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Báo cáo khoa học: Malonyl-CoA decarboxylase (MCD) is differentially regulated in subcellular compartments by 5¢AMP-activated protein kinase (AMPK) Studies using H9c2 cells overexpressing MCD and AMPK by adenoviral gene transfer technique potx

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Cells infected with Ad.CA-AMPK demonstrated a fourfold increase in Ad.CA-AMPK activity as compared with control cells expressing green fluorescent protein Ad.GFP.. Endogenous MCD activity

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Malonyl-CoA decarboxylase (MCD) is differentially regulated in

subcellular compartments by 5¢AMP-activated protein kinase (AMPK)

Studies using H9c2 cells overexpressing MCD and AMPK by adenoviral gene transfer technique

Nandakumar Sambandam, Michael Steinmetz, Angel Chu, Judith Y Altarejos, Jason R B Dyck

and Gary D Lopaschuk

Department of Pediatrics, Faculty of Medicine & Dentistry, University of Alberta, Edmonton, Canada

Malonyl-CoA, a potent inhibitor of carnitine pamitoyl

transferase-I (CPT-I), plays a pivotal role in fuel selection in

cardiac muscle Malonyl-CoA decarboxylase (MCD)

cata-lyzes the degradation of malonyl-CoA, removes a potent

allosteric inhibition on CPT-I and thereby increases fatty

acid oxidation in the heart Although MCDhas several Ser/

Thr phosphorylation sites, whether it is regulated by

AMP-activated protein kinase (AMPK) has been controversial

We therefore overexpressed MCD(Ad.MCD) and

consti-tutively active AMPK (Ad.CA-AMPK) in H9c2 cells, using

an adenoviral gene delivery approach in order to examine if

MCDis regulated by AMPK Cells infected with

Ad.CA-AMPK demonstrated a fourfold increase in Ad.CA-AMPK activity

as compared with control cells expressing green fluorescent

protein (Ad.GFP) MCDactivity increased 40- to 50-fold

in Ad.MCD+ Ad.GFP cells when compared with

Ad.GFP control Co-expressing AMPK with

MCDfur-ther augmented MCDexpression and activity in

Ad.MCD+ Ad.CA-AMPK cells compared with the

Ad.MCD+ Ad.GFP control Subcellular fractionation

further revealed that 54.7 kDa isoform of MCD expression was significantly higher in cytosolic fractions of Ad.MCD+ Ad.CA-AMPK cells than of the Ad.MCD+ Ad.GFP control However, the MCDactivities in cytosolic fractions were not different between the two groups Interestingly, in the mitochondrial fractions, MCDactivity significantly increased in Ad.MCD+ Ad.CA-AMPK cells when compared with Ad.MCD+ Ad.GFP cells Using phosphoserine and phosphothreonine antibodies, no phosphorylation of MCDby AMPK was observed The increase in MCDactivity in mitochondria-rich fractions of Ad.MCD+ Ad.CA-AMPK cells was accompanied by an increase in the level of the 50.7 kDa isoform of MCD protein

in the mitochondria This differential regulation of MCD expression and activity in the mitochondria by AMPK may potentially regulate malonyl-CoA levels at sites nearby CPT-I on the mitochondria

Keywords: malonyl-CoA decarboxylase; AMPK; cardiac cells

Malonyl-CoA is a potent inhibitor of carnitine palmitoyl

transferase-I (CPT-I), thereby playing a pivotal role in fuel

selection in cardiac muscle [1] CPT-I, localized on the outer

mitochondrial membrane, is the rate-limiting enzyme of

fatty acid transport into mitochondria for b-oxidation [2–4]

As b-oxidation of fatty acids contributes the majority of

energy produced by the normal aerobic heart [5,6],

malonyl-CoA has a key role in regulating cardiac energy metabolism

Tissue levels of malonyl-CoA are determined by its rate of

synthesis by acetyl-CoA carboxylase (ACC) and by its rate

of degradation by malonyl-CoA decarboxylase (MCD) [1] Various physiological and pathological conditions result

in rapid changes in malonyl-CoA levels [7–9] For instance, malonyl-CoA levels drop rapidly and dramatically during ischemia and reperfusion, which is associated with a significant increase in fatty acid oxidation [8] Similarly, rapid maturation of fatty acid oxidation in the developing heart is associated with a significant decrease in malonyl-CoA levels in the myocardium [7] While decreased synthesis

of malonyl-CoA by ACC is partly responsible for these changes in malonyl-CoA, a simultaneous degradation by MCDalso has an important role in lowering malonyl-CoA levels [10]

MCDwas originally identified in the uropygial gland of the goose [11] We also showed MCDto be highly expressed

in mammalian cardiac muscle [12], and provided evidence

to suggest that cardiac MCDplays an important role in regulating fatty acid metabolism in the heart [10,13] Regulation of MCDoccurs both at the level of transcription and post-translation [14,15] MCDhas several serine and threonine residues that can potentially be phosphorylated Previous studies in our lab and other groups have shown

Correspondence to G Lopaschuk, 423 Heritage Medical Research

Building, University of Alberta, Edmonton, Alberta T6G 2S2,

Canada Fax: + 1 780 492 9753, Tel.: + 1 780 4922170,

E-mail: gary.lopaschuk@ualberta.ca

Abbreviations: ACC, acetyl-CoA carboxylase; AICAR,

5-amino-imidazole-4-carboxamide riboside; AMPK, 5¢AMP-activated protein

kinase; CPT-I, carnitine pamitoyl transferase-I; GFP, green

fluores-cent protein; Itu, 5¢-iodotubercidin; MCD, malonyl-CoA

decarboxy-lase; moi, multiplicity of infection.

