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phosphorylation and inhibit cardiomyocyte hypertrophy Wenqiang Liao, Shuyi Wang, Chide Han and Youyi Zhang Institute of Vascular Medicine, Peking University Third Hospital and Key Labora

Trang 1

phosphorylation and inhibit cardiomyocyte hypertrophy Wenqiang Liao, Shuyi Wang, Chide Han and Youyi Zhang

Institute of Vascular Medicine, Peking University Third Hospital and Key Laboratory of Molecular Cardiovascular Science, Ministry of Education, Beijing, PR China

14-3-3 Proteins were first discovered in 1967 as acidic

proteins found abundantly in the brain 14-3-3

Pro-teins comprise a family of highly conserved proPro-teins

having a molecular mass of  30 kDa and an

isoelec-tric point of around 5 [1] The proteins of this family

are distributed ubiquitously and have been found in all

eukaryotic organisms, ranging from yeast to mammals

Many organisms contain multiple isoforms: at least

seven isoforms (b, c, e, f, g, h⁄ s and r) exist in

mam-mals and two to 12 isoforms in yeast, fungi, and

plants In all organisms, 14-3-3 proteins form

homo-or heterodimeric structures 14-3-3 Proteins have been

shown to bind with over 200 cellular proteins It is

possible that these interactions, like many of those

shown previously, occur through the conserved amphipathic groove of 14-3-3 [1–3] 14-3-3 Proteins specifically recognize phosphoserine⁄ threonine-contain-ing sequence motifs on target proteins, such as RSXpSXP, RXSX (S⁄ T) XP or RX (Y ⁄ F) XpSXP In addition, they can bind to unphosphorylated motifs: GHSL and WLDLE [4–6]

14-3-3 Proteins have been shown to interact with an array of partners, ranging from enzymes to structural proteins Often, these proteins are important in vital cellular processes including cell cycle control and apop-tosis Through its interaction, 14-3-3 either regulate the catalytic activity of its bound enzymes, determine the subcellular localization of target proteins, or both

Keywords

14-3-3 proteins; cardiomyocyte; hypertrophy;

NFAT; PKB ⁄ GSK3b

Correspondence

Y Zhang, Institute of Vascular Medicine,

Peking University Third Hospital and Key

Laboratory of Molecular Cardiovascular

Science, Ministry of Education, Beijing

100083, PR China

Fax: +86 10 82802306

E-mail: zhangyy@bjmu.edu.cn

(Received 28 September 2004, revised 28

January 2005, accepted 14 February 2005)

doi:10.1111/j.1742-4658.2005.04614.x

14-3-3 Proteins are dimeric phophoserine-binding molecules that participate

in important cellular processes such as cell proliferation, cell-cycle control and the stress response In this work, we report that several isoforms of 14-3-3s are expressed in neonatal rat cardiomyocytes To understand their function, we utilized a general 14-3-3 peptide inhibitor, R18, to disrupt 14-3-3 functions in cardiomyocytes Cardiomyocytes infected with adeno-virus-expressing YFP-R18 (AdR18) exhibited markedly increased protein synthesis and atrial natriuretic peptide production and potentiated the responses to norepinephrine stimulation This response was blocked by the pretreatment with LY294002, a phosphoinositide 3-kinase (PI3K) inhibitor Consistent with a role of PI3K in the R18 effect, R18 induced phospho-rylation of a protein cloned from the vakt oncogene of retrovirus AKT8 (Akt – also called protein kinase B, PKB) at Ser473 and glycogen synthase 3b (GSK3b) at Ser9, but not extracellular signal-regulated kinase 1⁄ 2 (ERK1⁄ 2) AdR18-induced PKB and GSK3b phosphorylation was com-pletely blocked by LY294002 In addition, a member of the nuclear factor

of activated T cells (NFAT) family, NFAT3, was converted into faster mobility forms and translocated into the nucleus upon the treatment of AdR18 These results suggest that 14-3-3s inhibits cardiomyocytes hyper-trophy through regulation of the PI3K⁄ PKB ⁄ GSK3b and NFAT pathway

Abbreviations

a 1 -AR, a 1 -adrenergic receptor; AdR18, adenovirus expressing R18 peptide; ANP, atrial natriuretic peptide; PI3K, phosphoinositide 3-kinase; GSK3b, glycogen synthase 3b; ERK1⁄ 2, extracellular signal-regulated kinase 1 ⁄ 2; MOI, multiplicity of infection; NE, norepinephrine; NFAT, nuclear factor of activated T cells; LY, LY294002; PD, PD98059; TDT, terminal deoxynucleotidyl transferase.

