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Up to 3 lm free calcium, in the presence of ATP, induced strong contraction of permeabilized cardiomyocytes with intact sarcomeres, accompanied by alterations in mitochondrial arrangemen

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regulation of mitochondrial respiration in permeabilized cardiac cells

Tiia Anmann1, Margus Eimre2, Andrey V Kuznetsov3,4, Tatiana Andrienko3, Tuuli Kaambre1,

Peeter Sikk1, Evelin Seppet2, Toomas Tiivel1,2, Marko Vendelin3,5, Enn Seppet1and Valdur A Saks1,3

1 Laboratory of Bioenergetics, National Institute of Chemical Physics and Biophysics, Tallinn, Estonia

2 Department of Pathophysiology, University of Tartu, Estonia

3 Laboratory of Fundamental and Applied Bioenergetics, INSERM E0221, Joseph Fourier University, Grenoble, France

4 Department of General and Transplant Surgery, Innsbruck Medical University, Austria

5 Institute of Cybernetics, Tallinn, Estonia

Calcium ions play a central role in the

excitation-contraction coupling in muscle cells [1,2] and

partici-pate in regulating the activities of multiple enzymes

and metabolic systems, including mitochondrial Krebs

cycle dehydrogenases, in many types of cells [2–6] The

presence of sophisticated Ca-transport systems in

mito-chondria allows these organelles to control the calcium

cycle in the cytoplasmic space [7–15] and the lifetime

of the cell, as overload of mitochondria with calcium

results in opening of the mitochondrial permeability

transition pore, which eventually leads to cell death [11–15] It has also been proposed that, owing to the simultaneous activation of the contractile system and mitochondrial enzymes by calcium, the ATP produc-tion is matched to its demand in cells (‘parallel activa-tion’ mechanism) [16–20] However, both experimental and theoretical studies with detailed mathematical modelling of the calcium effects on the mitochondria showed that calcium can induce, by stimulation of the steps of Krebs cycle, only twofold changes in the rate

Keywords

adenine nucleotides; calcium;

cardio-myocytes; intracellular energetic units,

mitochondria

Correspondence

V A Saks, Laboratory of Bioenergetics,

Joseph Fourier University, 2280, Rue de la

Piscine, BP53X – 38041, Grenoble Cedex 9,

France

Fax: +33 4 76514218

Tel: +33 4 76635627

E-mail: Valdur.Saks@ujf-grenoble.fr

(Received 15 March 2005, revised 21 April

2005, accepted 22 April 2005)

doi:10.1111/j.1742-4658.2005.04734.x

The relationships between cardiac cell structure and the regulation of mitochondrial respiration were studied by applying fluorescent confocal microscopy and analysing the kinetics of mitochondrial ADP-stimulated respiration, during calcium-induced contraction in permeabilized cardiomyo-cytes and myocardial fibers, and in their ‘ghost’ preparations (after selective myosin extraction) Up to 3 lm free calcium, in the presence of ATP, induced strong contraction of permeabilized cardiomyocytes with intact sarcomeres, accompanied by alterations in mitochondrial arrangement and

a significant decrease in the apparent Kmfor exogenous ADP and ATP in the kinetics of mitochondrial respiration The Vmax of respiration showed

a moderate (50%) increase, with an optimum at 0.4 lm free calcium and a decrease at higher calcium concentrations At high free-calcium concentra-tions, the direct flux of ADP from ATPases to mitochondria was dimi-nished compared to that at low calcium levels All of these effects were unrelated either to mitochondrial calcium overload or to mitochondrial permeability transition and were not observed in ‘ghost’ preparations after the selective extraction of myosin Our results suggest that the structural changes transmitted from contractile apparatus to mitochondria modify localized restrictions of the diffusion of adenine nucleotides and thus may actively participate in the regulation of mitochondrial function, in addition

to the metabolic signalling via the creatine kinase system

Abbreviations

FCCP, carbonyl cyanide-p-trifluoromethoxy phenylhydrazone; ICEU, intracellular energetic unit; LDH, lactate dehydrogenase; PK, pyruvate kinase; TMRE, tetramethylrhodamine ethyl ester.

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of mitochondrial oxidative phosphorylation [21–23].