(Received 26 February 2004, revised 14 April 2004, accepted 14 May

2004)

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that MCDcan either be inhibited or activated by

phos-phorylation [16,17] One potential kinase that could control

MCDactivity is 5¢AMP-activated protein kinase (AMPK)

AMPK is a cellular fuel gauge, and acts to

simulta-neously shut down ATP consuming biosynthetic processes

and facilitate ATP producing catabolic processes during

periods of metabolic stress [18] One important stress that

can occur in the heart is ischemia AMPK is rapidly

activated during myocardial ischemia [8,19,20], leading to

rapid changes in the control of glucose and fatty acid

metabolism AMPK stimulation of fatty acid metabolism

occurs as a result of AMPK phosphorylation and inhibition

of ACC [18,20–24] This activation of AMPK and

inhibi-tion of ACC results in a dramatic drop in malonyl-CoA

levels during and following ischemia [8,20]

Alterations in myocardial malonyl-CoA levels can not be

solely explained by suppression of ACC activity unless

simultaneous degradation of malonyl-CoA is occurring It

has therefore been hypothesized that AMPK could also

play a dual role by activating MCDto facilitate

malonyl-CoA degradation [12] However, the existing literature on

MCDregulation by AMPK is inconsistent in this regard

Although we [12] and others [25] have demonstrated that

MCDis not a direct substrate for AMPK in vitro, other

studies suggest that MCDis activated by phosphorylation

by AMPK [16,17] The inconsistencies in the literature

regarding AMPK’s role on MCDregulation may be partly

due to the fact that the above studies have either used

nonspecific means to activate AMPK [16,17] or have used

in vitroconditions that do not mimic conditions seen in

the intact cell [25]

Two alternate translational start sites on MCDappear to

give rise to two isoforms of molecular weight 54.7 kDa and

50.7 kDa, respectively [11,13,26] MCD could potentially

exist in different subcellular compartments, including

cyto-plasm, peroxisome or mitochondria [27] In cardiac

myo-cytes, the majority of the MCDis the 50.7 kDa isoform,

which is primarily expressed in the mitochondria [1,28]

How compartmentalization regulates cardiac MCDactivity

is not clearly understood In the present study we examined

whether cardiac MCDis regulated by AMPK, by

co-overexpressing a constitutively active mutated form of the

catalytic subunit of AMPK and the full length human

MCDin H9c2 cells (a rat cardiac ventricular cell line) using

an adenoviral gene delivery technique As MCDis localized

in various subcellular compartments, we also examined

whether AMPK differentially regulates MCDin

mito-chondrial and cytosolic fractions of these cardiac cells

Materials and methods

H9c2 cell culture

H9c2 cells (ATCC, Rockville, MD, USA) were grown as

myoblasts to confluency in 60-mm diameter cell culture

dishes in Dulbecco’s modified Eagles’ medium (DMEM;

Sigma) containing 10% (v/v) fetal bovine serum, 1% (w/v)

PenStrep (Sigma) and 0.25 mM L-carnitine (Sigma) Dishes

were incubated in a water-jacketed CO2 incubator

main-tained at 37C with 95% O2and 5% CO2 (v/v/v) Cells

were replenished with fresh media every 48 h Cells were

seeded at approximately 4000–5000 cells per cm2 On

reaching approximately 90% confluency, myoblasts were allowed to differentiate into myotubes in DMEM contain-ing 1% (v/v) fetal bovine serum, 1% (w/v) penstrep, and 0.25 mM L-carnitine In the presence of 0.25 mM L-carnitine, full differentiation of myoblast to myotubes occurred within

7 days of adding 1% (v/v) fetal bovine serum, using peak levels of myo-d expression as a marker of muscle cell differentiation (data not shown) Passages 12–25 were used for experiments described in this study

AICAR treatment H9c2 cells were treated with 2 mM 5-aminoimidazole-4-carboxamide riboside (AICAR) for 2 h, as described previously [29] Briefly, DMEM containing 1% (v/v) fetal bovine serum was removed and cells were incubated with Krebs’ Henseleit (KH) solution (118 mM NaCl, 3.5 mM

KCl, 1.3 mMCaCl2, 1.2 mMMgSO4, 1.2 mMKH2PO4) for

20 min at 37C At the end of 20 min, fresh KH solution with or without AICAR (2.0 mMfinal concentration) was added to each dish, and cells were incubated for 2 h Some cells were also treated with the AMPK antagonist 5¢-iodotubercidin (Itu, 50 lM) for 2 h, either with or without 2.0 mMAICAR Four groups were included: (a) control, (b) AICAR treated, (c) Itu treated, and (d) Itu + AICAR treated cells At the end of the 2-h incubation, cells were rapidly lysed as described previously [29] Cell lysates were then used for measurement of AMPK activities

Construction of recombinant adenovirus encoding MCD, AMPK, and GFP and infection of H9c2 cells