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[1,7] For example, 14-3-3 inhibits ASK1 (apoptosis

signal regulating kinase-1) activity by binding to

speci-fic residues surrounding Ser967 [8,9] This interaction

also controls the subcellular distribution of ASK1

[10,11] The binding of 14-3-3 with PI3K, PKC and

Raf can either inhibit or enhance the activities of these

enzymes [12,13] 14-3-3 Proteins associate with cdc25c,

FKHRL1, HDAC5⁄ 7, NFATc, p27 and PKUa,

pre-venting their entry into the nucleus [14,15] 14-3-3

Pro-teins can also modulate protein–protein interactions

For example, 14-3-3 interacts with the

apoptosis-promoting protein BAD, preventing BAD from binding

to and inhibiting the antiapoptotic function of Bcl-XL

[16,17]

Although many 14-3-3 binding partners have been

identified, the physiological functions of 14-3-3 remain

elusive in many biological systems This is especially

true in the cardiovascular system One method to

determine the importance of 14-3-3 is to use ligand

binding-defective 14-3-3 mutants Examples of these

include dominant-negative forms of 14–3-3f and g

with the point mutation K49E and the double

muta-tion R56A and R60A [8,18] It is hypothesized that

these mutants produce a dominant negative effect by

dimerizing with endogenous 14-3-3 monomers, thereby

inhibiting the function of these proteins However, this

inhibition is partial and only disrupts a certain

iso-form-mediated processes Additionally, there are

tech-nical limitations related to the use of stable cell lines,

which place restrictions on its applicability to many

14-3-3-mediated processes

R18 is a 20-mer peptide that was isolated from

a phage display screen [19] With the core motif

WLDLE, it was found to globally inhibit

14-3-3–lig-and interactions in a specific 14-3-3–lig-and isoform-independent

manner [4,20,21] In this study, we utilized the

adeno-virus-expressing YFP-R18 (AdR18) and found that

14-3-3 can inhibit cardiomyocyte hypertrophy and

negatively modulate a1-adrenergic receptor (a1

-AR)-mediated hypertrophy The phosphoinositide 3-kinase

(PI3K)⁄ protein kinase B (PKB) ⁄ glycogen synthase 3b

(GSK3b) and nuclear factor of activated T cells

(NFAT) pathway most likely contributes to this

pro-cess

Results

Different isoforms of 14-3-3 proteins are

expressed in cardiomyocytes

To determine which isoforms of 14-3-3 exist in

cardio-myocytes, northern blot analysis was performed using

specific probes for the b, c, e, f and h⁄ s isoforms of

14-3-3 Figure 1A shows that the mRNAs for the b, c,

e and f isoforms were detected in isolated cardiomyo-cytes, but no signal of h⁄ s isoform was observed (data not shown) Furthermore, western blot analysis using antibodies specific for 14-3-3b, c, e and f confirms the expression of these isoforms in cardiomyocytes (Fig 1A)

In adult rats treated with osmotic mini-pumps for continuous norepinephrine (NE) infusion, the expres-sion of 14-3-3f protein in the heart tissue was increased one day after the NE infusion (data not shown) To identify whether the expression of 14-3-3

in isolated cardiomyocytes could be affected by activa-tion of the a1-adrenergic receptor (a1-AR), cells were treated with 10 lm NE in the presence of 10 lm pro-pranolol for indicated times Through western blot analysis, we did not find any difference in the expres-sion of 14–3-3f, b, c and e (Fig 1B)

R18 significantly potentiates NE-induced protein synthesis

To investigate the role of 14-3-3 in a1-AR induced hypertrophy of cardiomyocytes, adenovirus expressing R18 peptide (AdR18), a specific and

isoform-independ-0 1 3 6 12 24 48 time (h)

14-3-3β ζ ε γ

14-3-3 14-3-3 14-3-3

B

14-3-3 mRNA

14-3-3 protein 18sRNA

A

β γ

ε ζ

Fig 1 (A) Different isoforms of 14-3-3 s were expressed in cardio-myocytes 14-3-3f, e, c and b isoforms expressed in isolated neo-natal cardiomyocytes Cardiomyocytes cultured in 10 cm plates were serum-free for 24 h, then total RNA was extracted for northern blot analysis The whole cell lysate was harvested for western blot analysis The results were representative of four inde-pendent experiments No signal was detected for the 14-3-3h ⁄ s isoform (B) No effects of the treatment of NE on the expression

of each 14-3-3 isoform Cardiomyocytes were deprived of serum for 24 h, and incubated with propranolol (10 l M ) for 30 min, then stimulated with NE (10 l M ) for the times indicated before lysis and analysis by western blotting The experiment was repeated three times with the same result.

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ent inhibitory peptide of 14-3-3, was used A [3

H]leu-cine incorporation assay was performed to measure

protein synthesis; an important parameter of

cardio-myocyte hypertrophy Incorporation of [3H]leucine

into cardiomyocytes was increased either by treatment

with NE (expressed as the fold of control, compared

with the control, the NE treated group 1.56 ± 0.31,

P< 0.05, n¼ 5) or by infection with AdR18 (the

AdR18 group 1.51 ± 0.23 vs the Ad group

1.14 ± 0.11, P < 0.05, n¼ 5) (Fig 2A)

Infection of AdR18 in cardiomyocytes significantly

potentiated the NE-induced hypertrophy (Fig 2B)