The magnitude of these direct effects of calcium on

mitochondrial respiration is too small to explain the

variations of the respiration rate in the heart cells

in vivo: in the perfused working rat heart, the

respir-ation rate can be enhanced by more than an order

of magnitude (indeed, by a factor of 20) during

work-load changes under conditions of metabolic stability

[24–27] Under physiological conditions in vivo, cardiac

work and respiration are linearly related [24] and both

are governed by the classical Frank–Starling

mechan-ism [28] The Frank–Starling mechanmechan-ism is based on

the length-dependent activation of sarcomere:

stretch-ing of myofibrils by increasstretch-ing left ventricle fillstretch-ing

increases the force of contraction, work performance

and respiration as a result of increased sensitivity of

the thin filaments to calcium [24,28,29] This results in

an increase in the number of active crossbridges,

with-out any significant changes in the cytoplasmic calcium

transients [30–32]

To explain the observed discrepancies (by a factor

of  10) between the direct effects of calcium on the

respiration of mitochondria and changes in the rates

of oxygen consumption in vivo under physiological

conditions of alteration of workloads, in addition to

the effects of calcium, the metabolic channelling of the

endogenous ADP by the organized energy transfer and

signalling networks (the creatine kinase, adenylate

kin-ase and glycolytic systems) has been proposed as a

major signal for regulating mitochondrial respiration

in cardiac cells [25] In myocytes, mitochondria are

arranged in a crystal-like tissue specific pattern [33],

and in oxidative muscle cells, mitochondria form

func-tional complexes with adjacent sarcoplasmic reticulum

and myofibrils, the intracellular energetic units

(ICEUs) [34–41] In these units, the channelling of

ADP by energy transfer networks overcomes local

restrictions of intracellular diffusion of adenine

nucleo-tides [34,39,40] and explains both the linear

relation-ship between workload and respiration and the

phenomenon of metabolic stability [25] Recently, we

have found, in a preliminary study, that structural

changes, caused by the calcium-induced contraction of

sarcomeres in permeabilized cardiac fibers, significantly

modify the kinetic parameters of mitochondrial

respi-ration regulation by exogenous ADP [35] Very similar

data have been reported for rainbow trout muscle cells

[36] In the current study, the structure–function

rela-tionships in cardiac cells have been studied further

with the aim of detailed quantitative analysis of the

structural and functional alterations induced by

chan-ging free calcium concentrations, both in permeabilized

cardiomyocytes and in myocardial fibers The results

show specific sarcomere–mitochondrial structural and functional links as a result of specific cell organization, and are consistent with the theory of a major role of the metabolic signalling mechanisms in the regulation

of mitochondrial respiration

Results

As could be expected, in the control experiments with isolated and permeabilized cardiomyocytes, neither ATP nor calcium (free calcium concentration 1–3 lm) added alone changed the size of the cardiomyocytes, showing an absence of contraction and of any of their nonspecific effects, as well as an absence of intracellu-lar ATP, endogenous substrates and residual ADP in the permeabilized cardiomyocytes (results not shown) However, when ATP (2 mm), or the respiratory sub-strates glutamate or malate and ADP, were present in the medium, the addition of calcium (at a concentra-tion of 1 lm) resulted in a very strong contracconcentra-tion of cardiomyocytes, and the length of cardiomyocytes was decreased by  50% (Fig 1) This strong contraction

of the cells, without subsequent relaxation, is termed

‘hypercontraction’ in this article These changes of cell size were clearly caused by the sarcomere contraction

as, after the extraction of myosin, the shape of the cells remained unaltered following the addition of ATP and calcium, or of mitochondrial substrates, ADP and calcium (Fig 2) In these experiments, the concentra-tion-dependent increase in the fluorescence intensity

of the mitochondrial calcium sensitive probe, Rhod-2 (Fig 2), clearly indicates significant accumulation of calcium in the mitochondrial matrix

It is known that the accumulation of calcium in mitochondria can lead to the opening of the permea-bility transition pore, associated with mitochondrial swelling and rupture of the outer mitochondrial mem-brane [9–15] Therefore, we used several different methods to test pore opening under the conditions of our experiments Figure 3A shows that the addition of ADP activated the respiration of permeabilized fibers

in the presence of 3 lm free calcium, and that the addition of exogenous cytochrome c did not change the respiration rate This means that endogenous cyto-chrome c always stayed in mitochondria and exogen-ous cytochrome c had no access to the intermembrane space, indicating that the outer mitochondrial mem-brane was intact [42] Monitoring of the memmem-brane potential in isolated heart mitochondria by measuring the uptake of Rhodamine 123 (Fig 3B) shows that the single addition of 3 lm free calcium did not change the membrane potential, but the membrane potential collapsed after the addition of an uncoupler, carbonyl

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cyanide-p-trifluoromethoxy phenylhydrazone (FCCP).

