescence in HeLa

cells The cells were transfected with R-luc and F-luc driven by the

c-Fos promoter region from ) 1264 to + 103 as indicated in

Experi-mental procedures Transfected cells were incubated for 6 h in

DMEM with or without 10 l M ouabain or 10% fetal bovine serum.

Means ± SE obtained from experiments performed in triplicate are

shown *P < 0.001 compared to control.

0 1 2 3 4 5

-+ + -+ +

-+ + -+ +

p<0.02 p<0.01

GF ouabain

Fig 9 Effect of serum and ouabain on the ratio of firefly luciferase (F-luc) and Renilla luciferase (R-luc) luminescence in HeLa cells Serum-starved cells, transfected with F-luc driven by the c-Fos pro-moter region from ) 650 to + 103 and containing wild-type (wt-c-Fos) (A) or mutated (mt-(wt-c-Fos) (B) SRE, were treated for 6 h

in control or K+-free medium with or without growth factors (GF, 40 ngÆmL)1 epidermal growth factor + 20 ngÆmL)1 insulin-like growth factor) and 10 l M ouabain For complete composition of the incubation medium, see the legend to Fig 3 Values of the F-luc ⁄ R-luc ratio in cells transfected with wt-c-Fos and incubated in con-trol medium without GF and ouabain were taken as 1.00 The means ± SE from experiments performed in triplicate are shown.

0

2

4

6

8

10

NS

NS

p<0.01

p<0.02

NS

p<0.01

Fig 8 Effect of ouabain and serum on the ratio of firefly luciferase

(F-luc) and Renilla luciferase (R-luc) luminescence in HeLa cells,

C11-MDCK cells and VSMCs The cells were transfected with R-luc

and F-luc driven by the c-Fos promoter region from ) 650 to + 103,

as indicated in Exeperimental procedures Transfected cells were

incubated for 6 h in DMEM with or without 10 l M (HeLa and

C11-MDCK cells) or 1000 l M (VSMCs) ouabain or 10% fetal bovine

serum (FBS) In the absence of the tested compounds, F-luc

lumin-escence in HeLa cells, C11-MDCK cells and VSMCs was

59 086 ± 5676, 9036 ± 843 and 1201 ± 148 c.p.m per well,

respectively; protein content of the cells varied in the range 120 to

142 lg per well Means ± SE obtained from experiments

per-formed in triplicate are shown NS, not significant.

Trang 8

at low concentrations transiently phosphorylated

ERK1⁄ 2 This effect was absent in rat VSMCs [6]

and HeLa cells (Fig 7A) Moreover, in contrast to

serum, the increase of c-Fos content in

ouabain-trea-ted HeLa cells was insensitive to the presence of the

ERK inhibitor PD98059 (Fig 7C) These negative

results are consistent with the lack of activation by

ouabain of ERK-sensitive transcription factors, such

as Elk-1, SRF, CREB and AP-1, documented in

transfected VSMCs [10]

To further explore the role of CRE and other known

transcriptional elements within the c-Fos promoter, we

studied the expression of F-luc driven by the c-Fos

5¢-UTR, using, as a negative control, R-luc driven by

the herpes simplex virus thymidine kinase promoter

region The lack of effect of ouabain on the F-luc⁄ R-luc

ratio in HeLa cells as well as in C11-MDCK cells and

VSMCs (Fig 8) showing more than 10-fold c-Fos

accu-mulation (Fig 1) [10] shows that [Na+]ielevation does

not affect c-Fos 5¢-UTR promoter activity

Three hypotheses can be proposed to explain the

distinct action of increased [Na+]ion c-Fos expression

and c-Fos promoter activity First, [Na+]i elevation

decreases c-Fos mRNA or protein degradation rather

than triggering de novo gene expression The first

hypothesis contradicts our results, which showed

com-plete inhibition of c-Fos mRNA accumulation in cells

treated with ouabain in the presence of actinomycin D,

a potent inhibitor of RNA synthesis (Fig 3), as well

as data obtained by run-on assays demonstrating

heightened c-Fos expression in nuclei isolated from

ouabain-treated human diploid fibroblasts [18]

Sec-ond, an increase in [Na+]i evokes c-Fos expression by

activation of NaRE located upstream or downstream

of the 5¢-UTR tested in our study (Figs 1, 8 and 9) It

should be underlined, however, that extension of the

5¢-UTR from position ) 650 to ) 1264 did not lead

to significant elevation of the F-luc⁄ R-luc ratio in

ouabain-treated cells as compared to the controls

(Table 3) The role of introns has been proven in a

transcription study of several genes, including c-Fos

[26–28], and their implication in Na+i-induced c-Fos

expression deserves further investigation Third,

increasing evidence indicates that, side-by-side with

regulation of the 5¢-UTR by transcription factors, gene

activation or silencing is under the complex control of

three-dimensional positioning of genetic materials and

chromatin in the nuclear space These data suggest

that gene silencing results in decreased chromatin

mobility and, conversely, gene activation and sustained

transcription are associated with long-range movement

of chromatin [29] Nuclease digestion assays have

documented two hypersensitive sites of c-Fos

chroma-tin architecture at positions ) 350 and ) 1900 [28] Importantly, the chromatin-mediated mechanism of gene expression does not contribute to the regulation