Compared with the Ad control group, the protein

syn-thesis of the Ad + NE treatment group (expressed as

the fold of Ad control, 1.51 ± 0.31, P < 0.05, n¼ 4)

increased about 50%, and the AdR18-infected group

(1.45 ± 0.26, n¼ 4) increased about 45% However,

for the AdR18 + NE treatment group (2.41 ± 0.38,

n¼ 4), the protein synthesis increased about 150%,

which is much more than the total increment induced

by the NE or R18 treatment These results indicate

that R18 potentiated NE-induced protein synthesis in

cardiomyocytes

PI3K is critical for R18-induced protein synthesis

We next examined which signaling molecule was

responsible for the effect of 14-3-3 on protein synthesis

and on NE-induced protein synthesis in cardiomyo-cytes For these experiments, the extracellular signal-regulated kinase 1⁄ 2 (ERK1 ⁄ 2) inhibitor, PD98059 (PD), and the PI3K inhibitor, LY294002 (LY), were used Figure 2C,D shows that the R18-induced protein synthesis was blocked significantly by LY (10 lm; expressed as fold of control, the AdR18 + LY group

vs the AdR18 group, P < 0.05, n¼ 3), whereas the NE-induced protein synthesis was blocked by PD (10 lm; the NE + PD group vs the NE group,

P < 0.01, n¼ 3) The treatment with PD decreased the protein synthesis of the AdR18 + NE group [the AdR18 + NE + PD group 1.31 ± 0.09 (n¼ 3) vs the AdR18 + NE group 2.56 ± 0.47 (n¼ 5), P < 0.05] to the level of the AdR18 treatment alone (the AdR18 group 1.38 ± 0.23, n¼ 5) (Fig 2E) Further-more, the protein synthesis was markedly reduced by the LY treatment (the AdR18 + NE + LY group 0.62 ± 0.07 vs the AdR18 + NE group, n¼ 3,

P < 0.01)

R18 induces ANP expression in cardiomyocytes

in a PI3K-dependent manner One of the characteristic phenotypic changes of cardio-myocyte hypertrophy is the enhanced expression of the embryonic gene atrial natriuretic peptide (ANP) A detectable level of ANP (40.3 ± 3.2 ng mL)1, n¼ 3)

0

1

2

protein synthesis fo

*

*

A

0 1 2 3

Ad Ad +NE AdR18 AdR18+NE

protein synthesis fo

*

*

B

0 1 2

Ad AdR18 AdR18+LY AdR18+PD

protein synthesis fo

*

C

0

1

2

CON NE NE+PD NE+LY

protein synthesis fo

**

0 1 2 3

Ad AdR18 AdR18

+NE AdR18 +NE +LY

AdR18 +NE +PD

protein synthesis fo

** *

Fig 2 R18 induced protein synthesis and potentiated the NE-induced protein synthesis in cardiomyocytes in a PI3K dependent manner Car-diomyocytes cultured in 24-well plates were infected with or without AdR18 or Ad at a MOI of 10 After starvation for 24 h and treatment with propranolol (10 l M ) as well as a different inhibitor for 30 min, cells were stimulated with NE (10 l M ) for 48 h and 1 lCiÆmL)1[ 3 H]Leu was added 6 h before analysis by [3H]Leu incorporation assay (A and B) R18 induced the protein synthesis (n ¼ 5) and also potentiated the NE-induced protein synthesis (C–E) PI3K was required for the R18-induced protein synthesis, and ERK1 ⁄ 2 for the NE-induced protein syn-thesis Cardiomyocytes were treated with or without propranolol (10 l M ) plus LY294002 (LY, 10 l M ) or PD98059 (PD, 10 l M ), respectively, for 30 min and then stimulated with NE (10 l M ) for 48 h, the protein synthesis was measured (n ¼ 3) The values shown are means ± SD and expressed as the fold of control, *P < 0.05; **P < 0.01.

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was found in the culture medium of untreated myocytes.

The ANP production was increased approximately

threefold upon the treatment of NE (10 lm) in the

pres-ence of propranolol (10 lm) for 40 h (expressed as the

fold of control, 116.8 ± 6.3 ngÆmL)1 vs the control

group, P < 0.05, n¼ 3), and about fourfold in the

medium of AdR18-infected myocytes (165.6 ± 35.4

ngÆmL)1, P < 0.01 vs the Ad control group, n¼ 3),

indicating an enhanced production of ANP in these cells

(Fig 3A) Figure 3B shows that compared with the Ad

control group, the level of ANP in the AdR18 + NE

group was increased appromimately fivefold (204.8 ±

23.3 ngÆmL)1, n¼ 3), fourfold in the AdR18 group and

threefold in the Ad + NE group Compared with the

Ad + NE group, the level of ANP in the AdR18 + NE

group was increased about 1.5-fold (P < 0.05, n¼ 3),

indicating that R18 enhanced the NE-induced ANP

production

Furthermore, we determined whether PI3K was

required for R18 enhancement of ANP production; as

in protein synthesis As shown in Fig 3C–E, treatment

with LY (10 lm), but not with PD (10 lm), markedly

blocked the R18-induced ANP expression (33.6 ±

0.3 ngÆmL)1, vs the AdR18 or the AdR18 + NE

group, respectively, P < 0.05, n¼ 3), whereas the

NE-induced ANP production was blocked by PD, not

by LY (the NE + PD group 45.37 ± 12.46 ngÆmL)1

vs the NE group, P < 0.01, n¼ 3)