However, when the mitochondria were titrated with

increasing concentrations of calcium for longer than

40 min, the membrane potential started to decrease after

a concentration of 3 lm calcium was reach (Fig 3C)

This is caused by the accumulation of calcium, over

time, from the Ca-EGTA buffer in medium into the

mito-chondrial matrix As the duration of our experiments

was usually less than 40 min, it is unlikely that the

mitochondrial permeability transition pore was open

Analysis of the confocal images of the permeabilized cardiomyocytes and fibers with intact sarcomeres (Figs 4 and 5) shows that hypercontraction completely disorganized the localization of mitochondria within these cells Here we used the quantitative method of image analysis of confocal micrographs, recently devel-oped in our laboratories [33], to analyse the changes in the arrangement of mitochondria observed in skinned muscles fixed at both ends (i.e in isometric condi-tions) In control solution (containing 0.1 lm free

Fig 2 Absence of contraction in ‘ghost’ cardiomyocytes after the addition up to 3 l M free calcium in the presence of ATP (1 m M ) and glu-tamate (5 m M ) (A) Control ‘ghost’ cardiomyocytes preloaded with 5 l M Rhod-2 (B) Cardiomyocytes after the addition of 1 l M free calcium (C) Cardiomyocytes after the addition of 3 l M free calcium A significant increase in the fluorescence intensity of Rhod-2 clearly shows an elevated calcium concentration in the mitochondrial matrix of ‘ghost’ cardiomyocytes, in particular after the addition of 3 l M free calcium.

Fig 1 Contraction of permeabilized

cardio-myocyte induced by calcium (1 l M

exter-nally added free Ca2+) in the presence of

ATP (1 m M ) Mitochondrial localization was

imaged using confocal microscopy from

autofluorescence of mitochondrial

flavopro-teins, as described in the Experimental

procedures Changes in the shape of one

cardiomyocyte (induced by calcium in the

presence of ATP), resulting in its

hyper-contraction, is shown over time.

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calcium and no ATP) the mitochondria exhibited a

regular distribution (Fig 4A,B), and Fig 4C shows

that the distances between mitochondrial centers taken

from image in Fig 4B were smallest in the direction

transversal to the fiber, whereas the largest distances

were observed in a diagonal direction (angle 45) The

distribution can be presented in a radial plot, where

the average distance between mitochondrial centers is related to the direction between mitochondria In this plot, the distances between the centers are given by the distances from the reference point (coordinates 0,0) plotted in the direction corresponding to each sector (Fig 4D) From inspection of the radial plot (Fig 4D), it is clear that the mitochondrial centers were not distributed randomly, but arranged according

to a strictly regular pattern

The situation was entirely different if fibers with intact sarcomeres were incubated in the presence of ATP and elevated free calcium (3 lm) (Fig 5) If the fiber is fixed by its ends, the elevated calcium leads to

a disorganization of mitochondrial arrangement in the demonstrated case Indeed, this is evident from the dis-tribution function (Fig 5B): the disdis-tribution function

is almost the same, regardless of the direction In the radial plot (Fig 5D), the centres tended to align along

a circle, which is the expected situation if the random distribution of mitochondria takes place The average distances are increased, in this case, if compared to the control (compare Fig 4D and Fig 5D)

Notably, the arrangement of mitochondria in the cells was changed by high calcium concentrations also

in isolated and permeabilized cardiomyocytes (data not shown) As cardiomyocytes are nonfixed cells, hyper-contraction resulted in a decrease of the length of fibers, and the mitochondria were pressed together between hypercontracted myofibrils [35]

In the permeabilized cardiac fibers with intact sar-comeres, in which an increase in the calcium concen-tration induced hypercontraction and disorganization

of the regular intracellular mitochondrial arrangement, calcium induced changes in the kinetics of regulation

of the respiration rate (Fig 6) This concerned mostly the changes in the apparent affinities for the exogenous adenine nucleotides: a very strong decrease in the val-ues of apparent Km, both for exogenous ADP and for ATP, and much smaller changes in the Vmax of respir-ation (Fig 6A,B) Similar changes were observed in