of L-luc transcription in cells transiently transfected with plasmid encoding the gene and employed in our experiments Keeping this in mind, the negative results obtained for ouabain’s effect on L-luc expression dri-ven by the c-Fos 5¢-UTR suggest that the activation of c-Fos transcription in ouabain-treated cells is caused

by [Na+]i-mediated reorganization of the DNA– chromatin complex This working hypothesis should

be verified in forthcoming studies

Experimental procedures c-Fos promoter design and cloning The c-Fos promoter region from ) 650 to + 103, contain-ing the major known response elements (Fig 1), was ampli-fied by PCR from human HeLa cell genomic DNA, using TCGCTAGCGTCTGCTTCCACGCTTTGCACT and ACAGATCTGCTGTGGAGCAGAGCTGGGTA primers bearing NheI and BglII restriction sites, respectively c-Fos promoter fragments were cloned into pGL3 basic vector from Promega (Madison, WI, USA), with NheI and BglII restriction enzymes and the firefly luciferase gene (F-luc) as

a reporter gene Mutation within the SRE of the ) 312 to ) 303 region (Fig 1) was introduced with the Quickchange site-directed mutagenesis kit (Stratagene, La Jolla, CA, USA), following the recommendations of the manufacturer, with the sense primer CTCCCCCCTTACACAGGATG TGGATATTACCACATCTGCGTCAGC and the corres-ponding antisense primer In additional experiments, we used the pGL3 vector containing F-luc driven by the c-Fos promoter region from) 1264 to + 103

Cell cultures HeLa cells derived from human epitheloid carcinoma and NIH 3T3 mouse fibroblasts were purchased from the Ameri-can Type Culture Collection (Rockville, MA, USA) Embry-onic rat heart-derived H9C2 myoblasts were kindly provided

by P Isenring (Laval University, Quebec, PQ, Canada) C7-MDCK and C11-MDCK cells, resembling principal and intercalated cells from the collecting ducts, were provided by

M Gekle (University of Wu¨rzburg, Germany) VSMCs were obtained by previously described explant methods [30] from the aortae of 10- to 13-week-old male Brown Norway (BN.lx) rats under Brietal anesthesia (3 mgÆkg)1) in accord-ance with the procedures outlined in the Guide for the Care and Use of Experimental Animals endorsed by the Canadian Institutes of Health Research The cells were maintained in DMEM supplemented with 2.5 gÆL)1 sodium bicarbonate,

2 gÆL)1Hepes, 100 UÆmL)1penicillin, 100 lgÆmL)1

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strepto-mycin, 25 mm glucose and 10% fetal bovine serum with

minor modifications for C7-MDCK and C11-MDCK cells

as described elsewhere [31] They were plated in Petri dishes

or 24-well plates at a density of 2–3· 103cellsÆcm)2 To

establish quiescence, the cells were incubated for 48 h before

experiments in DMEM containing 0.2% serum RNA

synthesis was measured as RNA labeling in the presence of

2 lCiÆmL)1of [3H]uridine [6]

Cell viability

Cell viability was estimated by counting colored cells after

incubation of cell suspensions with 0.2% trypan blue and

LDH release To measure LDH activity, 0.5 mL of

incuba-tion medium was mixed with the same volume of 1%

Triton X-100, and attached cells were solubilized with 0.5%

Triton X-100 Then, 300 lL of samples were transferred

into 2 mL of buffer containing 50 mm Tris⁄ HCl (pH 7.4),

50 mm KCl, 0.075 mm NADH and 1 mm sodium pyruvate

The kinetics of NADH degradation were monitored with a

SPEX FluoroMax spectrofluorometer (Jobin Yvon Inc.,

Edison, NJ, USA) at kex¼ 349 nm and kem¼ 420 nm (slits

4 and 20 nm, respectively)