PKB and GSK3b phosphorylation are induced

by R18 and blocked by PI3K inhibitor Glycogen synthase kinase-3 beta (GSK3b), a down-stream signaling molecule of the PI3K⁄ PKB pathway, and ERK1⁄ 2 play very important roles in the regula-tion of hypertrophic response Phosphorylated ERK1⁄ 2 (the active form of the enzyme) positively regulates the hypertrophic response, while dephosphorylated GSK-3b (the active form of the enzyme) negatively regulates the hypertrophic response [22–25] This caused us to speculate whether these signaling mole-cules are involved in the AdR18-induced cardiomyocyte hypertrophy The effect of R18 on ERK1⁄ 2, PKB and GSK3b phosphorylation is shown in Fig 4 Activation

of cardiac a1-AR significantly increased the ERK1⁄ 2 phosphorylation compared with the control group (Fig 4A) The infection of AdR18 in cardiomyocytes had no effect on the ERK1⁄ 2 phosphorylation treated either with or without NE However, the infection of AdR18 in cardiomyocytes markedly induced the PKB and GSK3b phosphorylation Compared with the Ad control, AdR18 induced about twofold increase on the GSK3b phosphorylation (n¼ 3, P < 0.05), and activation of a1-AR with NE (in the presence of 10 lm propranolol to block beta-ARs) also induced about a twofold increase (Fig 4B), but the PKB phospho-rylation was not induced by the treatment of NE

0

2

4

6

CON NE Ad AdR18

CON NE NE+PD NE+LY

*

**

A

0 2 4 6

Ad AdR18

Ad AdR18 AdR18

AdR18+NE Ad+NE

*

B

0 2 4 6

Ad AdR18 AdR18+LY AdR18+PD

**

C

0

2

D

0 2 4 6

+NE AdR18 +NE +LY

AdR18 +NE +PD

**

E

Fig 3 R18 induced ANP expression and enhanced the NE-induced ANP expression in cardiomyocytes in a PI3K-dependent manner Cardio-myocytes cultured in 24-well plates were infected with or without AdR18 or Ad at an MOI of 10 After starvation for 24 h and treatment with propranolol (10 l M ) and different inhibitors for 30 min, cells were stimulated with NE (10 l M ) for 40 h The culture medium was collec-ted for ANP assay using an ELISA kit (A and B) R18 induced ANP production, and also enhanced the NE-induced ANP production (C–E) PI3K was responsible for the role of R18, and ERK1 ⁄ 2 responsible for the NE-induced ANP production Cardiomyocytes were treated with

or without propranolol (10 l M ) plus LY294002 (LY, 10 l M ) or PD98059 (PD, 10 l M ) for 30 min and stimulated with NE (10 l M ) for 40 h Then, the ANP production was measured The values shown were means ± SD and expressed as the fold of control The level of ANP in control was 40.25 ± 3.23 ngÆmL)1, *P < 0.05; **P < 0.01 (n ¼ 3).

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(Fig 4A) The AdR18-induced PKB and GSK3b

phosphorylation was completely blocked by the PI3K

inhibitor LY (10 lm, n¼ 3, P < 0.05, compared with

the AdR18 treatment only), but the NE-induced

GSK3b phosphorylation was not blocked by LY Taken together, these results indicate that the regu-lation of GSK3b phosphoryregu-lation is involved in R18-induced cardiomyocyte hypertrophy

R18 converts NFAT3 into faster mobility forms and induces its nuclear translocation

NFAT3, a member of the nuclear factor of activated

T cells (NFAT) family, plays a pivotal role in cardio-myocyte hypertrophy [26] It is phosphorylated by activated GSK3b (dephosphorylated form) As the infection of AdR18 induced GSK3b phosphorylation – and thus inactivation – in isolated cardiomyocytes, we hypothesized that AdR18 expression may result in the dephosphorylation of NFAT3, inducing faster gel mobility Figure 5 shows that AdR18 indeed converts NFAT3 into the faster mobility forms and this effect

is abolished by cyclosporin A (400 nm), an inhibitor of calcineurin Next, we examined the cellular localization

of NFAT3 by immunofluorescence analysis As shown

in Fig 6A, NFAT3 was present predominantly in the nucleus upon the treatment of AdR18, but was mainly found in the cytoplasm of the control and Ad group

To confirm the above results, cytoplasmic and nuclear extracts were prepared for western blot analysis with

an anti-NFAT3 Ig Clearly, the nuclear fraction of NFAT3 was increased upon the treatment with AdR18 (Fig 6B) Together, these results indicate that the localization of NFAT3 can be regulated by the treat-ment with AdR18

Discussion

14-3-3 proteins are a family of regulatory molecules that are found ubiquitously in eukaryotes Through interaction with target proteins, 14-3-3 proteins partici-pate in regulation of cell cycle, intracellular signal transduction, cytoskeletal structure and apoptosis In

A

ERK1/2

Ad AdR18

Phospho-ERK1/2

NE

Phospho-PKB PKB

LY

Phospho-PKB PKB

B

0

1

2

3

4

+NE

AdR18 AdR18 +NE

*

*

0

1

2

3

4

con AdR18 AdR18

+LY

NE NE +LY

*

Fig 4 R18 induced PKB and GSK3b phosphorylation, which was

blocked by PI3K inhibitor, LY294002 (A) Cardiomyocytes were

infected with or without AdR18 or Ad and 24 h later, the cells were

serum-starved for 24 h prior to treatment with propranolol (10 l M )

as well as LY294002 (LY, 10 l M ) for 30 min, and then treated with

or without NE (10 l M ) for 10 min Phosphorylated PKB, GSK3b and

ERK1 ⁄ 2 were detected by western blot with antibodies to

phos-pho-Ser473 PKB, phospho-Ser9 GSK-3b and phospho-ERK1 ⁄ 2 The

same membranes were stripped and re-probed with general

GSK-3b and ERK1 ⁄ 2 antibody (B) The data is means ± SD and

expressed as the fold of control, *P < 0.05 (n ¼ 3).

