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Tiêu đề Metabolic control of mitochondrial properties by adenine nucleotide translocator determines palmitoyl-CoA effects: implications for a mechanism linking obesity and type 2 diabetes
Tác giả Jolita Ciapaite, Stephan J. L. Bakker, Michaela Diamant, Gerco Van Eikenhorst, Robert J. Heine, Hans V. Westerhoff, Klaas Krab
Trường học Vrije Universiteit Amsterdam
Chuyên ngành Molecular cell physiology
Thể loại Research article
Năm xuất bản 2006
Thành phố Amsterdam
Định dạng
Số trang 15
Dung lượng 770,96 KB

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2A, when experimentally obtained values of ATPout⁄ ADPout ratios Table 1 and [16] are used in the calculation, inhibition with palmitoyl-CoA would cause an increase in [AMP]out of 17% an

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nucleotide translocator determines palmitoyl-CoA effects Implications for a mechanism linking obesity and type 2 diabetes Jolita Ciapaite1,5, Stephan J L Bakker2, Michaela Diamant3, Gerco van Eikenhorst1,

Robert J Heine3, Hans V Westerhoff1,4and Klaas Krab1

1 Department of Molecular Cell Physiology, Institute for Molecular Cell Biology, Faculty of Earth and Life Sciences, VU University,

Amsterdam, the Netherlands

2 Department of Internal Medicine, University of Groningen and University Medical Center Groningen, the Netherlands

3 Department of Endocrinology, Institute for Cardiovascular Research, VU University Medical Center, Amsterdam, the Netherlands

4 Manchester Centre for Integrative Systems Biology, MIB, University of Manchester, UK

5 Centre of Environmental Research, Faculty of Nature Sciences, Vytautas Magnus University, Kaunas, Lithuania

Keywords

metabolic control analysis; oxidative

phosphorylation; palmitoyl-CoA; reactive

oxygen species; type 2 diabetes

Correspondence

J Ciapaite, Centre of Environmental

Research, Faculty of Nature Sciences,

Vytautas Magnus University, Kaunas,

Vileikos 8, LT-44404, Lithuania

Fax: +370 37 327904

Tel: +370 37 327905

E-mail: jolita.ciapaite@falw.vu.nl

(Received 21 June 2006, revised 19 August

2006, accepted 4 October 2006)

doi:10.1111/j.1742-4658.2006.05523.x

Inhibition of the mitochondrial adenine nucleotide translocator (ANT) by long-chain acyl-CoA esters has been proposed to contribute to cellular dys-function in obesity and type 2 diabetes by increasing formation of reactive oxygen species and adenosine via effects on the coenzyme Q redox state, mitochondrial membrane potential (Dw) and cytosolic ATP concentrations

We here show that 5 lm palmitoyl-CoA increases the ratio of reduced to oxidized coenzyme Q (QH2⁄ Q) by 42 ± 9%, Dw by 13 ± 1 mV (9%), and the intramitochondrial ATP⁄ ADP ratio by 352 ± 34%, and decreases the extramitochondrial ATP⁄ ADP ratio by 63 ± 4% in actively phosphorylat-ing mitochondria The latter reduction is expected to translate into a 24% higher extramitochondrial AMP concentration Furthermore, palmitoyl-CoA induced concentration-dependent H2O2 formation, which can only partly be explained by its effect on Dw Although all measured fluxes and intermediate concentrations were affected by palmitoyl-CoA, modular kin-etic analysis revealed that this resulted mainly from inhibition of the ANT Through Metabolic Control Analysis, we then determined to what extent the ANT controls the investigated mitochondrial properties Under steady-state conditions, the ANT moderately controlled oxygen uptake (control coefficient C¼ 0.13) and phosphorylation (C ¼ 0.14) flux It controlled intramitochondrial (C¼)0.70) and extramitochondrial ATP ⁄ ADP ratios (C¼ 0.23) more strongly, whereas the control exerted over the QH2⁄ Q ratio (C¼)0.04) and Dw (C ¼ )0.01) was small Quantitative assessment

of the effects of palmitoyl-CoA showed that the mitochondrial properties that were most strongly controlled by the ANT were affected the most Our observations suggest that long-chain acyl-CoA esters may contribute

to cellular dysfunction in obesity and type 2 diabetes through effects on cellular energy metabolism and production of reactive oxygen species

