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Tiêu đề Leptin protects H9c2 rat cardiomyocytes from H2O2-induced apoptosis
Tác giả Megumi Eguchi, Yuantao Liu, Eyun-Jung Shin, Gary Sweeney
Trường học York University
Chuyên ngành Biology
Thể loại Article
Năm xuất bản 2008
Thành phố Toronto
Định dạng
Số trang 9
Dung lượng 706,3 KB

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Exposing H9c2 cells to H2O2 decreased cell viability, and this was attenuated by pretreating cells with leptin for 1 h, but not 24 h.. Further investigation of underlying mechanisms of l

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H2O2-induced apoptosis

Megumi Eguchi*, Yuantao Liu*, Eyun-Jung Shin and Gary Sweeney

Department of Biology, York University, Toronto, Canada

The rapid increase in the prevalence of obesity to

epi-demic proportions is a serious concern, as obesity is

associated with the development of many complications

including type 2 diabetes, hypertension and heart failure

[1] Heart failure is a leading cause of mortality in

indus-trialized countries, and is accompanied by progressive

left ventricular remodeling characterized by

hypertro-phy of the myocytes, impaired vascularization in the

heart, abnormal extracellular matrix composition

(fibro-sis) and elevated cardiomyocyte cell death [2] However,

in addition to increasing the risk for initial myocardial

infarction, obesity may confer protective effects that

limit cardiac remodeling post-infarction, the so-called

obesity paradox [3] Necrosis was initially viewed as the

major pathway by which cardiomyocytes are lost during

remodeling; however, research in the past 10–15 years

has indicated that apoptosis has important

pathophysio-logical consequences in the development and progres-sion of heart failure [4,5] Indeed, the apoptotic rate is significantly increased (from 0.001% to 0.08%) in the failing heart [2]

Adipokines, collectively referring to factors derived from adipose tissue, have attracted tremendous research interest in recent years as an important mech-anistic link between obesity and various associated complications [6] The circulating adipokine profile is altered in obese individuals, and it is now clear that development of heart failure can be directly influenced

by adipokines [1] Leptin is the product of the obese (ob) gene, and its main function is to control appetite and energy expenditure by acting on the hypothalamus [7] There is a positive correlation between circulating leptin concentration and the body mass of an indiv-idual This suggests the existence of leptin resistance in

Keywords

apoptosis; caspase; heart failure; leptin;

mitochondria

Correspondence

G Sweeney, Department of Biology, York

University, Toronto, M3J 1P3 Canada

Fax: +1 416 736 5698

Tel: +1 416 736 2100 ext 66635

E-mail: gsweeney@yorku.ca

*These authors contributed equally to this

work

(Received 23 January 2008, revised 25

March 2008, accepted 14 April 2008)

doi:10.1111/j.1742-4658.2008.06465.x

Obesity is a known risk factor for induction of myocardial infarction, but, paradoxically, may also confer a protective effect against subsequent remodeling leading to heart failure In this study, we investigated the effect

of leptin, the product of the obese (ob) gene, on cardiomyocyte apoptosis,

a well-characterized component of cardiac remodeling after myocardial infarction Exposing H9c2 cells to H2O2 decreased cell viability, and this was attenuated by pretreating cells with leptin for 1 h, but not 24 h Leptin also attenuated the ability of H2O2to increase phosphatidylserine exposure and annexin V binding Further investigation of underlying mechanisms of leptin’s protective effect demonstrated that the H2O2-induced decrease in mitochondrial membrane potential (Y) leading to cytochrome c release was attenuated by leptin pretreatment, and this was associated with reduced translocation of the pro-apoptotic Bax protein to the mitochondrial mem-brane Finally, leptin prevented H2O2-induced increases in caspase-3 cleav-age and activity, although again 24 h leptin pretreatment did not confer significant protection In summary, we have demonstrated that acute leptin pretreatment mediates anti-apoptotic effects in H9c2 rat cardiomyocytes, which may be of significance in clarifying the direct impact of leptin on the heart

Abbreviations

JC-1, 5,5¢,6,6¢-tetrachloro-1,1¢,3,3¢-tetraethylbenzimidazoyl carbocyanide iodide; MTT, 3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyl-tetrazolium bromide; PS, phosphatidylserine.