CON Ad AdR18 AdR18

+CysA

NFAT3

Fig 5 R18 converted NFAT3 into the faster mobility forms Neona-tal cardiac myocytes were infected with or without Ad or AdR18 in the presence or absence of cyclosporin A (Cys A, 400 n M ) for

30 min The whole cell lysate from these cells was subject to west-ern blot (6% gel) with anti-NFATc3 Ig The experiment was repea-ted three times with the same result.

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the present investigation, we have evaluated the role of

14-3-3 in cardiomyocyte hypertrophy by using an

adenovirus vector expressing the YFP-R18 fusion

pep-tide (AdR18) to inhibit 14-3-3 interactions Compared

with dominant-negative forms of 14-3-3s, the use of a

global inhibitor of 14-3-3 provides a more complete

view of the role of these proteins [20,21]

While some isoforms of 14-3-3 proteins were found

in the whole rat heart by using northern blot and

west-ern blot analysis previously [27], our results

demon-strate that 14-3-3c, e, b and f isoforms are expressed

in cultured neonatal rat cardiomyocytes R18 markedly

increased protein synthesis and ANP production and

also potentiated the a1-AR-mediated protein synthesis

and ANP production These were decreased by PI3K

inhibition, but not by ERK1⁄ 2 inhibition In addition,

R18 induced both PKB and GSK3b phosphorylation,

which was blocked completely by LY294002, whereas

NE only induced GSK3b phosphorylation, which was

not blocked by LY294002 Lisa et al have reported

that the a1-AR-induced GSK3b phosphorylation is

mediated by PKC, but not by PI3K [25] Further, we

found that NFAT3, a member of the nuclear factor

of activated T cells family, was converted into the

dephosphorylated, faster mobility forms, and

translo-cated into the nucleus upon AdR18 treatment These

results indicate that the PI3K⁄ PKB ⁄ GSK3b and

NFAT pathway is probably involved in the hyper-trophic response induced by R18

Using the R18 peptide as an inhibitor of 14-3-3, pre-vious work has shown that the R18 peptide negatively regulates early Xenopus development and induces apoptosis under some apoptotic stimulation [20,21] Using dominant-negative (DN)-14-3-3 transgenic mice

as model, Muslin et al found that transgenic mice, after transverse aortic constriction, developed signifi-cant cardiac hypertrophy and left ventricular dilation, and the survival of these mice decreased markedly [18] Until now, the effect of 14-3-3 on cardiomyocyte hypertrophy has not been reported

In this study, R18 treatment increased markedly protein synthesis and ANP production in cardio-myocytes, which was blocked by LY294002 but not

by PD98059 In addition, R18 potentiated the NE-induced protein synthesis and enhanced the NE-induced ANP production The effects of R18 on NE-induced hypertrophy were not caused by inhibiting 14-3-3 expression, because 14-3-3 protein levels were not altered upon the stimulation with NE To our sur-prise, the protein synthesis in the AdR18 + NE group was blocked by either LY294002 or PD98059 but the ANP production in this group was blocked only by LY294002 and not by PD98059 The reason for this difference was attributed to the probability that only a

Ad

CON

AdR18

A

NFAT3

cytoplasm

CON Ad AdR18 CON Ad AdR18

nucleus

B

Fig 6 R18 induces NFAT3 nuclear localiza-tion (A) Cardiomyocytes grown on glass coverslips were infected with or without AdR18 at an MOI of 10 and then starved for

24 h After fixation, the cellular localization

of NFAT3 was detected using an antibody against rabbit NFAT3 After washing in NaCl ⁄ P i , samples were incubated with Cy5-conjugated goat anti-(rabbit IgG) Ig (red) plus Hoechst 33342 (blue) and examined by con-focal microscopy NFAT3 was predominantly localized in the nucleus upon the treatment

of AdR18, whereas, in the CON and Ad group, NFAT3 was mainly localized in the cytoplasm Scale Bar, 16 lm (B) Cardio-myocytes were infected with Ad and AdR18, respectively, and then starved for

24 h Cytoplasmic and nuclear protein extra-ction were prepared and subject to western blot analysis using anti-NFAT3 Ig The experi-ment was repeated two times with the same result.