Fig 3 (A) Cytochrome c test of permeabilized cardiac fibers dem-onstrates the intactness of the outer mitochondrial membrane ADP was added to a final concentration of 2 m M , and cytochrome

c was added to a final concentration of 8 l M (B) Stability of the mitochondrial inner membrane potential at 3 l M free Ca 2+ The fluorescence intensity of Rhodamine 123 (0.25 l M ) in 2 mL of gently stirred solution B (0.1 l M free Ca 2+ ) containing 5 m M gluta-mate and 2 m M malate as mitochondrial substrates and 2 mgÆmL)1

of BSA Isolated rat heart mitochondria were added to a final pro-tein concentration of 0.2 mgÆmL)1 (C) Changes of the mitochond-rial inner membrane potential after a gradual increase of free calcium from 0.1 to 3 l M Arrows show the final concentration of free calcium in the system.

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1 0.8 0.6 0.4 0.2 0

Distance, µm

45°

90°

3 2 1 0 –1 –2 –3 –3 –2 –1 0 1 2 3

50%

X, µm

Fig 4 Quantitative analysis of the regular

arrangement of mitochondria in cardiac cells

preloaded with tetramethylrhodamine ethyl

ester (TMRE) (50 n M ) Representative

confocal image of cardiac muscle fiber (A).

Centers of mitochondria were marked with

small black boxes, as shown in (B) On the

basis of this image, distribution function

(subplot C) and radial plot (subplot D) were

found In subplot C, the distribution

func-tions of distance between the centers of

neighboring mitochondria along the fiber

(direction 90), in cross-fiber direction (0),

and in the diagonal direction (45) are shown.

In subplot D, the distance that encloses

25%, 50%, and 75% of neighboring

mitoch-ondrial centers is shown in the radial plot In

this plot, the distance between

mitochond-rial centers is given through the distance

from the reference point (coordinates 0,0)

and the direction is taken equal to the

middle of the corresponding sector Sector

borders are indicated by dashed lines.

1 0.8 0.6 0.4 0.2 0

Distance, µm

45°

90°

3 2 1 0 –1 –2 –3

50%

X, µm

Fig 5 Quantitative analysis of mitochondrial

arrangement after treatment with calcium.

Fibers were preloaded with

tetramethylrhod-amine ethyl ester (TMRE), as described in

the legend to Fig 4, and fixed at both ends

in a flexiperm chamber Mitochondrial

arran-gement was analyzed after the addition of

3 l M free calcium and incubation for 5 min

at room temperature (A) Representative

confocal image of cardiac muscle fiber (B)

Centers of mitochondria were marked with

small black boxes On the basis of this

image, distribution function (subplot C) and

radial plot (subplot D) were found Note that

the distances between mitochondrial

centres are independent from direction This

is clear from inspecting the distribution

function (subplot C) which is similar in all

directions Some increase of the

intermito-chondrial distances is also seen.

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experiments in which the inhibitor of the

mitochond-rial calcium uniporter, Ruthenium Red, was used to

avoid any accumulation of calcium in the

mitochon-dria and a possible contribution of the PTP opening

into the kinetics of the respiration regulation (results

not shown) The apparent Km for exogenous ADP

decreases by an order of magnitude, from 320 ±

20 lm to 17 ± 3 lm, with an elevation of the free

cal-cium concentration up to 4 lm (Fig 6B) At the same

time, the Vmax values for respiration only showed a

tendency to increase, with a maximum at 0.4 lm

Ca2+, and then to decrease (Fig 6A) Similarly,

the apparent Km for ATP decreased from

286 ± 49 lm to 54 ± 3 lm (Fig 6B) The Vmax value

was always lower than that with ADP and only

minimally changed with alteration in the free calcium

concentration

On the contrary, no changes in the values of the

apparent Kmfor exogenous ADP were found in

perme-abilized ghost cardiac fibers after the extraction of

myosin, when contraction of sarcomere structures was

made impossible (Fig 2) There was only a slight

ten-dency for a decrease of the apparent Km value, which

was not statistically significant Fig 6D Similarly,

there was only a tendency of a decrease in the Vmax

for the respiration with exogenous ADP in ghost fibers

at calcium concentrations higher than 2 lm (Fig 6C)