To construct recombinant adenovirus, full length human MCDcDNA containing the two putative start sites [30] was subcloned into a pAdTrack-CMV shuttle vector, linearized with Pme 1 and inserted into adenovirus using pAdEasy-1 system for homologous recombination in Escherichia coli [31] The full-length hMCDwith two start sites can express two isoforms of MCD(a 50 kDa and 54.7 kDa isoforms) The longer form has a putative mitochondrial targeting sequence, as well as peroxisomal targeting sequence [32] The pAdTrack-CMV shuttle vector also contained a gene encoding enhanced green fluorescent protein (GFP) There-fore, the adenovirus used to express MCDprotein also expressed GFP, which served as a marker of successful viral infection and protein overexpression

A similar protocol was used to construct adenoviruses encoding a myc-tagged constitutively active (T172D) catalytic l1subunit (1–312 amino acid residues) of AMPK (CA-AMPKa1(312)) [33], as well as an adenovirus encoding GFP alone (used as a control)

Differentiated H9c2 cells cultured in DMEM with 1% (v/v) fetal bovine serum were infected with either five multiplicity of infection (moi) per cell of Ad.MCD, 25 moi per cell of Ad.GFP or 25 moi per cell of Ad.CA-AMPK Ad.CA-AMPK (25 moiÆcell)1) were determined to yield optimum CA-AMPKa1(312) expression and activity from series of Ad.CA-AMPK concentrations (5, 10, 25 and 50 moiÆcell)1) Some cells were double infected with Ad.MCD (5 moi) and Ad.CA-AMPK (25 moi) to study the effect

of overexpressed AMPK on overexpressed MCDacti-vity (Ad.MCD+ Ad.CA-AMPK) Cells infected with

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Ad.MCD(5 moi) and Ad.GFP (25 moi) served as the

control (Ad.MCD+ Ad.GFP) to the above group Cells

were allowed to express the proteins for 48 h and lysed

rapidly as described below

Cell lysis and sample preparation for MCD and

AMPK assays

Cells were subjected to a rapid lysis procedure to avoid

activation of endogenous AMPK, as slow lysis of cells has

been shown previously to increase cellular AMP levels [29]

Culture dishes were placed on ice, ice-cold lysis buffer was

added, cells were scraped carefully with a rubber scraper

and transferred to microfuge tubes Samples were then

immediately homogenized by ultrasonication (Sonifier,

Model W185D, Heat Systems-Ultrasonics, Inc., NY, USA)

and centrifuged at 17 000 g for 3 min [29] Supernatants

were subsequently collected and stored at )80 C For

AMPK and ACC assays, cells were lysed in buffer

containing 50 mM Tris-base, 250 mM mannitol, 1 mM

EDTA, 1 mMEGTA, 50 mMNaF, 5.0 mMNaPPi, 1 mM

dithiothreitol, mammalian protease inhibitor cocktail

(Sigma) and 1% (v/v) Triton X-100 For MCDassays,

lysis buffer containing 75 mMKCl, 20 mMsucrose, 10 mM

Hepes, 1 mM EGTA, 50 mM NaF, 5 mM NaPPi, 1 mM

dithiothreitol, and a protease inhibitor cocktail was used

Samples were subjected to ultrasonication on ice for 5 s

and whole cell lysates were used for MCDassay Protein

concentrations of the cell lysates were determined by a

Bradford protein assay kit

Subcelluar fractionation to isolate cytosol and

mitochondrial fractions

To prepare mitochondrial and cytoplasmic fractions, three

60 mm dishes were pooled Cytoplasmic fractions were

obtained by permeabilization of plasma membrane by

digitonin (30 lM) treatment for 20 min at 37C [34] Each

60 mm dish was treated with buffer containing 30 lM

digitonin, 0.15 mM MgCl2, 10 mMKCl, 10 mM Tris/HCl,

pH 6.7) Following incubation the buffer was removed, and

centrifuged at 1500 g for 5 min Supernatant was

con-centrated using Amicon Ultrafree-MCTM ultrafiltration

(30 kDa molecular mass cut-off) units, centrifuged at

5500 g for 1 h in 4C

Mitochondrial fraction was prepared from the above

digitonin permeabilized cells, as described previously [35]

Cells were quickly washed with ice-cold NaCl/Pi and

scraped into ice cold NaCl/Pi in 15 mL centrifuge tubes

Cells were pelleted by centrifuging at 1000 g for 10 min The

pellet was then re-suspended in approximately six volumes

of homogenizing buffer (0.15 mM MgCl2, 10 mM KCl,

10 mM Tris/HCl, pH 6.7), transferred to a glass-Teflon

homogenizer (Potter-Elvehjem, between 0.10 and 0.15 mm

clearance), and homogenized by 10–15 up and down strokes

while revolving at 500 r.p.m Homogenate was then

trans-ferred to a microfuge tube, and sucrose was added to the

homogenate to a final concentration of 0.25M and

dissolved The homogenate was centrifuged at 1500 g for

3 min to remove nuclei and larger fragments The

superna-tant was then centrifuged at 5000 g for 10 min to pellet

mitochondria The pellet was resuspended in 10 m

Tris-acetate (pH 6.7) buffer containing 0.15 mM MgCl2,

250 mMsucrose and re-centrifuged at 5000 g for 10 min The pellet was then suspended in 10 mM Tris-acetate (pH 7.0) buffer containing 250 mMsucrose This procedure

is known to yield a mitochondrial-rich fraction of high purity and functional integrity [36]