Trang 7

portion of the signaling molecules and transcription

factors modulated by 14-3-3 proteins were shared by

the processes of protein synthesis and ANP

produc-tion In addition, we found that the effect of NE on

ANP production was not blocked by LY alone, but

the combination of NE and AdR18 is inhibited by LY

to a level even greater than that of NE alone On the

other hand, PD could inhibit the effect of NE alone,

but could not affect the combination of NE and

AdR18 on the ANP production (Fig 3D,E) These

results suggest that cross talk may occur between NE

and R18 in regulation of ANP expression The

mech-anism of this cross talk remains to be clarified

One of the established roles of 14-3-3 proteins is to

inhibit apoptosis The disruption of 14-3-3 interactions

has been shown to lower the apoptotic threshold of

cells Interestingly, we found that R18 induced

cardio-myocyte hypertrophy, and the phosphorylation of

GSK3b on Ser9 was involved in this hypertrophic

response Similarly, a previous study has revealed that

the activation of the Fas receptor, another molecule

related to apoptosis, could induce cardiomyocyte

hypertrophy, which also was dependent on the

inacti-vation of GSK3b by Ser9 phosphorylation [28]

GSK3b is an established target of the PI3K⁄ PKB

signaling pathway, where PKB phosphorylates and

thereby inactivates GSK3b Phosphorylation and

inacti-vation of GSK3b, a negative regulator of cardiomyocyte

hypertrophy, has been identified to be necessary and

suf-ficient for the hypertrophy induced by hypertrophic

stimuli [25,29] GSK3b phosphorylated various cellular

substrates, including glycogen synthase, cyclin D1,

c-Jun, and NFAT Phosphorylation of cellular

sub-strates by GSK3b either directly suppressed enzyme

activities or changed subcellular localizations [30]

NFAT3 plays a crucial role in cardiomyocyte

hypertro-phy NFAT phosphorylation by GSK3b leads to NFAT

interaction with 14-3-3 proteins, causing the

redistribu-tion of NFAT from the nucleus to the cytoplasm This

results in the subsequent inhibition of NFAT-mediated

transcription [26,31] In our study, we found that R18

could convert NFAT3 into the faster mobility forms

(unphosphorylated NFAT) Cyclosporin A, an inhibitor

of calcineurin, abolished this effect of AdR18 on

NFAT3 In addition, R18 could induce the nuclear

localization of NFAT3 Therefore, the R18-induced

hypertrophy is probably caused by one or all of the

fol-lowing mechanisms: (a) R18 removes the negative

con-straint of GSK3b on NFAT; (b) R18 disrupts the

NFAT)14-3-3 interaction and inhibits the protective

role of 14-3-3 on phosphorylated NFAT; (c) R18

pre-vents NFAT translocation from nucleus to cytoplasm

Figure 7 shows a working model depicting the effects of

14-3-3 on these molecules In this model, NFAT is a pivotal molecule and R18 disrupts the balance between the unphosphorylated and phosphorylated forms of NFAT However, it is probable that R18 induced cardio-myocyte hypertrophy involves disruption of 14-3-3 inter-action with other binding proteins such as PI3K As R18 inhibits 14-3-3 proteins in an isoform-independent manner, the role of each isoform of 14-3-3 in cardio-myocyte hypertrophy remains to be elucidated

In summary, our findings establish that several iso-forms of 14-3-3 proteins (c, e, b and f) are expressed

in rat cardiomyocytes We have also shown that 14-3-3 inhibits cardiomyocyte hypertrophic responses and negatively regulates the a1-AR-induced hypertrophy, in which the PI3K⁄ PKB ⁄ GSK3b and NFAT pathway is likely involved The regulation of GSK3b phosphoryla-tion and the compartmentaphosphoryla-tion of NFAT by 14-3-3 probably contributes to this process

Experimental procedures

Materials The ERK1⁄ 2 inhibitor (PD98059), PI3K inhibitor (LY294002), propranolol and norepinephrine (NE) were

Hypertrophic stimuli

1 -AR NE

Cytoplasm

NFAT Nucleus

PKC

Hypertrophy

14-3-3

calcineurin

Cys A

PKB

-ser-9-P GSK3

PI3K

P NFAT

14-3 P NFAT GSK3

Hypertrophic stimuli

1 -AR

NE α1-AR NE

Cytoplasm

NFAT Nucleus

PKC

Hypertrophy

14-3-3

calcineurin

Cys A

PKB

-ser-9-P

Active Inactive

GSK3β

PI3K

P NFAT P NFAT

14-3

14-3 P NFAT P NFAT GSK3 β

Fig 7 A working model depicts 14-3-3 proteins inhibiting the cardio-myocyte hypertrophy Upon stimulation, PKB is phosphorylated via activated PI3K and GSK3b is phosphorylated via both PKC and PI3K, leading to GSK3b inhibition The active, dephosphorylated GSK3b phosphorylates NFAT and counteractes the effect of calcineurin on NFAT 14-3-3 Proteins inhibit PI3K and activate GSK3b, keeping NFAT in cytoplasm by binding to phosphorylated NFAT R18 induces cardiomyocyte hypertrophy in part by removal of the modulatory effect of 14-3-3 on PI3K, GSK3b, and NFAT, leading to transcrip-tional activation of NFAT in nucleus NE, norepinephrine; Cys A, cyclosporin A; PI3K, phosphoinositide 3-kinase; NFAT, nuclear factor

of activated T cells PKB, protein kinase B.

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purchased from Sigma Chemical Co (St Louis, MO, USA).