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the hypothalamus of such individuals; however,

whether the heart is leptin-resistant is still controversial

[8,9] Leptin’s action is mediated by six isoforms of

leptin receptors [10] These receptors can be classified

as secreted (Ob-Re), short (Ob-Ra, c, d and f) and

long (Ob-Rb) forms The adult heart has been shown

to express both long and short ObR isoforms, but

pre-dominantly short forms of the receptor [11], and it has

also been shown that the heart is a site of leptin

production [12] The local expression of leptin and

its receptors in the heart further suggests that leptin

can potentially affect cardiac function by directly

acting on the heart, and this has been confirmed by

several recent studies [13–15]

Exposure of cardiomyocytes to H2O2and other

reac-tive oxygen species is increased in the heart, especially

after short ischemia⁄ reperfusion, and excessive

oxida-tive stress contributes to the pathogenesis of heart

fail-ure [16] A high circulating leptin concentration is seen

in the majority of obese individuals In this study, we

have investigated the effects of leptin on H2O2-induced

cell death in H9c2 cells, the most appropriate in vitro

model of cardiomyocytes currently available This

was accomplished by analyses of apoptotis

[3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyl-tetrazolium bromide

(MTT) assay and annexin V binding], together with

investigation of the mechanistic role played by the

intrinsic pathway of apoptosis (change in

mitochon-drial membrane potential (Y), cytochrome c release

and caspase-3 activity)

Results

Leptin treatment for 1 h but not 24 h protects

H9c2 cells from H2O2-induced decreases in cell

viability

The effect of H2O2 treatment on the cell viability of

H9c2 cells was measured by the uptake and reduction

of MTT to an insoluble formazan dye H2O2treatment

for 5 h significantly reduced the cell viability as

expected, and this effect was attenuated upon 1 h

pre-incubation with 6 nm leptin but not 24 h

pre-incuba-tion (Fig 1) The dose of leptin was chosen based on

preliminary experiments, previous work by ourselves

and others in vitro [17,18], and because it is relevant to

the circulating levels observed in obesity [19]

H2O2-induced phosphatidylserine exposure is

decreased by leptin treatment

Appearance of phosphatidylserine (PS) in the outer

leaflet of the phospholipid bilayer without disrupted

integrity of the membrane is one of the earliest char-acteristics of apoptotic cells In order to study the effect of leptin on H2O2-induced PS exposure, cells were incubated with appropriate treatments as indi-cated, and analyzed for the degree of annexin V binding to the surface of intact cells (Fig 2A,B) Cells were counterstained with propidium iodide to allow distinction between apoptosis and necrosis Leptin treatment alone did not affect PS exposure, but an increase in annexin V binding was observed after as little as 2 h H2O2 treatment No increase in propidium iodide staining was apparent under these conditions, but was seen in positive control experi-ments (data not shown), indicating that the cell death was predominantly due to apoptosis Quanti-tative assessment of fluorescence (Fig 2C) showed that 1 h leptin pretreatment significantly attenuated the level of annexin V binding detected in response

to H2O2 Although apparently decreasing the effects

of H2O2, 24 h leptin pretreatment did not have a significant effect

Leptin pretreatment attenuates H2O2-induced loss of mitochondrial membrane potential The mitochondrial membrane potential (Y) is a critical factor in maintaining the integrity of mitochondria and subsequent regulation of apoptosis Loss of mito-chondrial membrane potential will lead to release of the cytochrome c from mitochondria, which in turn

Leptin (h)

0 0.2 0.4 0.6 0.8 1 1.2

*

Fig 1 Leptin pretreatment for 1 h but not 24 h attenuates the abil-ity of H 2 O 2 to decrease cell viability H9c2 cells were treated with

or without 6 n M leptin for 1 h or 24 h prior to exposure to H 2 O 2 (400 l M ) for 5 h, and cell viability was measured using the MTT assay Data represent mean ± SEM (n = 4) The asterisk indicates

a statistically significant difference from H 2 O 2 treatment alone (P < 0.05).

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activates downstream caspases to cause apoptosis

[20,21]

5,5¢,6,6¢-tetrachloro-1,1¢,3,3¢-tetraethylbenzimi-dazoyl carbocyanide iodide (JC-1) accumulates as

aggregates in the normal hyperpolarized mitochondria,

resulting in red fluorescence, but JC-1 exists in the

monomeric form in apoptotic cells and stains cells

green Here we observed that untreated control cells

exhibit numerous brightly stained mitochondria that

emit red fluorescence (Fig 3) Cells treated with H2O2

exhibited fewer red JC-1 aggregates, and more green

fluorescence of monomers appeared in the cytoplasm,

indicating dissipation of the mitochondrial membrane

potential Leptin pretreatment attenuated these H2O2

-induced changes (Fig 3)