Remarkably, the apparent Kmfor exogenous ATP in

the regulation of respiration changed in a manner

simi-lar to that for ADP (Fig 6B) Addition of exogenous

ATP activates intracellular ATPases (the kinetics of

this activation is described below) and endogenous ADP production that, in turn, activates respiration It has been observed before [37–39] and is shown in Fig 6B that in the regulation of respiration, the appar-ent Kmfor exogenous ATP is the same as that for exo-genous ADP In both cases it depends, in very similar manner, on the calcium concentration (Fig 6B) In the case of ghost fibers, both are practically independent

of the free calcium concentration (Fig 6D) This com-parison shows very clearly that the observed decrease

in the apparent Kmfor exogenous adenine nucleotides

in the regulation of respiration of permeabilized fibers with intact sarcomeres is related to the changes induced by their contraction These results show also that the direct effects of changes of free calcium on mitochondrial respiration cardiac cells in situ are not significant

An interesting observation is described in Fig 7 It has been described in multiple studies that the appar-ent Km for exogenous ADP in the regulation of mitochondrial respiration in skinned fibers can be effectively decreased by short-term proteolytic treat-ment [43] Figure 7 shows the result of the experitreat-ments

in which the skinned cardiac fibers were incubated with different concentrations of trypsin, at 4C, in solution B containing 0.1 or 3 lm free calcium and ATP, and then the apparent Km values were deter-mined under standard conditions – in the oxygraphic medium containing 0.1 lm free calcium It is clearly seen in Fig 7 that structural changes induced by sarco-mere contraction decreased the rate of the proteolytic

3,5

2,5

1,5

0,5

3

2

1

100 200 300 400

Km

0 100 200 300 400

Km

Ca 2+ , µM

Ca 2+ , µM

Ca 2+ , µM

Ca 2+ , µM

-1 (ww)*min

3,5

2,5

1,5

0,5

3

2

1

0

-1 (ww)*min

SF, ADP

SF, ATP

GF, ADP

SF, ADP

SF, ATP

Fig 6 The effect of free calcium on the regulation of respiration in skinned (A, B) and ‘ghost’ (C, D) fibers by exogenous ADP and ATP The left panel shows the effect of free calcium on the maximal respiration rates and the right panel shows the effect

of free calcium on the values of apparent

K m of respiration Maximal respiration rates were reached at 2.0 and 1.5 m M exogen-ously added ADP and ATP, respectively The apparent Kmand the maximal rates of respiration are shown as means and SD of the data from different experiments and at different concentrations of free calcium Curves in all graphs are illustrative and show the tendency of the effect of free calcium in skinned and ghost fibers The number of independent experiments used to calculate mean values and SD in all groups, was 3–6 See the text for further details.

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degradation of proteins that participate in the regular

arrangement of mitochondria and contribute in

mecha-nisms resulting in a high apparent Km for exogenous

ADP, possibly being responsible for the restriction of

ADP diffusion within fibers and across the outer

mito-chondrial membrane [34,40]

Relating to the results described in Fig 7 are data

showing that the effect of the free calcium on the

apparent Kmfor exogenous ADP is reversible (Fig 8)

When cardiomyocytes or fibers incubated in the

med-ium with 3 lm free calcmed-ium were placed again into the

solution containing 0.1 lm free calcium, the apparent

Km for exogenous ADP increased again up to 300 lm

(Fig 8D) Figure 8A–C shows that this occurred in

parallel with a significant recovery of the initial shape

of permeabilized cardiomyocytes

Figure 9 shows the results of studies in which the

fluxes of endogenous ADP in the permeabilized cells

were measured continuously by using a

spectrophoto-metric method with the coupled enzyme system

consisting of the pyruvate kinase (PK),

phospho-enolpyruvate and lactate dehydrogenase (LDH) [37,39]

In the absence of mitochondrial substrates, the total

MgATPase activity of permeabilized fibers (flux of

ADP out of fibers; upper curves in Fig 9A–C)

increased with the addition of calcium, and the

reac-tion was characterized by a very high apparent Km(of

between 1 and 2 mm) for ATP Similar parameters of

the total MgATPase reactions, Km¼ 1.60 ± 0.49 mm,

were found by HPLC (results not shown), under

conditions when they were uncoupled from the mitoch-ondrial respiration If, then, the mitochmitoch-ondrial sub-strates glutamate and malate were added to activate respiration, the flux of ADP out of fibers (as measured

by using the coupled enzyme assay) was strongly decreased, and, vice versa, the addition of atractyloside restored the ADP production rate (as detected by using the PK⁄ LDH assay) to the levels seen without the respiratory substrates (Fig 9A) Thus, the differ-ence between the ATPase activities before and after the addition of respiratory substrate gave the flux of endogenous ADP channelled from MgATPases directly into mitochondria (Fig 9A) It can be seen that this channelled flux was highest at resting levels of cytoso-lic free calcium (0.1 lm) (Fig 9B) Hypercontraction

of sarcomeres caused by increasing the calcium con-centration up to 2 lm significantly decreased the flux available to mitochondria; owing to disorganization

of the cellular structure, more ADP produced by ATPases could diffuse to and be captured by the PK+phosphoenolpyruvate system