Abbreviations

[AMP]out, concentration of extramitochondrial AMP; AMPK, AMP-activated protein kinase; ANT, adenine nucleotide translocator;

Ap5A, P1,P5-di(adenosine-5¢)-pentaphosphate; ATP in ⁄ ADP in ratio, ATP to ADP ratio in the mitochondrial matrix; ATP out ⁄ ADP out ratio,

extramitochondrial ATP to ADP ratio; C X m

i , concentration control coefficient, quantifying control of intermediate Xmby module i; C J k

i , flux control coefficient, quantifying control of flux Jkby module i; Dw, membrane potential, i.e electrical potential across the inner mitochondrial membrane; J 1 , proton leak flux; J o , oxygen uptake flux; J p , phosphorylation flux; LCAC, long chain acyl-CoA ester; QH 2 ⁄ Q ratio, ratio of reduced to oxidized coenzyme Q; ROS, reactive oxygen species; S-13, 5-chloro-3-t-butyl-2¢-chloro-4¢-nitrosalicylanilide.

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In mammals, mitochondria produce the majority

of ATP required to drive energy-dependent cellular

processes However, mitochondria also play more

indirect roles Impaired mitochondrial function is

emerging as an important factor in insulin-resistant

states: less efficient mitochondrial oxidative

phos-phorylation has been demonstrated in both the

elderly and insulin-resistant offspring of patients with

type 2 diabetes compared with young, healthy

con-trols [1,2] Although under physiological conditions

nonesterified fatty acids are an important source of

fuel for many tissues because they can yield relatively

large quantities of ATP, obesity-related persistent

oversupply of nonesterified fatty acids and

accumula-tion of triacylglycerols in nonadipose tissues is

thought to contribute to the molecular mechanisms

underlying both insulin resistance and b-cell

dysfunc-tion in type 2 diabetes [3,4] Nonesterified and

esteri-fied fatty acids interfere with mitochondrial oxidative

phosphorylation in vitro [5,6] Furthermore, an

imbal-ance in fatty acid metabolism resulting in activation

of nonoxidative rather than oxidative pathways and

accumulation of biologically active molecules [e.g

long-chain acyl-CoAs (LCACs), ceramide,

diacylglyc-erol] could adversely affect cellular function by direct

effects on a variety of enzymes and induction of

apoptosis [4]

Tight regulation of intracellular concentrations of

free LCACs by acyl-CoA-binding protein can be

impaired under pathological conditions with excess

lipid supply (e.g obesity) because of inadequate

expression of the latter [7] LCACs modulate the

activity of the mitochondrial adenine nucleotide

translocator (ANT) from both the outer and matrix

sides of the inner mitochondrial membrane by

com-petitive displacement of the nucleotide from its

bind-ing site on the protein [8] It has been hypothesized

that increased concentrations of free LCACs interfere

with mitochondrial function through inhibition of

the ANT, leading to lower cytosolic ATP and matrix

ADP availability, increased mitochondrial membrane

potential (Dw), and reduction level of coenzyme Q

[9] The two latter events are expected to promote

the formation of reactive oxygen species (ROS)

[10,11], resulting in impaired cellular functions and

cell death Moreover, increased AMP production by

adenylate kinase caused by the low cytosolic

ATP⁄ ADP ratio and further breakdown of AMP to

adenosine is expected to result in an increase in

extracellular adenosine concentration [12] The latter

is a potent vasodilator [13], which can promote

sodium retention in the kidney and stimulate

sympa-thetic nervous system activity [14]

Fatty acid-induced insulin resistance in liver is one

of the main causes of hyperglycemia in type 2 diabetes [15], and the role of mitochondria in this dysfunction

is not fully elucidated We have shown that, in isolated rat liver mitochondria oxidizing succinate, palmitoyl-CoA inhibited the ANT and induced working-condi-tion-dependent changes in intramitochondrial and extramitochondrial ATP concentrations and Dw [16] The relative contribution of a particular enzyme to the control of metabolic pathway flux and concentrations