Leptin pretreatment reduces cytochrome

c release from mitochondria

Release of cytochrome c from mitochondria is a

criti-cal step in progression of the intrinsic apoptotic

path-way [20,21] H2O2 treatment for 2 h increased the

release of cytochrome c from mitochondria, as can be

seen by the loss of co-localization of cytochrome c and mitochondria (Fig 4) The effect of H2O2 was again attenuated by preincubation with leptin for 1 h (Fig 4) Co-localization was unaffected in cells treated with leptin alone

The mechanism whereby leptin attenuates the intrinsic pathway of apoptosis involves reduced Bax integration in the mitochondrial membrane

To assess translocation of the apoptotic Bax pro-tein to the mitochondrial membrane, we utilized an approach exploiting the observation that the N-termi-nal domain is only exposed and recognized by a spe-cific antibody when this protein translocates and integrates into the membrane [22] In viable control cells, or those treated with leptin, little or no Bax immunofluorescence was observed (Fig 5) However, when cells were exposed to H2O2, we observed pro-nounced staining for Bax, with a maximal effect after

4 h, and this was clearly attenuated in cells pretreated with leptin for 1 h (Fig 5)

A

B

C

Fig 2 H2O2-induced annexin V binding to the cell surface decreases with leptin pretreatment Phosphatidylserine externali-zation was assessed via annexin V binding

in the absence (A) or presence (B) of 2 h

H 2 O 2 (400 l M ) treatment with or without leptin pretreatment (6 n M , 1 h or 24 h) Cells were treated to allow detection of both ann-exin V (green) and propidium iodide (red), and images representative of those obtained for at least eight independent experiments are shown for each condition The results from all experiments (n > 3) were quanti-fied, and (C) shows the mean fluorescence (±SEM) The asterisk indicates a significant difference compared with H 2 O 2 alone (P < 0.05).

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H2O2-induced increases in caspase-3 cleavage

and activity are attenuated by leptin

pretreatment

Caspase-3 is an executioner of apoptosis, and is

involved in many important events that lead to the

completion of apoptosis [23] Cleavage of caspase-3 is

indicative of activation, and in cells treated with leptin

alone there was no change in the cleavage of caspase-3

compared to control H2O2 treatment increased

gener-ation of the cleaved form of caspase-3, and this was

attenuated by 1 h leptin pretreatment (Fig 6A) The

levels of cleaved caspase-3 correlated well with

enzy-matic activity, which was increased 1.8-fold compared

to control upon H2O2 treatment This effect of H2O2

was again significantly reduced by leptin 1 h

pretreat-ment, but not significantly by 24 h pretreatment

(Fig 6B) In order to determine the functional

conse-quences of the above findings, we examined whether

the protective effect of leptin on cell viability was

observed after a prolonged time period subsequent to

H2O2 exposure When the number of living cells, as

determined by trypan blue exclusion, was counted

three days after exposure to H2O2, over 2.2-fold more

cells were viable when pretreated with leptin for 1 h as

opposed to exposure to H2O2alone (data not shown)

Discussion

There has been great interest in the relationship between circulating leptin levels and the development

of cardiovascular diseases, but the precise role of leptin

is still controversial [24] Hyperleptinemia, which is commonly seen in obese individuals, has been pro-posed to play a role in the development of various car-diovascular diseases [25,26] Heart failure is a common end-stage event resulting from various cardiovascular diseases, and it is now well established that cardiomyo-cyte apoptosis is an important component of cardiac remodeling, ultimately leading to heart failure An excellent recent study suggested that leptin can prevent the increased levels of apoptosis observed upon ageing

in ob⁄ ob mice [13] However, the direct effect of leptin

on cardiomyocyte apoptosis and the intracellular mechanisms involved are still unclear

H9c2 cells, together with use of H2O2to induce apop-tosis, have been used on many occasions as a model system to study regulation of cardiomyocyte cell death [27–29] Here we used this model system to show the effects of short-term (1 h) and long-term (24 h) exposure

of H9c2 cells to leptin on H2O2-induced cell death Our results indicate that 1 h pretreatment with leptin is able

to significantly decrease the apoptotic effects of H2O2

on H9c2 cells and thus protect them from death How-ever, when 24 h preincubation was used, a protective effect was not observed This is not entirely without precedent, as we have previously shown that acute and chronic leptin treatments have distinct effects on insulin signaling and subsequent regulation of glucose uptake

in skeletal muscle cells [30,31] These results suggest that transient intracellular effects stimulated by acute leptin treatment play an important role in the cardioprotective role of leptin, and that the enhanced lipid accumulation found after 24 h treatment with leptin [18] may convey deleterious effects [32,33] The effects observed after a short period of leptin exposure may be of physiological relevance given the fact that circulating leptin levels fluctuate with diurnal rhythm and are not consistently high for 24 h [34]