Voltage dependent anion-selective channel protein 1 (VDAC-1), a mitochondrial porin, was used as a marker

to check the mitochondrial fractions [37] Digitonin perme-abilization followed by mitochondrial fractionation did not affect mitochondrial integrity as determined by negligible amounts of cytochrome C released into cytosol

Western blot and SDS/PAGE for AMPK, MCD and mitochondrial markers

To identify AMPK and MCDin the samples, SDS/PAGE and Western blot analysis was peformed Thirty micrograms

of either whole cell lysates or subcellular fractions were loaded in each well of 10% SDS gel Following electrophor-esis, proteins were transferred to nitrocellulose membranes which were then blocked overnight with either 5% (w/v) bovine serum albumin (for MCD) or in 5% (w/v) skim-med milk powder (for AMPK) in NaCl/Tris For CA-AMPKa1(312) which is myc-tagged, polyclonal anti-myc (Santa Cruz Biotechnology Inc., CA, USA); and for MCD, rabbit polyclonal anti-MCD IgG [12,13] were used Enhanced chemiluminscence detection was carried out to visualize the protein bands on an autoradiograph

Western blot analyses for VDAC1, cytochrome C oxidase and ubiquinone-cytochrome C core 2 subunit of complex III were performed using respective primary antibodies (polyclonal goat anti-VDAC1, Santa Cruz Biotechnology Inc.; monoclonal mouse anti-cytochrome c, BDBiosciences Pharmingen, San Diego, CA, USA; mono-clonal mouse anti-core 2 subunit, Molecular Probes, Eugene, OR, USA)

AMPK assay Both endogeous AMPK and overexpressed

CA-AMP-Ka1(312) activities were measured as previously described [8] Samples were diluted to a concentration of 1 mgÆmL)1in re-suspension buffer containing 100 mM Tris-base, 1 mM

EDTA, 1 mMEGTA, 50 mMNaF, 5 mMNaPPi, 10% (v/v) glycerol, 1 mMdithiothreitol, 0.1% (w/v) mammalian pro-tease inhibitor cocktail and 0.12% (v/v) Triton X-100 Two microlitres of the above sample was then incubated with the synthetic 200 lM AMARA (AMARAASAAALARRR) peptide, 200 lM [32P]ATP[c-P], 0.8 mM dithiothreitol,

5 mMMgCl2, 200 lMAMP in buffer (pH 7.0) containing

40 mMHepes/NaOH, 80 mMNaCl, 8% (w/v) glycerol for

5 min at 30C (total volume 25 lL) This incubation leads to incorporation of32P into the AMARA peptide At the end of

5 min, 15 lL of the incubation mixture was blotted onto a

1 cm2phosphocellulose paper The paper was then washed three times for 10 min in 150 mMphosphoric acid followed

by a 5 min final wash in acetone The papers were then dried and counted in 4 mL of scintillation fluid (EcoLiteTM, ICN,