Among the results reported in this work, the decrease in the Vmax of respiration with an increase in the free calcium concentration (Fig 6A) is of interest, and may be explained by an inhibitory effect of increased calcium concentration in the mitochondrial matrix on the ATP synthase, as reported by Holmu-hamedov et al [44] To check this possibility, we repeated the kinetic experiments at 2 lm free calcium

in the presence of 40 mm Na+, which reversed the inhibitory effect on the ATP synthase by activating the

Ca2+⁄ Na+ exchange mechanism in the experiments

of Holmuhamedov et al [44] The results shown in Fig 10 demonstrate that the contraction-induced decrease of Vmax is not reversed by 40 mm Na+, nei-ther in the case of exogenous ADP nor of exogenous ATP Thus, a decrease in the Vmax of respiration in skinned cardiac fibers is caused by hypercontraction but not by the direct effect of calcium on mitochond-rial respiration This is in concordance also with an insignificant decrease of Vmax in ghost fibers during elevation of the free calcium concentration in the medium (Fig 6C)

The experiments described above were carried out under experimental conditions that are far from normal physiological conditions The first of the nonphysio-logical conditions is the absence of a contraction– relaxation cycle and of muscular work performance, which results in the rapid production of ADP in the myofibrillar actomyosin reaction The second is the absence of creatine required to activate the creatine kin-ase–phosphocreatine energy transfer pathway In many earlier publications, the strong stimulatory effect of

Fig 7 Change in sensitivity of the skinned fibers, when in a

hycontracted state, to treatment with trypsin The treatment was

per-formed with increasing trypsin concentrations at a low (0.1 l M , d)

and high (3.0 l M , m) calcium concentration in solution B in the

presence of respiratory substrates, glutamate (5 m M ) and malate

(2 m M ), but not supplemented by BSA, at 4 C Higher trypsin

con-centrations are required for a decrease in the Kmvalue for

endo-genous ADP at a high calcium concentration.

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creatine on respiration in skinned fibers, by decreasing

the apparent Km for exogenous ADP, has been

des-cribed [37,39] Figure 11 shows that a very strong

stimu-latory effect of creatine is observed when exogenous

ATP is used In the presence of creatine, the apparent

Kmfor ATP was decreased from 280 lm to  130 lm

at a free calcium concentration of 0.1 lm, and the Vmax

was strongly increased as a result of ADP production in

the local coupled creatine kinase reactions, including

mitochondrial creatine kinase [38–40] Increase of the

free calcium concentration to 2 lm resulted in some

decrease of the Vmax, but its value stayed higher in the

presence of creatine than in the presence of ATP alone

(Fig 11) Under these conditions, the apparent Km for

ADP remained low because of the presence of both

cal-cium and creatine Thus, under physiological conditions mitochondrial respiration is under the control of the creatine kinase system, and this control may be modified

by an increase in the free calcium concentration

Discussion

The results of this study show that in permeabilized cardiac cells, a significant shortening of sarcomeres – hypercontraction – caused by excess free calcium results in a reversible alteration of the regular arrange-ment of mitochondria in the cells, in the changes in the kinetics of regulation of mitochondrial respiration

by exogenous ADP and ATP, and in the direct channelling of endogenous ADP and ATP between

C

D

Fig 8 Reversibility of the calcium-induced contraction of permeabilized cardiomyo-cytes (A) Cells were incubated and mitoch-ondrial flavoproteins were imaged at 0.1 l M free calcium (B) The hypercontraction shown was induced by increasing the free calcium concentration to 1.0 l M in the pres-ence of 2 m M ATP and 10 m M glutamate (C) Cardiomyocytes were then transferred back into solution B that contained 0.1 l M calcium but no ATP and respiratory sub-strates (D) Reversibility of the effects of calcium-induced contraction of cardiomyo-cytes on the kinetics of regulation of mito-chondrial respiration by exogenous ADP The kinetics of respiratory regulation was measured in solution B containing the respiratory substrates and 3 l M free cal-cium, then fibers were washed twice (7 min each wash) in solution B containing 0.1 l M calcium, and the kinetics were measured again in the presence of 0.1 l M calcium (return to this calcium concentration is shown by 0.1*) The average data for three separate experiments (±SD) are shown.