of reaction intermediates determines to what extent inhibition of that enzyme would affect pathway flux and intermediate concentrations The control can be quantitatively assessed using Metabolic Control Analy-sis [17–19] The control of fluxes and intermediates is a system property, i.e it is determined by all enzymes constituting the pathway For this reason here we quantitatively assessed the control of fluxes and inter-mediates of oxidative phosphorylation not only by the ANT but also by other components of oxidative phos-phorylation Furthermore, we tested parts of the above hypothesis by determining the effects of palmitoyl-CoA on actively phosphorylating (state 3) mitochon-dria oxidizing a more physiological NADH-delivering substrate, i.e glutamate plus malate To investigate which mitochondrial enzymes are involved in the multiple effects that we encountered, we implemented modular kinetic analysis We found that palmitoyl-CoA acts directly on the ANT, and then indirectly induces ROS production and a concomitant reduction

in the extramitochondrial ATP⁄ ADP ratio The extent

to which palmitoyl-CoA affected different mitochond-rial properties can largely be explained by the magni-tude of the control exerted by the ANT over these properties

Results

Palmitoyl-CoA effects on steady-state fluxes and intermediate concentrations

Table 1 summarizes the effects of 5 lm palmitoyl-CoA

on the steady-state fluxes and intermediate concentra-tions in isolated rat liver mitochondria respiring on glutamate plus malate Palmitoyl-CoA decreased oxygen uptake flux (Jo) by 56 ± 3% and phosphoryla-tion flux (Jp) by 58 ± 7%, and increased proton-leak flux ( J1) by 37 ± 6% The opposite effect was found

on the extramitochondrial and matrix ATP⁄ ADP ratios: the former decreased by 63 ± 4%, and the lat-ter increased by 352 ± 34% The reduced to oxidized coenzyme Q ratio (QH2⁄ Q) increased by 42 ± 9%, and Dw increased by 13 ± 1 mV (9%) The QH2⁄ Q

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ratio in mitochondria respiring on succinate was

4.9 ± 0.3 and 5.4 ± 0.2 in the absence and presence

of 5 lm palmitoyl-CoA, respectively We conclude that

palmitoyl-CoA affects virtually all steady-state

proper-ties of these mitochondria, albeit to various extents

Palmitoyl-CoA effects on mitochondrial H2O2

production

We have shown that 5 lm palmitoyl-CoA caused a

significant increase in Dw in actively phosphorylating

mitochondria (state 3) respiring on succinate [16] and

NADH-delivering substrate (Table 1) To test the

notion that the palmitoyl-CoA-induced increase in Dw would stimulate ROS production [10], we determined the effect of palmitoyl-CoA on H2O2 production in mitochondria respiring on succinate Figure 1A shows that palmitoyl-CoA induced H2O2 production in state 3 in a concentration-dependent manner The palmitoyl-CoA-induced H2O2 production was partially sensitive to protonophore S-13, suggesting dependence

on Dw (Fig 1B) In line with this, inhibition of the ANT with atractyloside or carboxyatractyloside and ATP synthase with oligomycin also induced H2O2 formation, although to a lower extent (Fig 1B)

To test whether palmitoyl-CoA metabolism via b-oxidation contributes to increased H2O2 production,

we determined the effect of palmitoyl-l-carnitine (sub-strate for b-oxidation) and malonyl-CoA (inhibitor

of palmitoyl-carnitine transferase 1, part of the mito-chondrial acyl-CoA transport system)

Palmitoyl-l-carnitine (5 lm) alone and in combination with atractyloside (to test whether the effect of palmitoyl-CoA requires both its oxidation and its inhibition of the ANT) stimulated H2O2 production rate less than

5 lm palmitoyl-CoA (Fig 1B), suggesting that b-oxi-dation was not involved Furthermore, rotenone, an inhibitor of respiratory chain complex I, had no significant effect on palmitoyl-CoA-induced H2O2 pro-duction However, partial inhibition of palmitoyl-CoA-induced H2O2 production with malonyl-CoA (Fig 1B) suggests that palmitoyl-CoA partially exerts its effect from the matrix side

Table 1 Steady-state values of fluxes and intermediates, as

affec-ted by palmitoyl CoA Values are mean ± SEM from four

experi-ments.

No Palmitoyl-CoA

+ 5 l M

Palmitoyl-CoA

Jo[nmol O2Æmin)1Æ(mg protein))1] 53 ± 3 23 ± 2**

Jp[nmol ADPÆmin)1Æ(mg protein))1] 375 ± 26 160 ± 15**

J 1 (nmol O 2 Æmin)1Æ(mg protein))1] 3.3 ± 0.3 4.5 ± 0.4**

*P < 0.05 and **P < 0.01 versus no palmitoyl-CoA.