CA, USA) AMPK activity was expressed as picomoles of

32P incorporated into AMARA peptide per minute per milligram protein

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MCD assay

MCDactivity was determined by radiometric assay that

was slightly modified from a previously described method

[10] Acetyl-CoA, the product of malonyl-CoA degradation

by MCD, was converted to [14C]citrate by incubation with

[14C]oxaloacetate in the presence of citrate synthase

(0.73 lUÆlL)1) [14C]Oxaloactetate in turn was produced

from [U-14C]aspartate (5 lCiÆmL)1) and a-ketoglutarate

(2 mM) by transamination in the presence of glutamic

oxaloacetate transaminase One hundred microliters of

whole cell lysates or cytoplasmic and mitochondrial

frac-tions of either undiluted samples for endogenous MCDin

nonoverexpressing cells (2.0–3.0 mgÆmL)1protein

concen-tration) or 20–40 times diluted samples for cells

overex-pressing MCDwere incubated with 90 lL incubation buffer

containing phosphatase inhibitors 50 mM NaF, 5 mM

NaPPi, 1 mM dithiothreitol and 100 mM Tris-base

(pH 8.0) The timed reaction was started by adding

1.0 mM malonyl-CoA to the incubation mixture and

incubated at 37C for 20 min to allow formation of

acetyl-CoA The reaction was stopped with 40 lL of 0.5M

perchloric acid, neutralized with 10 lL of 2.2M KHCO3

(pH 10) and centrifuged at 1500 g at 4C for 5 min to

remove precipitated proteins Supernatants containing

formed acetyl-CoA were incubated with 22 lL of a mixture

of 0.01 mM dithiothreitol, 1.0 mM CuSO4, and 400 mM

potassium acetate solution, 20 lL of 60 mM EDTA and

30 lL of 30 mMN-ethylmaleimide to remove excess CoA

remaining in the later stages of the reaction so that the

citrate present could not generate non-MCDderived

acetyl-CoA The unreacted [14C]oxaloacetate was converted back

to aspartate by the addition of glutamic oxaloacetate

transaminase (0.533 lUÆlL)1) in the presence of 6.8 mM

sodium glutamate The resulting reaction mixture was then

added to 1 mL of a 1 : 1 suspension of Dowex 50 W-X8

(100–200 mesh, hydrogen form) in distilled water Dowex

binds the aspartate while leaving citrate in the supernatant

0.5 mL of supernatant was collected after centrifuging the

slurry at 1000 g for 5 min, mixed with 4 mL of scintillation

fluid (EcoLiteTM, ICN, CA, USA) and counted in a liquid

scintillation counter The radioactivity was converted to

nanomoles of acetyl-CoA formed in the reaction using a

standard curve generated from 0 to 20 nMrange of standard

acetyl-CoA which underwent similar treatment as that of

samples Preliminary experiments established that 20 min

incubation and the amount of samples used were in the

linear range of MCDenzyme activity

In vitro phosphorylation of MCD by AMPK using lysates

of cells overexpressing either MCD or CA-AMPKa1(312)

H9c2 cells overexpressing MCDwere lysed with buffer

containing 75 mM KCl, 20 mM Sucrose, 10 mM Hepes,

1 mMEGTA, 1 mMdithiothreitol, and a protease inhibitor

cocktail on ice by ultrasonication for 5 s and whole cell

lysates were used Cells overexpressing CA-AMPKa1(312)

were lysed with buffer containing 50 mMTris-base, 250 mM

mannitol, 1 mM EDTA, 1 mM EGTA, 50 mM NaF,

5.0 mM NaPPi, 1 mMdithiothreitol, mammalian protease

inhibitor cocktail (Sigma) and 1% (v/v) Triton X-100 by

ultrasonication as mentioned above Whole cell lysates of

cells overexpressing MCDwere incubated with the lysates

of cells overexpressing CA-AMPKa1(312)for 20, 30, 60, 120 and 180 min At the end of the indicated time points samples were immunoprecipitated for MCDwith rabbit polyclonal anti-MCDIgG bound to protein-A sepharose beads Immunoprecipitates were subjected to SDS/PAGE and Western blotting and probed with antiphosphoserine or antiphosphothreonine antibodies In some experiments cell extracts were incubated in the presence of 100 lCi of [32P]ATP[c-P] for the above-indicated duration followed by immunoprecipitation as above and autoradiographed for

1 week in)20 C

Statistical analysis Data are presented as means ± SEM Statistically signifi-cant differences between groups of two were assessed using the paired Students t-test A two-tailed value of P < 0.05 was considered to be significant

Results

Effect of AICAR on endogenous AMPK and MCD activities Incubation of H9c2 cells with AICAR increased AMPK activity significantly (916 ± 130 pmolÆmgÆmin)1) when compared with untreated control cells (588 ± 81 pmolÆmgÆ min)1) AICAR treatment also increased MCDactivity only modestly (to 126% of untreated controls, 1.3 ± 0.3 nmolÆmin)1Æmg)1, one tailed P < 0.05) Itu,

an inhibitor of AMPK, inhibited AMPK activity (381 ± 66 pmolÆmin)1Æmg)1) but did not affect MCD activity (1.5 ± 0.6 nmolÆmin)1Æmg)1) However, Itu did inhibit AICAR-stimulatable AMPK activity significantly (394 ± 46 pmolÆmin)1Æmg)1, P < 0.05), as well as the small increase in MCDactivity (1.9 ± 0.2 nmolÆ min)1Æmg)1 in AICAR-treated cells vs 1.3 ± 0.03 nmolÆ min)1Æmg)1in Itu + AICAR-treated cells, P < 0.05)

Endogenous MCD activity by overexpressed CA-AMPKa1(312)

Overexpression of CA-AMPKa1(312) using recombinant adenovirus (Ad.CA-AMPK) resulted in an increase in AMPK expression and activity in a concentration-depend-ent manner when compared with control cells expressing GFP (Fig 1Ai,ii) As a concentration of 25 moiÆcell)1 Ad.CA-AMPK yielded maximum activity, we used the above concentration of Ad.CA-AMPK for all further studies Control cells were infected with an equivalent amount of Ad.GFP virus per cell

Overexpression of CA-AMPKa1(312) did not increase endogenous cytoplasmic MCDactivity measured when compared with Ad.GFP cells (Fig 1Bi) In mitochondrial rich fractions, there was trend towards an increase in MCD activity in response to CA-AMPKa1(312) overexpression, which was not statistically significant when compared with Ad.GFP cells (Fig 1Bii, P < 0.07) As shown, the endogenous MCDactivities were very low and difficult to obtain a reproducible result in subcellular fractions There-fore, due to low endogenous MCDactivities in H9c2 cell fractions, we decided to increase the expression of MCDin