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ATPases and mitochondria (channelling meaning the

use of ADP or ATP produced without their release

into the medium) Thus, this study demonstrates

strong structure–function relationships between

ATP-producing and ATP-consuming systems [37–40] and

localized restrictions of the intracellular diffusion of

ADP and ATP related to the precise structural

organ-ization of the cell [34,40]

There is abundant information on the effects of

calcium on mitochondria, including its effects on

mito-chondrial respiration, obtained in studies carried out

on isolated mitochondria during the last three decades; these important investigations date back to the work

by Lehninger et al [3,45,46] and later work to those

by Hansford, Denton, McCormack and others [4–10] These studies have recently been extended to in vivo conditions by using confocal imaging and recombinant protein targeting technology [10–16,47–49] The

con-Fig 9 Kinetics of ADP production in dependence of [ATP] in conditions of the absence (continuous line) and presence (with 10 m M gluta-mate and 2 m M malate, dashed line) of oxidative phosphorylation in skinned cardiac fibers Solution B was supplemented with 5 m M phos-phoenolpyruvate, 0.24 m M NADH, a large excess of pyruvate kinase (PK) (20 IU mL)1) and lactate dehydrogenase (LDH) (20 IUÆmL)1), and different [Ca 2+ ] (nominally 0, 0.1 and 2 l M ) at 25 C The curves are produced from data representing the mean values of groups (n ¼ 2–8).

*P < 0.05 compared to the parameter value in the absence of oxidative phosphorylation (A) ADP production rates without free [Ca 2+ ], K m

for ATP without (1.53 ± 0.16 m M ) and with (0.79 ± 0.03 m M *) respiratory substrates, respectively Glut+Mal represents the effect of respir-atory substrates 10 m M glutamate and 2 m M malate, respectively, and Atr the effect of atractyloside (98 l M ) (B) ADP production rates with 0.1 l M free Ca 2+ , Kmwithout (2.33 ± 0.41 m M ) and with (1.15 ± 0.26 m M *) respiratory substrates (C) ADP production rates with 2 l M free

Ca2+, K m without (1.88 ± 0.32 m M ) and with (2.68 ± 0.71 m M ) respiratory substrates To obtain the K m and V max values for each individual measurement the data were fitted to a Michaelis–Menten relationship, and then average values and standard errors were calculated.

1,2

1

0,8

0,6

0,4

0,2

0

200 400 600 800

µM

-1 (WW)*min

1000 1200 1400 1600

ADP, -Na + ADP, +Na + ATP, -Na + ATP, +Na +

Fig 10 The kinetics of regulation of respiration in permeabilized

cardiac fibers by exogenous ADP and ATP and the effect of

Na-acetate Stimulation of mitochondrial respiration at 2 l M free Ca2+

by exogenous ADP (circles) and ATP (squares) in the absence

(white symbols) and presence of 40 m M Na + (black symbols) is

shown The change in the value of maximal respiration rate was

not significant The number of experiments was 4–8.

ATP, µM

3

2

1

0 0,5 1,5 2,5

-1 (ww)*min

Fig 11 The effect of creatine on the kinetics of respiration of skinned fibers by exogenous ATP at 0.1 and 2.0 l M free calcium.

At the 0.1 l M calcium concentration, and in the presence of creat-ine, the V max value increased from 1.48 ± 0.15, in the absence of creatine, to 2.76 ± 0.10, and decreased at 2.0 l M calcium down to 1.64 ± 0.12, but remained still higher than in with 0.1 l M calcium The apparent K m decreased from 275 ± 78 l M to 132 ± 25 l M in the presence of creatine at 0.1 l M calcium and to 108 ± 26 l M at 2.0 l M calcium.