Fig 1 Effect of palmitoyl-CoA on H2O2production in isolated mitochondria respiring on succinate (A) Dependence of H2O2production on palmitoyl-CoA concentration (B) Comparison of the effects of various inhibitors on H2O2production St 3, State 3; p-CoA, palmitoyl-CoA (5 l M ), protonophore S-13 (0.2 l M ); AT, atractyloside (1.5 l M ); CAT, carboxyatractyloside (0.1 l M ); Oligo, oligomycin (0.5 l M ); Ro, rotenone (2 l M ); M-CoA, malonyl-CoA (0.1 m M ); PC, palmitoyl- L -carnitine (5 l M ) All inhibitors were added in state 3 Values are mean ± SEM from four experiments *P < 0.001 versus state 3; #P < 0.02 and $P < 0.002 versus 5 l M palmitoyl-CoA.

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Palmitoyl-CoA effects on extramitochondrial AMP

concentration

We have shown that 5 lm palmitoyl-CoA caused a

sig-nificant decrease in the extramitochondrial ATP⁄ ADP

ratio (ATPout⁄ ADPout) (Table 1) However, in this

par-ticular experiment it was not possible to determine the

effect of decreased extramitochondrial ATP availability

on extramitochondrial AMP formation experimentally,

as we used P1,P5-di(adenosine-5¢)-pentaphosphate

(Ap5A) as inhibitor of adenylate kinase to prevent

depletion of available ATP and ADP and to maintain

steady-state respiration Instead, we did a theoretical

calculation of the extramitochondrial AMP

concentra-tion ([AMP]out) expected at different ATPout⁄ ADPout

ratios This calculation assumes that the adenylate

kin-ase reaction is at equilibrium, which is a safe

assump-tion because there is not much net flux expected

through this enzyme under the conditions investigated

Figure 2A shows [AMP]out predicted to be present at

different steady-state ATPout⁄ ADPout ratios when the

total adenylate concentration is 0.1 mm, with the

assumption that the proportions of adenine nucleotides

are regulated by the adenylate kinase equilibrium In the range of relatively low ATPout⁄ ADPout ratios, a small decrease leads to a large increase in [AMP]out, whereas [AMP]out changes relatively little in the range

of high ATPout⁄ ADPout ratios As indicated in Fig 2A, when experimentally obtained values of ATPout⁄ ADPout ratios (Table 1 and [16]) are used in the calculation, inhibition with palmitoyl-CoA would cause an increase in [AMP]out of 17% and 24% with succinate and glutamate plus malate as substrates, respectively

However, such a low ATPout⁄ ADPout ratio (< 0.2) obtained using excess hexokinase and low concentra-tion of total adenylates (i.e 100 lm) is not likely to

be relevant under physiological conditions For this reason we performed an experiment without adenylate kinase inhibitor and with higher and more physiologi-cally relevant total adenylate concentration (2 mm)

We determined how palmitoyl-CoA (5 and 10 lm) affects the ATPtotal⁄ ADPtotal ratio and [AMP]total in actively phosphorylating (state 3) mitochondria respir-ing on succinate and compared the experimental and calculated values (Fig 2B) Because the total adeny-late concentration in the medium was high (2 mm) and the contribution of the matrix adenylates was relatively low ( 10 lm), we assumed that changes

in the ATPtotal⁄ ADPtotal ratio reflect changes in the ATPout⁄ ADPout ratio Palmitoyl-CoA caused a signi-ficant concentration-dependent decrease in the ATPtotal⁄ ADPtotal ratio and increase in [AMP]total, which corresponded quite well to the correlation of [AMP]out and the ATPout⁄ ADPout ratio predicted by the calculation

Palmitoyl-CoA specifically affects the ANT

To identify the sites of oxidative phosphorylation directly affected by palmitoyl-CoA, we applied modu-lar kinetic analysis in two different ways: with either

Dw or matrix ATP⁄ ADP ratio (ATPin⁄ ADPin) as an intermediate Modular kinetic analysis with Dw as con-necting intermediate revealed that palmitoyl-CoA inhibits the phosphorylating module (Fig 3A), as the flux through the module (Jp) was significantly lower in the presence of palmitoyl-CoA than in its absence, when both conditions were compared for the same lev-els of Dw The flux through the substrate-oxidation module was slightly, although not significantly, higher

in the presence of palmitoyl-CoA (Fig 3B), indicating

a tendency of palmitoyl-CoA to stimulate the activity

of this module, possibly via its effect on b-oxidation The proton-leak module was not affected directly by palmitoyl-CoA (Fig 3C)

Fig 2 Dependence of AMP concentration on the ATP ⁄ ADP ratio.