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these cells along with CA-AMPKa1(312)to examine the role

of AMPK in the regulation of MCD

MCD activity in H9c2 cells coinfected with Ad.CA-AMPK

and Ad.MCD

Infection of H9c2 cells with Ad.MCDresulted in a

significant increase in MCDprotein and activity when

compared with Ad.GFP cells (Fig 2Ai,ii) In order to study

the effect of AMPK on MCD, we coinfected H9c2 cells with

Ad.MCDand Ad.CA-AMPK viruses (Ad.MCD+

Ad.CA-AMPK) and compared our results to control cells

coinfected with an equivalent number of viral particles/cells

of Ad.MCDand Ad.GFP (Ad.MCD+ Ad.GFP) Our

Western blot analysis show that there was a significant

increase in both the 50.7 and 54.7 kDa isoform of MCD

protein levels in Ad.MCD+ Ad.CA-AMPK cells

com-pared with Ad.MCD+ Ad.GFP cells (Fig 2Bi–iii) The

enzyme activity of MCDshowed a trend towards increase

which was not statistically significant (from 80.7 ± 7.3

nmolÆmin)1Æmg)1 in Ad.MCD+ Ad.GFP cells to

108.5 ± 14.2 nmolÆmin)1Æmg)1 in Ad.MCD+ Ad.CA-AMPK cells, P¼ 0.058; Fig 2Biv)

MCD expression and activity in subcellular fractions

of H9c2 cells overexpressing both MCD and AMPK Previous studies have shown that MCDexists in both the cytoplasmic and mitochondrial compartments [25] Hence,

we wanted to determine if there is a differential expression and activation in various subcellular compartments We therefore isolated cytoplasmic and mitochondrial rich fractions to determine MCDdistribution and its regulation

in different compartments in response to increased AMPK activity

Mitochondrial-rich fractions showed enrichment of a mitochondrial specific protein VDAC1 that was absent in cytoplasmic fractions (Fig 3Ai) Further, most of the cytochrome C was confined to mitochondrial rich fractions and very little of cytochrome C was released into the cytoplasmic fractions (Fig 3Aii) suggesting that digitonin permeabilization resulted in a negligible damage to mito-chondria Taken together, our data suggest that the subcellular fractions were relatively pure Figure 3Aiii shows that overexpressed MCDwas present in both cytoplasmic and mitochondrial rich fractions While the majority of over expressed MCDactivity was present in mitochondria, about 30–40% of total MCDactivity was measured in cytoplasmic fractions (33 ± 18 nmolÆmin)1Æ

mg)1in cytoplasmic fractions vs 81 ± 7 nmolÆmin)1Æmg)1

in whole cell lysates) This distribution is consistent with previously published studies [1]

Cytoplasmic MCD Figure 3Bi–iv shows the effect of CA-AMPKa1(312) overexpression on cytoplasmic MCDprotein levels and activities As observed in Western blot analysis, cyto-plasmic fractions show both isoforms of MCD In Ad.MCD+ Ad.CA-AMPK cells, there was increase in MCDprotein levels (both long and short isoforms; Fig 3Bi) when compared with Ad.MCD+ Ad.GFP cells This increase was more pronounced with the long isoform

in Ad.MCD+ Ad.CA-AMPK cells (optical density 1.29 ± 0.11 AU vs 0.16 ± 0.02 AU in Ad.MCD+ Ad.GFP cells, P < 0.0001; Fig 3Bi,ii) Interestingly, the increase in short isoform of MCDprotein was not statistically significant Despite the increased expression of MCDprotein, MCDactivity in cytoplasmic fraction (normalized to milligrams of total protein) was not different between two groups (Fig 3iv)

Mitochondrial MCD MCDactivity was augmented in mitochondrial fractions obtained in response to co-overexpression of AMPK

in Ad.MCD+ Ad.CA-AMPK cells compared with Ad.MCD+ Ad.GFP cells (Fig 4Aiii) Unlike the cyto-plasmic fractions, almost all of the MCDwas the shorter form (50.7 kDa) The increase in MCD activity in the mitochondrial rich fractions was accompanied by a corres-ponding increase in MCDprotein levels (Fig 4Ai,ii,iii) Figure 4Bi,ii shows that levels of other

mitochondrial-Fig 1 AMPK overexpression by adenoviral gene transfer and

endogenous MCD activity (A) AMPK expression (i) and activity (ii) in

H9c2 cells infected with Ad.CA-AMPK or Ad.GFP Control H9c2

cells had no viral infection while Ad.GFP cells had 25 moiÆcell)1of

Ad.GFP virus As AMPK is myc tagged, anti-myc antibody was used

to probe overexpressed CA-AMPK a1(312) Western blot is a

represen-tative of n ¼ 2 experiments, AMPK activity values are average of n ¼

2 experiments (B) Endogenous MCDactivity in cytosolic (i) and

mitochondrial (ii) fractions of H9c2 cells infected with Ad.CA-AMPK

or Ad.GFP Values are mean ± SE of n ¼ 5 experiments.