We have shown here that leptin’s cardioprotective effect against H2O2-induced apoptosis occurs through the prevention of activation of apoptotic markers at

an early stage, including PS exposure to the outer membrane – one of the first detectable signs of apopto-sis [35] The lack of significant propidium iodide stain-ing in our annexin V bindstain-ing studies suggests that 2 h treatment with H2O2 does not induce significant necro-sis in these cells Furthermore, upon investigation of the mechanisms underlying H2O2-induced apoptosis and their regulation by leptin, we observed changes in

Fig 3 Leptin attenuates H2O2-induced mitochondrial membrane

potential loss in H9c2 cells Quiescent H9c2 cells with or without

1 h leptin (6 n M ) pretreatment were exposed to 0.4 l M H2O2 for

30 min JC-1 fluorescence was measured by confocal microscopy,

assessing the emission shift from green (530 nm) to red (590 nm)

using 488 nm excitation Composite red and green fluorescence is

shown Results are representative of those from three separate

experiments.

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major components of the intrinsic pathway of apopto-sis Notably, the mechanism whereby leptin prevents activation of the intrinsic pathway of apoptosis appears to involve prevention of the H2O2-induced change in the cellular localization and activity level of the pro-apoptotic Bax protein [36] detected by immu-nofluorescence microscopy using a conformation-sensi-tive antibody [22] Accordingly, attenuation of a decrease in mitochondrial membrane potential, and of the subsequently increased cytochrome c release and caspase-3 activation was also observed in cells pre-treated with leptin

The theory of selective leptin resistance occurring in obese individuals has been suggested based upon observations that, while the effects of leptin on satiety and energy metabolism were blunted, the sympatho-excitatory effects were maintained in obese individuals [9,37] Whether enhanced or suppressed myocardial leptin action, either direct or centrally mediated, exists pre- and post-myocardial infarction in obese

Merged

A

B

C

D

Fig 4 Leptin decreases H 2 O 2 -induced cyto-chrome c release from mitochondria Confo-cal analysis of H9c2 cells treated with or without leptin (6 n M , 1 h) prior to exposure

to H2O2(400 l M ) for 2 h shows immuno-staining of cytochrome c (green), Mitotrac-ker staining of mitochondria (red), and merged images of the two showing co-local-ization in yellow Upon release of cyto-chrome c from mitochondria, green fluorescence can be seen independently (A) Control, (B) leptin treatment for 1 h, (C)

H 2 O 2 treatment, (D) H 2 O 2 treatment with

1 h leptin pretreatment Images shown are representative of four independent experiments.

Fig 5 Leptin attenuates H 2 O 2 -induced exposure of the Bax

N-ter-minus Immunofluorescence staining (green) of Bax using Bax

N-terminal (N20) antibody, which only detects Bax localized in

mito-chondrial membrane The results are for cells after 4 h exposure to

H 2 O 2 (400 l M ) with or without leptin pretreatment (6 n M , 1 h).

Images are representative of three independent experiments.

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individuals is still a matter of some debate Our study

clearly indicates a direct, as opposed to systemic or

centrally mediated, role for leptin in mediating

cardio-myocyte apoptosis, and reinforces data from in vivo

studies suggesting a cardioprotective role for leptin via

mediation of anti-apoptotic effects As mentioned

above, leptin- or leptin receptor-deficient rodents

dis-play an increased rate of cardiac apoptosis The

increase in apoptotic rate and mortality was abolished

upon leptin injection in ob⁄ ob mice but not db ⁄ db

mice, indicating that leptin plays an important role in

cardioprotection [13] Furthermore, it has recently

been shown that perfusion of the heart with leptin

dur-ing a short reperfusion period (35 min) significantly

decreased mitochondrial membrane pore opening and

the infarct size induced by ischemia⁄ reperfusion [38]