(A) Dependence of AMP concentration on the ATP ⁄ ADP ratio when

the total concentration of adenylates is 100 l M [AMP] was

calcula-ted as described in Experimental procedures using an equilibrium

constant for adenylate kinase equal to 0.442 [42] The points on the

curve show [AMP] expected to be present at the experimentally

obtained mean values of ATP out ⁄ ADP out for succinate [16] and

glutamate plus malate (Table 1), respectively, if adenylate kinase

was not inhibited (B) Dependence of AMP concentration on the

ATP⁄ ADP ratio when the total concentration of adenylates is

2 m M The points show experimentally determined dependence of

[AMP]total on the ATPtotal⁄ ADP total ratio in actively phosphorylating

(state 3) mitochondria respiring on succinate with no adenylate

kin-ase inhibitor added The points correspond to conditions with 0, 5

or 10 l M palmitoyl-CoA added, and are mean ± SEM from three

independent experiments *P < 0.05 versus no palmitoyl-CoA.

Succ, Succinate; g + m, glutamate plus malate; p-CoA,

palmitoyl-CoA Open symbols, no palmitoyl-CoA; closed symbols, +

palmi-toyl-CoA.

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Further analysis with the ATPin⁄ ADPin ratio as an

intermediate showed that the ATP-consuming module

(comprising the ANT and hexokinase) was inhibited

by palmitoyl-CoA (Fig 4A), as concluded from lower

flux through the module in the presence of

palmitoyl-CoA, while the ATP-producing module was not

affected (Fig 4B) We have shown previously that

hexokinase is not inhibited by palmitoyl-CoA [16]

Therefore our current data indicate that, also in

mitochondria respiring on the NADH-delivering sub-strate, ANT is the only component of oxidative phos-phorylation affected by palmitoyl-CoA, although a stimulatory effect on substrate oxidation cannot be excluded Thus the multitude of effects on steady-state fluxes and intermediate concentrations exerted by palmitoyl-CoA is achieved through inhibition of the ANT

Metabolic control of mitochondrial properties

To determine whether palmitoyl-CoA affected the properties it would be expected to affect for its direct action on the ANT, and to see if we could account for the observation that some properties were affected more than others, we used the systems biology method

of Metabolic Control Analysis To assess the control

of fluxes and intermediates, we took a modular approach (Fig 5)

Metabolic control of fluxes Control coefficients of the six modules of oxidative phosphorylation over the oxygen uptake (Jo) and phosphorylation flux (Jp) for both respiratory sub-strates are summarized in Table 2 The distribution pattern of the control over Jpamong the modules was similar to that of Jo for both substrates used except for the negative control exerted by the proton leak (because it dissipates Dw which is needed to drive ADP phosphorylation and adenine nucleotide trans-location) In all conditions, the control distribution

Fig 3 Effect of palmitoyl-CoA on the kinetics of the oxidative phosphorylation modules around Dw (A) Kinetics of the phosphorylation mod-ule as determined by titration of the substrate oxidation modmod-ule with 0–25 n M myxothiazol (B) Kinetics of the substrate oxidation module determined by titrating the phosphorylation module with 0–0.3 l M oligomycin (C) Kinetics of the proton leak module as determined by titra-tion of the substrate oxidatitra-tion module with 0–55 n M rotenone when the phosphorylation module was blocked with 0.3 l M oligomycin J p

was calculated as: Jp¼ J o ) J h at the same value of Dw; J 1 was measured as Join the absence of ADP phosphorylation [46] Values are mean ± SEM from four experiments Open symbols, no palmitoyl-CoA; closed symbols, +5 l M palmitoyl-CoA.