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associated proteins like VDAC1 and

ubiquinone-cyto-chrome C-core 2 subunit of complex III are not affected

by increased CA-AMPKa1(312)

Discussion

Regulation of MCDby AMPK remains controversial

[16,17,25] In this study, we demonstrate that AMPK

regulates MCDby increasing levels of mitochondrial MCD

protein and activity whereas, cytoplasmic MCDprotein

levels increased without a change in enzyme activity In vitro

incubation of purified enzymes confirms that MCDmay not

be a direct substrate for AMPK [12,25] However, it cannot

be excluded that AMPK could indirectly modulate MCD activity in intact cells Stimulation of MCDactivity with AICAR in intact cells was very modest This is probably due

to the fact that AICAR stimulation of AMPK is only modest and also the level of endogenous MCDactivity was very low in H9c2 cells to see a significant change in activity

We therefore, overexpressed CA-AMPKa1(312)in H9c2 cells and examined the regulation of MCDactivity by AMPK However, low levels of endogenous MCDin H9c2 cells posed a practical problem to measure either the protein or the enzyme activity in subcellular fractions Hence, we also

Fig 2 MCD overexpression and activity in H9c2 cells co-expressing Ad.CA-AMPK or Ad.GFP (A) MCDexpression (i) and activity (ii) in H9c2 cells infected with Ad.MCDor Ad.GFP In the Western blot, lanes 1 and 2 ¼ Ad.GFP and lanes 3 and 4 ¼ Ad.MCD Western blot is a representative of n ¼ 3 experiments Activity values are means ± SE of n ¼ 5 experiments *Significantly different from Ad.GFP control,

P < 0.05 (B) MCD expression (i), optical density of 54.7 kDa isoform (ii), optical density of 50.7 kDa isoform (iii) and activity (iv) in whole cell lysates of H9c2 cells coinfected with Ad.MCD+ Ad.GFP or Ad.MCD+ Ad.CA-AMPK virus In the representative Western blot, lanes 1 and

3 ¼ Ad.MCD+ Ad.GFP and lanes 2 and 4 ¼ Ad.MCD+ Ad.CA-AMPK The relative intensity and activity values are means ± SE of n ¼ 5 experiments *Significantly different from Ad.MCD+ Ad.GFP group, P < 0.05.

Trang 7

overexpressed MCD Overexpression of CA-AMPKa1(312)

resulted in a three- to fourfold increase in AMPK protein

and activity Similarly, MCDoverexpression yielded a

several-fold increase in MCDexpression and activity When

AMPK was co-overexpressed, there was an increase in

MCDactivity in the mitochondrial fraction, which was due

to an increase in the amount of MCDlocalized to the

mitochondria On the other hand, cytoplasmic fractions

exhibited increases only in MCDprotein levels and no

change in activity compared with control conditions

In the heart, we and others [1,12] have previously

demonstrated that the majority of MCDprotein is in the

short form ( 50.7 kDa) associated with mitochondria

Whether this short form is as a result of alternate splicing at

the level of transcription or as a result of post-translational

modification of full length protein ( 54.7 kDa), is not yet known It was proposed that once MCDis targeted to mitochondria, it may lose the mitochondrial target sequence

by proteolytic cleavage and exists in the short form [38] Our data support this concept When we overexpressed human recombinant MCDin H9c2 cells both the short and the long forms of MCDwere expressed While the majority of the overexpressed MCDwas the short form and was localized

to mitochondria, the long form was expressed in Ad.MCD cells and was observed primarily in cytoplasm As mito-chondria are a rich source of MCD, it is possible that the short isoform could have leached out of mitochondria into cytoplasm during the fractionation procedures In spite of

an increased MCDprotein in the cytoplasm, the activity did not increase in response to AMPK overexpression In fact,

Fig 3 MCD expression and activity in cytosolic fractions of H9c2 cells (A) Western blots for VDAC1 (i), cytochrome C (ii) and MCD expression (iii) in cytoplasmic and mitochondrial fractions from H9c2 cells infected with Ad.GFP or Ad.MCD Western blots are representative of n ¼ 2 experiments (B) MCDexpression (i), optical density of 54.7 kDa isoform (ii), optical density of 50.7 kDa isoform (iii) and activity (iv) of cytoplasmic fractions obtained from H9c2 cells coinfected with Ad.MCD+ Ad.GFP or Ad.MCD+ Ad.CA-AMPK virus Western blot is representative of n ¼ 6 experiments and relative intensities are means ± SE of n ¼ 6 experiments Lanes 1 and 3 for Ad.MCD + Ad.GFP and lanes 2 and 4 for Ad.MCD+ Ad.AMPK cells Activity values are means ± SE of n ¼ 5 experiments *Significantly different from Ad.MCD+ Ad.GFP control, P < 0.05.

Trang 8

the specific activity per amount of protein was lower when

compared with control cells suggesting that the long

isoform, which contributes to most of the increases in

cytoplasmic MCDprotein, may be less active than the short

form Our data suggest that AMPK augments levels of both

isoforms of MCD Whether this increase in MCD

expres-sion by AMPK is a result of post-transcriptional regulation

either affecting mRNA stability or protein stability is not

known Although evidence suggests that AMPK may

regulate MCDtranscription via PGC1 and PPARa

[14,15,39,40], it may not be applicable here as MCD

overexpression per se is driven by the cytomegalo virus

promoter present in the recombinant Ad.MCDvirus

The heart predominantly expresses the 50 kDa isoform

of MCD[12] In this study, we observed that this short

isoform is mainly associated with mitochondria In this

study we demonstrated that AMPK overexpression

faci-litated an increase in the short MCDisoform in mitochondria, with a parallel increase in MCDactivity Although we did not screen for all the mitochondrial proteins, the increased CA-AMPKa1(312) activity did not affect the levels of other mitochondria-associated proteins like VDAC1 and ubiquinone–cytochrome c–core 2 sub-unit of complex III This suggests that the role of AMPK

in increasing MCDprotein and activity in the mitochondria may be selective to MCDwhen compared with the other proteins tested above