Transfection and luciferase assay

Transient transfections of cells with constructs were

per-formed using LipofectAMINE-PLUS reagent (Invitrogen,

Carlsbad, CA, USA) in accordance with the manufacturer’s

instructions Briefly, cells grown in 24-well plates ( 105

per well) were incubated with DNA–liposome complexes in

serum-free and antibiotic-free DMEM for 3 h in the

pres-ence of 100 ng per well of c-Fos-pGL3b firefly luciferase

(F-luc) reporter plasmid This medium also contained

100 ng per well of pRL-TK vector with the herpes simplex

virus thymidine kinase promoter region upstream of the

Renillaluciferase (R-luc) reporter gene (Promega) We

tes-ted the construct as a control for transfection efficacy and

the possible nonspecific impact of Na+⁄ K+-ATPase

inhibi-tion on the transcripinhibi-tion⁄ translation machinery The cells

were incubated overnight in serum-deprived DMEM

sup-plemented with glutamine 2 mm, Hepes 10 mm and 0.1%

BSA, and this was followed by 6 h of incubation with the

desired media, whose compositions are indicated in the

figure legends Then, the cells were washed twice with

NaCl⁄ Pi, and lysed in Mammalian Protein extraction

rea-gent (Pierce, Rockford, IL, USA), and the lysates were

assayed for F-luc and R-luc activity in the dual-luciferase

reporter assay system from Promega

Western blotting

Cells grown in petri dishes and treated as indicated in the

figure legends were scraped with a rubber policeman,

washed with ice-cold medium C, which contained 150 mm NaCl and 10 mm Hepes⁄ Tris (pH 7.4), and centrifuged (500 g, 5 min) The resultant cell pellet was washed twice with the same medium, and lysed with buffer containing

150 mm NaCl, 25 mm Hepes⁄ Tris (pH 7.5), 0.1% SDS, 0.25% sodium deoxycholate, 2 mm EGTA, 2 mm EDTA,

1 mm Na3VO4, 10 mm NaF, 200 lm phenylmethylsulpho-nyl fluoride, 1 lgÆmL)1 leupeptin and 1 lgÆmL)1 aprotinin Equal portions of cell lysate (20 lg per lane) were electro-phoresed on 10% SDS-polyacrylamide gel, transferred to a nitrocellulose membrane, washed with NaCl⁄ Piand incuba-ted overnight at 4C with antibodies to c-Fos or p-ERK (Santa Cruz Biotechnology, Santa Cruz, CA, USA) in NaCl⁄ Pi containing 0.05% Tween-20 and 5% skimmed milk After incubation, the membranes were washed three times with NaCl⁄ Pi⁄ Tween and incubated for 1 h with horseradish peroxidase-conjugated antibody (Santa Cruz Biotechnology) The membranes were then washed with NaCl⁄ Pi⁄ Tween, and the protein bands were visualized with

an enhanced chemiluminescence detection kit (Santa Cruz Biotechnology) before exposure to X-ray film Relative pro-tein content was quantified with the nih image program

Northern blotting Total RNA from HeLa cells was isolated with TRIZOL reagent (Life Technologies, Burlington, ON, Canada) in accordance with the manufacturer’s instructions Ten micr-ograms of total RNA, measured by UV spectrophotometry, was subjected to gel electrophoresis, transferred to a Hybond N+ membrane (Amersham Pharmacia Biotech, Baie d’Urfe´, PQ, Canada), UV-immobilized and hybridized

to 32P-labeled probes c-Fos mRNA forward (AGG AATAAGATGGCTGCAGCCAAG) and reverse (GACTC TGGGGTGGTAGCCTCAG) primers, corresponding to the 569–838 region of rat c-Fos mRNA, were synthesized

by the primer-designed genefisher program The probes were purified with the Wizard PCR Preps DNA purification system from Promega, and quantified with the Low DNA Mass Ladder (Life Technologies) They were labeled with a Random primer DNA-labeling system kit (Life Technol-ogies), purified on Sephadex G-50, hybridized for 24 h, visualized on a Phosphor-Imager (Molecular Dynamics, San Diego, CA, USA) and quantified by imagequant (ver-sion 5.1) software from the same company

Intracellular exchangeable K+and Na+ These were measured as the steady-state distribution of extracellualr and intracellular 86Rb and 22Na, respectively,

as described previously in detail [1] Briefly, to establish iso-tope equilibrium, cells growing in 24-well plates were prein-cubated for 6 h in control or K+-free DMEM-like media with or without ouabain and containing 0.5 lCiÆmL)1

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RbCl or 2 lCiÆmL)1 22NaCl At the end of incubation,

the cells were transferred onto ice, washed four times with

2 mL of ice-cold medium W containing 100 mm MgCl2and

10 mm Hepes⁄ Tris buffer (pH 7.4), and lysed with 1%

SDS⁄ 4 mm EDTA The radioactivity of the incubation

medium and cell lysate was quantified, and intracellular

cation content was calculated as A⁄ am, where A was the

radioactivity of the samples (c.p.m.), a was the specific

radioactivity of 86Rb (K+) and 22Na in the medium

(c.p.m.Ænmol)1), and m was protein content

Chemicals

22

NaCl, 86RbCl, [3H]uridine and [32P]ATP[cP] were

pro-cured from Amersham Biosciences The remaining

chemi-cals were purchased from Gibco, Sigma (Oakville, ON,

Canada) and Anachemia Science (Montreal, PQ, Canada)

Statistics

The data were analyzed by Student’s t-test or the t-test for

dependent samples, as appropriate Significance was defined

as P < 0.05

Acknowledgements

This work was supported by grants from the Canadian

Institutes of Health Research and the Heart and

Stroke Foundation of Canada The technical assistance

of Monique Poirier and the editorial help of Ovid Da

Silva, Research Support Office, Research Centre and

CHUM are appreciated

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