Fig 4 Effect of palmitoyl-CoA on the kinetics of the modules of

oxidative phosphorylation around the intramitochondrial ATP ⁄ ADP

ratio (A) Kinetics of the ATP-consuming module as determined by

titration of the ATP-producing module with 0–20 n M myxothiazol.

(B) Kinetics of the ATP-producing module as determined by titration

of the ATP-consuming module with 0–0.75 l M atractyloside Jp

was calculated as: J p ¼ J o ) J h at the same value of Dw and

multi-plied by the ADP ⁄ O ratio [16] (ADP ⁄ O ¼ 2.7 ± 0.1) Values are

mean ± SEM from four experiments Open symbols, no

palmitoyl-CoA; closed symbols, +5 l M palmitoyl-CoA.

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was as expected for state 3: the bulk of flux control

was shared between the respiratory chain and the

mod-ules involved in the production of extramitochondrial

ATP (actually glucose 6-phosphate), with hardly any

control by the proton-leak module The contribution

of the ANT to the control of Jo and Jp was moderate and similar with both respiratory substrates

When the two substrates are compared, using glu-tamate plus malate instead of succinate, control of the fluxes shifts from the respiratory chain to ATP synthe-sis Furthermore, the distribution of the control within the respiratory chain shifts from the part downstream

of coenzyme Q with succinate to the part upstream of coenzyme Q with glutamate plus malate

In agreement with the fact that the ANT is the only target of palmitoyl-CoA in the system of oxidative phosphorylation under these experimental conditions,

we found that, with both respiratory substrates, the control exerted by the ANT over Jo and Jp signifi-cantly increased upon inhibition with palmitoyl-CoA The control of Joincreased by 67% and 55% with suc-cinate and glutamate plus malate, respectively, whereas the control of Jp was affected more strongly: it increased by 87% and 83% with succinate and glutam-ate plus malglutam-ate, respectively Owing to the summation property of flux control coefficients [17,18], an increase

in the control strength of one component of the system automatically leads to a decrease in the control strength of other component(s) In our case, an increase in the control of fluxes by the ANT was mainly compensated for by decreased control by the respiratory chain modules (Table 2) Furthermore, the control by the proton-leak module slightly but signifi-cantly increased because palmitoyl-CoA increases Dw, moving the system to a new steady state that is closer

to state 4, where control by proton leak is high

Fig 5 Division of the oxidative phosphorylation into modules The modules: 1, Q-reducing module, comprising dicarboxylate carrier and sub-strate dehydrogenases (malate and NADH dehydrogenases in the case of glutamate plus malate oxidation, or succinate dehydrogenase in the case of succinate oxidation); 2, QH 2 -oxidizing module, comprising cytochrome bc 1 and cytochrome c oxidase; 3, proton leak module, comprising passive membrane permeability to protons and cation cycling; 4, ATP synthesis, comprising ATP synthase and phosphate carrier;

5, adenine nucleotide translocator; 6, hexokinase The intermediates: a, QH2⁄ Q ratio; b, membrane potential (Dw); d, matrix ATP ⁄ ADP ratio (ATP in ⁄ ADP in ); c, extramitochondrial ATP ⁄ ADP ratio (ATP out ⁄ ADP out ) Arrows marked e, h1and p indicate electron flux, transmembrane pro-ton flux, and ATP flux, respectively The dashed arrow h 1 going from Q-reducing module to Dw is valid only when glutamate + malate is used as a substrate.

Table 2 Metabolic control of fluxes The control coefficients were

calculated from elasticity coefficients (Supplementary material,

Table S2) and steady-state fluxes (Table 1 and [16] for glutamate

plus malate and succinate, respectively) Values are mean ± SEM

from three (succinate) or four (glutamate plus malate)

experi-ments (indicated as subscript) Q red, Q-reducing module; QH2ox,

QH2-oxidizing module; Leak, proton-leak module; ATP synth,

ATP-synthesis module; ANT, adenine nucleotide translocator; Hk,

hexo-kinase; p-CoA, palmitoyl-CoA.

Module, i

C J o

i

No p-CoA + 5 l M p-CoA No p-CoA + 5 l M p-CoA

Succinate

ATP synth 0.060.00 0.120.04* 0.060.01 0.150.05*

Glutamate plus malate

Leak 0.040.00 0.140.01** ) 0.03 0.00 ) 0.06 0.01 **

*P < 0.05 and **P < 0.01 versus no palmitoyl-CoA.