In summary, our current in vitro study suggests that

leptin exerts a protective effect against H2O2-induced

apoptosis in H9c2 rat cardiomyocytes by preventing

activation of components of the

mitochondrial-depen-dent intrinsic pathway of apoptosis This is in keeping

with other recent data [13], butt the effect mediated by

leptin in vivo may depend on the development of leptin

resistance, the stage in progression of heart failure or

other variables Overall, the direct influence of leptin

on cardiac structure and function is still uncertain, but

appears to be of growing importance

Experimental procedures

Culture of H9c2 rat cardiomyocytes

The rat embryonic ventricular myocardial cell line H9c2

was maintained as described previously [39] in DMEM with

4.5 gÆL)1glucose supplemented with 10% (v⁄ v) fetal bovine

serum and 1% penicillin⁄ streptomycin (v ⁄ v) Cells were routinely grown to 80% confluence in 75 cm2 flasks at

37C with an atmosphere of 5% CO2prior to passage and seeding for experiments All cell-culture materials were pur-chased from Wisent (Quebec, Canada) For the induction

of cell death, cells were exposed to H2O2 (400 lm, Sigma-Aldrich, St Louis, MO, USA) for various time periods as indicated following treatment with leptin (6 nm) We analyzed ObR expression in these cells by PCR, and found expression of both long (ObRb) and short (ObRa) receptor isoforms (data not shown)

Determination of cell viability The MTT assay was performed as described previously [40]

as a measure of cell viability In addition, trypan blue exclusion was used in some experiments, and the number of trypan blue-negative cells was counted using a hemocytom-eter 3 days after the end of H2O2treatment

Annexin V binding assay Annexin V Alexa Fluor 488 (Molecular Probes, Eugene,

OR, USA) was used to detect PS exposure to the outer sur-face of the cell membrane according to the manufacturer’s protocol Briefly, cells were grown in a 12-well plate with cover slips in each well They were treated with H2O2 follow-ing incubation with leptin Then the cells were washed with cold NaCl⁄ Piand 1· binding buffer (10 mm Hepes pH 7.4,

140 mm NaCl, 2.5 mm CaCl2) Cells were then incubated with annexin V Alexa Fluor 488 (1 : 20 dilution) and

1 lgÆmL)1propidium iodide diluted in 1· binding buffer for

15 min After incubation, cells were washed twice in 1· bind-ing buffer before mountbind-ing the cover slips on glass slides using DAKO fluorescent mounting medium (DakoCytoma-tion, Missisauga, Canada) Annexin V Alexa Fluor 488 was

H2O2 Leptin (24h) +

+ + + – –

– –

Cleaved caspase 3 Total caspase 3

Leptin (1h)

H2O2 + + + + – – – –

Cleaved caspase 3 Total caspase 3

0 0.5 1 1.5 2 2.5

H2O2

Leptin (h)

+ + + –

0 – –

0 1 24

24

1

Caspase 3 activity (f

A

B

Fig 6 H 2 O 2 -induced cleavage and

activa-tion of caspase-3 are reduced in leptin

pre-treated cells (A) Representative western

blots of cell lysates prepared after H 2 O 2

treatment (400 l M , 4 h) with or without

lep-tin pretreatment (6 n M , 1 h or 24 h) Levels

of the cleaved form of caspase-3

(17⁄ 19 kDa) as well as changes in total

cas-pase-3 levels (35 kDa) were analysed by

western blotting (B) Quantitative analysis of

the activity of caspase-3 measured using a

specific caspase-3 activity assay kit

(mean-s ± SEM, n = 3) The a(mean-steri(mean-sk indicate(mean-s a

statistically significant difference from H 2 O 2

treatment alone (P < 0.05).

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excited at 495 nm, and the fluorescence of cells was

deter-mined using a confocal microscope (Olympus Fluoview

Center Valley, PA, USA) Quantification was performed by

analyzing the fluorescence intensity per cell, and the data

shown are means ± SEM of all experiments, in which two

cover slips were used per condition and nine fields of view

from each cover slip were quantified

Immunofluorescent detection of conformational

changes in Bax (N-terminal exposure) by confocal

microscopy

For analysis of Bax immunofluorescence, cells grown on

cover slips were washed twice with NaCl⁄ Pi, fixed with 4%

paraformaldehyde in NaCl⁄ Pi for 15 min, permeabilized

with 0.2% Triton X-100 for 5 min and blocked using 3%

BSA in NaCl⁄ Pi for 1 h at room temperature Cells were

then incubated for 1 h at 37C with anti-Bax N-terminal

IgG (Santa Cruz Biotechnology, Santa Cruz, CA, USA;