Terminal deoxynucleotidyl transferase (TDT) was from

Invitrogen Corporation (Carlsbad, CA, USA) [3H]Leucine

was from Amersham Biosciences (Little Chalfont, Bucks,

UK) Other reagents were obtained from commercial

sup-pliers

Isolation and culture of neonatal ventricular

myocytes

Procedures with experimental animals followed the National

Institute of Environmental Health Sciences Animal and

Use Committee guidelines Primary cultures of

cardio-myocytes were prepared from the ventricles of 1-day-old

Sprague–Dawley rats (from the experiment animal

depart-ment of the Medical Science Center, Peking University,

Beijing, China) by enzymatic digestion in 0.1% trypsin,

0.03% collagenase II as described previously [32] Neonatal

rats were put into a glass beaker containing a cotton mass

wetted with ethyl ether After anaesthesia and decapitation,

hearts were taken out immediately and put into ice-cold

NaCl/Pi, and then cut into pieces Cells in suspension were

collected after several rounds of digestion of heart pieces,

then divided into several 100-mm culture dishes and

incuba-ted for 1 h The suspension containing unattached

cardio-myocytes was then collected and seeded at a density of

1.5· 105cellsÆcm)2 in culture media (Dulbecco’s modified

Eagle’s medium with 10% fetal bovine serum, 0.1 mm

5-bromodeoxyuridine, 50 lgÆmL)1 penicillin and 50 lgÆ

mL)1streptomycin) After incubation at 37C in humid air

with 5% (v⁄ v) CO2for 24 h, the cardiomyocytes were then

deprived of serum and incubated for another 24 h before

treatment Cells were preincubated with 10 lm propranolol

to block b-adrenergic receptors with or without different

inhibitors for 30 min before stimulation with 10 lm NE

Recombinant adenovirus vectors

The plasmid containing R18 peptide, pAAV-EYFP-R18 was

made by subcloning the  100 bp NheI ⁄ XhoI fragment of

pSCM-136 plasmid into the 4.5 kbp XbaI ⁄ XhoI fragment of

pAAV-MCS (Stratgene, Heidelberg, Germany), and the

pAAV-EYFP was made by subcloning the 800 bp NheI ⁄

Hin-dIII fragment of pEYFP-C1 into the 4.5 kbp XbaI ⁄ HindIII

fragment of pAAV-MCS The adenovirus shuttle constructs

pAdTrack-EYFP-R18 and pAdTrack-EYFP were made by

subcloning the BamHI⁄ XhoI fragments of pAAV-EYFP-R18

and pAAV-EYFP, respectively, into

pAdTrack-cytomegalo-virus (CMV) digested with BglII⁄ XhoI Recombinant

adeno-viruses expressing EYFP-R18 (AdR18) or EYFP (Ad, as a

control) were constructed using a method described

previ-ously [33] Briefly, shuttle construct was linearized with PmeI

and electroporated into Escherichia coli BJ5183 (ATCC,

Manassas, VA, USA) together with the adenoviral backbone

plasmid pAdEasy-1 Homologous recombinants were selected

and were identified by restriction analysis Finally, the PacI-linearized recombinant was transfected into HEK293A (ATCC) packaging cells The adenoviruses produced were used to infect additional HEK293A cells, and a high titer adenovirus stock was made following several rounds of amplification All recombinant adenoviruses were tested for transgene expression in cardiac myocytes by reverse transcriptase-polymerase chain reaction and western blot Cardiomyocytes were infected with AdR18 or Ad at a multi-plicity of infection (MOI) of 10 for 24 h and then subjected

to experiments after deprived of serum for 24 h

Northern blot analysis The total cellular RNA was extracted from cardiomyocytes using a total RNA isolation system kit (Promega Corp., Madison, WI USA) The total RNA (15 lg) was separated

on a horizontal 1.0% agarose⁄ 2.2 m formaldehyde gel and transferred onto a nylon membrane (Millipore Corp., Bill-erica, MA, USA) The membrane was then hybridized with probe at 42C overnight, washed and autoradiographed [34] The synthesized 45-mer oligonucleotide probes were labeled using terminal deoxynucleotidyl transferase with [32P]dATP[aP] The sequences of probes are as follows: 14-3-3f probe: 5¢-TGAGTGTAGTCTGTGTGGGTACTG TAAGGCTTGGAGCACTTGTGA-3¢; 14-3-3h probe: 5¢-TC CTCTAGCAAGGAAGCCCATTCATGTGTATGGGGTC AACTGTTT-3¢; 14-3-3b probe: 5¢-GTCTATTGAGCTCT GTGATCTGTTTGGTGTCACTGTATCCTCCAC-3¢; 14-3-3c probe: 5¢-CAGGTGGACTGGCAGCGCACGCTGATGC TACTACTGCAGTCTTTA-3¢; 14-3-3e probe: 5¢-ACCTAA AGCTGGGACCAGTAAAATCCACAGAAATTCACTCT TGCC-3¢; 18sRNA probe: 5¢-ACGGATTCTGATCGTCTT CGAACC-3¢

Western blot analysis Cells seeded on 30-mm plates were washed once with ice-cold NaCl⁄ Piat the appropriate time after treatment, and lysed in 0.15 mL lysis buffer [20 mm Tris⁄ HCl, pH 7.4,

100 mm NaCl, 10 mm sodium pyrophosphate, 5 mm EDTA, 50 mm NaF, 1 mm sodium vandate, 0.1% (w⁄ v) SDS, 10% (w⁄ v) glycerol, 1% (v ⁄ v) Triton X-100, 1% (w⁄ v) sodium deoxycholate] containing 1 lm leupeptin, 0.1 lm aprotinin, 1 mm phenylmethanesulfonyl fluoride and