Contrary to our findings, Habinowski et al observed

no differences in MCDactivities between cytoplasmic and mitochondrial fractions [25] In their study, an islet cell line was used, where a greater expression of the longer isoform of MCDis observed Previous studies have shown that pancreatic MCDis post-translationally processed and regulated differently than either heart or muscle MCD

Fig 4 MCD expression and activity in mitochondrial fractions of H9c2 cells (A) MCDexpression (i), optical density of 50.7 kDa isoform (ii) and activity (iii) of mitochondrial fractions obtained from H9c2 cells coinfected with Ad.MCD+ Ad.GFP or Ad.MCD+ Ad.CA-AMPK virus In the Western blot, lanes 1 and 2 are for Ad.MCD+ Ad.GFP cells and lanes 3 and 4 are for Ad.MCD+ Ad.CA-AMPK cells Western blot is a representative of n ¼ 3 experiments and relative intensity values are means ± SE of n ¼ 3 experiments Activity values are means ± SE of n ¼ 5 experiments *Significantly different from Ad.MCD+ Ad.GFP control, P < 0.05 (B) Western blots for VDAC 1 protein (i) and cytochrome c Core 2 subunit of complex III (ii) in mitochondrial fractions obtained from H9c2 cells infected with Ad.MCD+ Ad.GFP or Ad.MCD+ Ad.CA-AMPK virus Lanes 1, 2, 5 and 6 represent Ad.MCD+ Ad.GFP cells and lanes 3, 4, 7 and 8 represent Ad.MCD+ Ad.CA-Ad.CA-AMPK cells Results represent n ¼ 4 different passages from each group.

Trang 9

[12,38] Pancreatic MCDappears in both longer and

shorter forms while heart and muscle show mainly the

shorter form of MCD[12,38] This greater distribution of

MCDin the cytoplasmic compartment may explain the

lack of AMPK regulation of MCDin pancreatic islets in

the above study

MCDprotein has several potential Ser/Thr sites,

phos-phorylation of which could result in either a decrease or

increase in activity [12,16,17] Previously we have shown

that dephosphorylation of MCDusing alkaline

phospha-tase increased MCDactivity suggesting that MCDis down

regulated by phosphorylation [12] However, recent studies

in skeletal muscle demonstrated that phosphorylation of

MCDincreases its activity and that dephosphorylation by

PP2A decreases or prevents the raise in MCD activity in

response to activation of AMPK [16] On the other hand

in vitro incubation of purified MCDwith heterotrimeric

AMPK holoenzyme as well as constitutively active a1

subunit found that there was no phosphorylation of MCD

[12,25] In the present study, when we incubated the lysates

from cells overexpressing MCDwith those overexpressing

CA-AMPKa1(312), we did not observe any phosphorylation

of MCD(data not shown) Also, when immunoprecipitated

MCDwas probed for the myc-AMPK by Western blot

analysis, we did not observe AMPK suggesting that there

may be no physical interaction between the two proteins

(data not shown) Taken together, this indicates that MCD

may not be a direct substrate for AMPK in vivo However,

this does not rule out that AMPK can regulate MCDvia

other intermediary protein and by other post-translational

modifications In this regard, previous studies suggested that

a 40 kDa protein that coprecipitated with MCD could be

an MCD-inhibitory protein [41]

Although this study has limitations in that (a) a

nonphysiological model system overexpressing MCDas

well as AMPK was used, and (b) a constitutively active

fragment of catalytic subunit of AMPK rather than

physiological heterotrimeric form was used, the

observa-tions are interesting and support the possibility of

differen-tial regulation of MCDin different subcellular

compartments Of particular interest, basal malonyl-CoA

levels in tissues are well above the inhibitory concentration

for CPT-1 [42], suggesting a compartmentalization of

cardiac CoA Thus, it is possible that

malonyl-CoA levels in the vicinity of CPT-I (on the outer

mito-chondrial membrane) could undergo changes sufficient

enough to either activate or inhibit CPT-I In support of

this, a recent study in human skeletal muscle observed a

moderate increase in malonyl-CoA concentrations (20% of

control) led to significant decrease in fatty acid oxidation

(41% of control) [43] Therefore, it is tempting to speculate

that an AMPK mediated increase in MCDexpression and

activity selectively in mitochondria could potentially

decrease malonyl-CoA levels sufficiently in the vicinity of

CPT-I to increase CPT-I activity This in turn would

increase fatty acid uptake and oxidation In summary, our

results demonstrate that increasing AMPK activity by

overexpression of constitutively active AMPK increases

both MCDexpression and activity Whereas cytoplasmic

MCDlevels rise without any change in activity, both

mitochondrial MCDlevels and activity increase Whether

this differential regulation of MCDby AMPK is at the

post-transcriptional or post-translational level needs further investigation

Acknowledgements

This study was funded by a grant from the Canadian Institute for Health Research N.S is a postdoctoral fellow of the Alberta Heritage Foundation for Medical Research and Heart and Stroke Foundation

of Canada J.R.B.D is a Scholar of the Alberta Heritage Foundation for Medical Research and a Canadian Institutes of Health Research New Investigator G.D.L is a Medical Scientist of the Alberta Heritage Foundation for Medical Research.

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