1 : 150) in blocking buffer The unique feature of this assay

is that the N-terminal epitope is not detected when Bax is

retained in the cytosol, but is exposed and detected upon

Bax insertion into the mitochondrial membrane [22] The

cells were washed three times in NaCl⁄ Pi, and incubated

for 1 h at room temperature in anti-rabbit IgG Alexa

Fluor 488 serum (Molecular Probes; 1 : 2000) After

wash-ing, cells were mounted using DAKO mounting medium

and confocal images were analysed as above

Measurement of mitochondrial membrane

potential (Y) using JC-1

H9c2 cells were grown on cover-slips, treated as indicated

in Fig 3, and then washed twice with NaCl⁄ Pi The cells

were incubated with 5 lm JC-1 dye (Molecular Probes) in

serum-free medium for 15 min at 37C The medium was

then removed, and the cells were washed three times with

NaCl⁄ Pi The cells were examined immediately under a

con-focal microscope JC-1 fluorescence was measured to assess

the emission shift from green (530 nm) to red (590 nm) in

polarized mitochondria at 488 nm excitation

Immunofluorescent detection of intracellular

cytochrome c localization by confocal microscopy

To detect cytochrome c release from the mitochondria, cells

grown on cover slips were first treated to stain mitochondria

by incubation for 10 min at room temperature with 10 nm

MitoTracker CMTMRos dye (Molecular Probes) in

NaCl⁄ Pi Cells were fixed with 4% paraformaldehyde for

15 min, permeabilized with 0.2% Triton X-100 for 5 min,

and blocked using 3% serum dissolved in NaCl⁄ Pi for

30 min at room temperature Cells were then probed

with monoclonal anti-cytochrome c IgG (BD Biosciences

Pharmingen, Oakville, Canada; 1 : 250 dilution in blocking solution) for 1 h at room temperature, followed by staining with goat anti-mouse Alexa Fluor 488 (Molecular Probes;

1 : 1000) for 1 h at room temperature After washing, cells were mounted using DAKO mounting medium, and ana-lyzed by confocal microscopy

Caspase-3 activity assay Caspase-3 activity was measured using an Apo-ONE homo-geneous caspase-3 assay kit (Promega, Madison, WI, USA) according to the manufacturer’s protocol Briefly, cells grown on 96-well plates were treated with H2O2 with or without leptin pretreatment After exposure to H2O2, Apo-ONE caspase-3⁄ 7 reagent was added, and the mixture incubated at room temperature for up to 18 h The level of fluorescence was measured using a Wallac 1420 Victor 3 apparatus (Perkin Elmer, Waltham, MA, USA) with excita-tion⁄ emission at 499 ⁄ 521 nm

Immunoblotting for total and cleaved forms of caspase-3

After appropriate treatment of cells, they were washed in NaCl⁄ Piand lysed using lysis buffer (0.5 m Tris⁄ HCl pH 6.8, 2% v⁄ v SDS, 15% v ⁄ v glycerol 10% v ⁄ v 2-mercaptoethanol, 0.2 mm phenylmethanesulfonyl fluoride, 10 lgÆmL)1 leupep-tin, 1 mm pepstatin A, 0.5 mm Na3VO4, 0.2 mm E64, 2 mm okadoic acid, a few grains of bromophenol blue) Centri-fugation at 1500 g was used to precipitate floating cells, which were collected and lysed with the cells growing in culture dish Each lysate was collected and transferred to Eppendorf tubes, which were heated to 65C for 15 min, and the cells were further lysed by passing five times through

a 25-gauge needle⁄ syringe After centrifuging each sample at

12 000 g for 2 min at 4C, 35 lL aliquots were loaded onto

a 10% SDS–PAGE gel After protein transfer to poly(vinyli-dene difluoride) membrane, the membrane was incubated with the primary caspase-3 antibody solution (1 : 1000, Cell Signaling Technology, Beverly, MA, USA) at 4C overnight The antibody detects both total (35 kDa) and cleaved (17⁄ 19 kDa) forms of caspase-3 Then the membrane was incubated in horseradish peroxidase-linked secondary anti-body solution (1 : 10 000) for 1 h and analyzed by enhanced chemilunenescence The b-actin content was routinely checked to confirm the accuracy of protein loading on gels (data not shown) Quantification of band intensity upon wes-tern blotting was conducted using nih image software (National Institutes of Health, Bethesda, MD, USA)

Statistical analysis All data presented are expressed as means ± SEM Sta-tistical analysis was undertaken using Student’s t-test

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Differences between groups were considered significant at

P< 0.05

Acknowledgements

Funding for this work was provided by the Canadian

Institutes of Health Research (CIHR) via an operating

grant and a New Investigator award to GS

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