1 lm pepstatin Protein concentration was calculated using the BCA protein assay kit (Pierce Biotechnology, Inc., Rockford, IL, USA) Protein was loaded onto a 10% SDS⁄ polyacrylamide gel and electrophoretically transferred

to nitrocellulose membranes (Pall Corporation, East Hill,

NY, USA), analyzed with antibodies according to the supplier’s protocol, and visualized with peroxidase and

an enhanced-chemiluminescence system (ECL kit, Pierce Biotechnology, Inc.) The following antibodies were used

in this study: anti-14-3-3b, anti-14-3-3c, anti-14-3-3e,

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anti-14-3-3f, anti-eIF-5, anti-GSK3b and anti-NFATc3

(1 : 1000 dilution, Santa Cruz Biotechnology, Inc., Santa

Cruz, CA, USA), and anti-ERK1⁄ 2 (1 : 2000 dilution,

Upstate Biotechnology, Charlottesville, VA, USA),

anti-PKB, anti-(Ser473-phospho-PKB),

anti-(Ser9-phospho-GSK3b), anti-(Thr202⁄ Tyr204-phospho-ERK1 ⁄ 2) Igs (1 : 1000

dilution, Cell Signaling Technology, Inc., Beverly, MA, USA)

Immunofluorescence and confocal microscopic

assay

Cardiomyocytes grown on glass coverslips in six-well dishes

were infected with or without AdR18 for about 24 h and

then starved for 24 h After washing with 37C NaCl ⁄ Pi,

cells were fixed with 4% paraformaldehyde, permeabilized

with 0.2% Triton X-100, and incubated with an

anti-NFAT3 Ig (1 : 250) at 4C overnight, and Cy5-conjugated

AffiniPure Goat anti-(rabbit IgG) Ig (Jackson

Immuno-Research, West Grove, PA, USA) (1 : 500) at 37C for 1 h

Cells were counterstained with 5 lgÆmL)1 Hoechst 33342

(Sigma-Aldrich) to visualize the nucleus Microscopic images

were acquired using a Leica Confocal Microscope

Cytoplasmic and nuclear protein extract

preparation

Cardiomyocytes cultured in 10-cm plates were infected with

Ad and AdR18, respectively, at an MOI of 10, and then

starved for 24 h Cytoplasmic and nuclear protein

extrac-tions were prepared according to the instrucextrac-tions of

NE-PER Nuclear and Cytoplasmic Extraction Reagents kit

(Pierce Biotechnology, Inc.) Briefly, cells were washed

twice with ice-cold NaCl⁄ Pi, recovered by scraping, then

pelleted and resuspended in 0.2 mL ice-cold CER I

contain-ing protease inhibitors (Halt Protease Inhibitor Cocktail

Kit, Pierce Biotechnology) Cells were broken by vortexing

vigorously and then adding 11 lL ice-cold CER II and

vortexed vigorously again After centrifugation (5 min at

16 000 g, 4 C), the supernatant (cytoplasmic extract) was

collected and the insoluble fraction containing nuclei was

resuspended in 0.1 mL ice-cold NER containing protease

inhibitors After four rounds of vortexing (15 s) and

incu-bating on ice (10 min), then centrifuging for 10 min at

 16 000 g, 4 C, the supernatant (nuclear extract) fraction

was collected After protein quantification, cytoplasmic and

nuclear proteins (30 lg) were electrophoresed on an 8%

SDS⁄ polyacrylamide gel, transferred to nitrocellulose, and

immunoblotted as described above

Atrial natriuretic peptide (ANP) enzyme-linked

immunosorbent assay

Cardiomyocytes cultured in 24-well plates were

preincu-bated with different inhibitors for 30 min and treated with

NE in serum-free medium for 40 h The supernatants were collected for the ANP assay using an ELISA kit (Phoenix Pharmaceuticals Inc., Belmont, CA, USA) following the manufacturer’s instruction

Protein synthesis assay ([3H]leucine incorporation)

Cardiomyocytes cultured in 24-well plates were serum deprived for 24 h, pretreated with or without a variety of inhibitory agents, and then incubated for 48 h with NE in serum-free medium [3H]leucine (1 lCiÆmL)1) was added 6 h before the harvest At the end of the incubation, the plates were quickly washed twice with ice-cold NaCl⁄ Pi, kept for

30 min with ice-cold 10% (v⁄ v) trichloroacetic acid at 4 C, and washed with NaCl⁄ Pi Precipitates were solubilized in 0.1 m NaOH with gentle shaking at 37C for 1 h The radioactivity incorporated into trichloroacetic acid-precipita-ble materials was determined by liquid scintillation spectro-metry (Beckman Coulter Inc., Fullerton, CA, USA)

Statistical analysis All data represent the mean ± SD of at least three inde-pendent experiments The analysis of variance (anova) was performed for the comparison of three or more groups and the post-test comparison was performed by the method of Tukey A value of P < 0.05 was accepted as significant

Acknowledgements

The authors wish to thank Prof Haian Fu (Pharmacol-ogy Department at Emory University, USA) for the generous gift of pSCM136 and pEYFP-C1 plasmids and Lisa M Cockrell (Emory University) for critical reading

of the manuscript This work was supported by grants from the foundation of national key basic research and development project (G2000056906) and national nat-ural science foundation (30270540, 30200321)

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