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clusion from all these studies is that mitochondria

par-ticipate, by rapid uptake and release of calcium, in the

regulation of localized cellular calcium metabolism and

calcium transients in the cytoplasm, and that calcium

controls cell life and death under pathological

condi-tions by controlling the opening of the mitochondrial

permeability transition pore [9–15] The results of

com-prehensive and excellent biochemical studies have

sometimes also led to the conclusion that calcium may

regulate the main function of mitochondria –

respir-ation and ATP production in oxidative

phosphoryla-tion – in parallel with the activaphosphoryla-tion of contracphosphoryla-tion

(‘parallel activation’ mechanism) [6,7,16,19–22] While

in some types of cells with very low energy fluxes the

activation of ATP synthesis by calcium may be

suffi-cient to satisfy the increased energy demand [16–18],

this enthusiasm in extrapolation of important

informa-tion of Ca–mitochondrial interacinforma-tions to support the

hypothesis of ‘parallel’ activation of respiration and

contraction by calcium may not be justified in the case

of cardiac muscle cells Indeed, direct experimental

studies carried out by Territo et al [21,22], on isolated

heart mitochondria, showed that calcium increases the

respiration rate in the state 3 by a factor of 2–2.5, and

the respiration rate is remarkably high already at a

cal-cium concentration of zero This experimental result

was confirmed by Cortassa et al., from calculations

obtained by using an integrated model of cardiac

mito-chondrial energy metabolism and calcium dynamics

[23] Under physiological conditions, the regulation of

contraction and related energy fluxes in the heart is

governed by the classical Frank–Starling mechanism,

according to which the cardiac work and oxygen

con-sumption may be increased by a factor of 15–20 by

increasing the diastolic filling of the left ventricle

[24,28,29] Under these conditions no changes in the

cytoplasmic calcium transients have been found [30–

32] The cellular explanation of the Frank–Starling

mechanism is based on the length-dependent activation

of myofilaments as a result of the increased sensitivity

of the thin filaments to calcium at a greater sarcomere

length [30–32,50–52] This results in changes in the

number of active crossbridges within sarcomeres at a

constant concentration of intracellular free calcium,

and consequently in the alteration of force

develop-ment, MgATP consumption, and MgADP and Pi

pro-duction Apparently, this initiates an effective feedback

metabolic regulation of respiration via energy transfer

networks [25] The results of this study are in favour

of the latter physiological mechanism Indeed, in the

presence of an excess of exogenous ADP when this

substrate is available at a high concentration, in the

case of the ‘parallel activation’ mechanism, the

max-imal respiration rates should be dependent only upon calcium concentration both in permeabilized cardiac fibers with intact sarcomeres and in ghost fibers, and one should expect a strong increase in the respiration rate with an increase in the calcium concentration However, as shown in Fig 6, there is only a slight increase of Vmax (by some 40%), with the optimum free calcium concentration of 0.4 lm, in permeabilized fibers, and a subsequent decrease in Vmaxat higher cal-cium concentrations, and these modest changes in

Vmax are completely eliminated in ghost fibers, from which most of the myosin ATPase is depleted Similar observations have been made previously [35,36] Clearly, calcium ions are unable to stimulate oxidative phosphorylation without involvement of extramito-chondrial ATPases Under conditions of hypercont-raction, in the absence of relaxation and force development, the contraction cycle is probably slowed down and the related actomyosin MgATPase activity decreased, thus decreasing the direct supply of ADP to mitochondria

This conclusion is also consistent with the results of Khuchua et al., who have shown that there is no direct significant activation of mitochondrial respiration by

Ca2+ions in muscle cells in situ [53] but the effects of changes in free calcium concentration rather result from indirect effects of the Ca2+ stimulation of acto-myosin crossbridge cycling that provides ADP to acti-vate respiration [53]

This study shows also that unitary organization of intracellular energy metabolism into ICEUs confers the effective regulative mechanisms of ATPases to car-diac cells This is evident from comparison of the ATPase vs [ATP] relationships in isolated myofibrils and skinned fibers: whereas our analysis revealed the

Kmfor MgATP in the MgATPase reaction to be close

to 1.5–2 mm in saponin-skinned cardiac fibers, the value of Km was more than two orders of magnitude less in isolated myofibrils (10–50 lm) [54,55] in the absence of oxidative phosphorylation In both prepara-tions the PK+phosphoenolpyruvate system was used for measurements of ADP produced by ATPases However, in contrast to isolated myofibrils, where the PK+phosphoenolpyruvate system could effectively eliminate the accumulation of ADP (a product of the ATPase reaction), thereby conferring high ATP-sensi-tivity to myofibrils, the PK+phosphoenolpyruvate system was unable to consume the endogenous ADP produced in the interior space of the ICEUs in skinned fibers, as it has been many times demonstrated [35,37,39] Hence, ADP could accumulate and remain inside the ICEUs owing to restricted diffusion out from that structure For the same reasons, ATP could

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