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Control of the QH2/Q ratio and Dw

Coenzyme Q reduction level and Dw are among the

factors that determine ROS production by the

mitoch-ondrial respiratory chain [11,12] The control of these

intermediates by the six modules of oxidative

phos-phorylation is summarized in Table 3 The sum of all

concentration (also Dw) control coefficients in a

path-way is zero, by definition [17,18] Accordingly, the

val-ues of the coefficients can be positive or negative

depending on whether an enzyme is involved in the

production or the consumption of an intermediate,

respectively For both substrates used, the QH2⁄ Q

ratio was almost solely controlled by the respiratory

chain enzymes, with the coenzyme Q reducing module

exerting a positive control and the coenzyme QH2

oxidizing module exerting a negative control, while the

control of Dw was shared equally between the

gen-erating (positive control) and consuming or

Dw-consumption-stimulating processes (negative control)

(Table 3) In the case of succinate oxidation, most of

the control of Dw within the respiratory chain resided

in the part downstream of coenzyme Q (cytochrome

bc1 complex and cytochrome c oxidase), whereas, in

the case of glutamate plus malate, the part upstream

of coenzyme Q (dicarboxylate carrier and substrate

dehydrogenases) had slightly more control of Dw,

poss-ibly because NADH dehydrogenase, a proton-pumping

enzyme, becomes active With both respiratory

substrates, the ANT exerted negative control over the

QH2⁄ Q ratio and Dw (Table 3) This is because activa-tion of the ANT stimulates the phosphorylaactiva-tion branch of oxidative phosphorylation, which consumes

Dw The negative control over the QH2⁄ Q ratio is explained similarly

Palmitoyl-CoA had hardly any effect on the control

of the QH2⁄ Q ratio when glutamate plus malate was used as a substrate With succinate, palmitoyl-CoA mainly affected the control of the QH2⁄ Q ratio by respiratory-chain modules: control by both coen-zyme Q-reducing and coencoen-zyme QH2-oxidizing mod-ules has decreased Furthermore, palmitoyl-CoA had little effect on the control of Dw except that the con-trol by the coenzyme Q-reducing and ATP-synthesis module significantly decreased with glutamate plus malate as substrate, and for both substrates the negat-ive control exerted by the proton leak slightly increased because of the effect of palmitoyl-CoA on Dw

Control of matrix and extramitochondrial ATP/ADP ratios

The control of the ATPin⁄ ADPin ratio and ATPout⁄ ADPout ratio is summarized in Table 3 For both sub-strates used, control of the ATPin⁄ ADPin ratio was shared among all modules of oxidative phosphoryla-tion, with a slight negative control exerted by the proton leak The ANT exerted a large negative control

Table 3 Metabolic control of intermediates The control coefficients were calculated from elasticity coefficients (Supplementary material, Table S2) and steady-state fluxes (Table 1 and [16] for glutamate plus malate and succinate, respectively) Values are mean ± SEM from three (succinate) or four (glutamate plus malate) experiments (indicated as subscript) Q red, Q-reducing module; QH 2 ox, QH 2 -oxidizing module; Leak, proton-leak module; ATP synth, ATP-synthesis module; ANT, adenine nucleotide translocator; Hk, hexokinase; p-CoA, palmi-toyl-CoA.

Module, i

CQH2 =Q

i CiD CATPin =ADP in

i CATPout =ADP out

i

Succinate

Glutamate plus malate

*P < 0.05 and **P < 0.01 versus no palmitoyl-CoA.

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over the ATPin⁄ ADPin ratio, because it functions as a

‘consumer’ of matrix ATP by transporting it from

mitochondria to the intermembrane space The

distribution of control within the respiratory chain

depended on the substrate used: for succinate, the

QH2-oxidizing module exerted more control than

Q-reducing module, whereas, with glutamate plus

ma-late as substrate, it was the opposite Palmitoyl-CoA

tended to increase the positive control of the ATPin⁄

ADPinratio by ATP synthesis and the negative control

by the proton leak The negative control of the ATPin⁄

ADPinratio by the ANT increased by 100% and 82%

with succinate and glutamate plus malate as substrate,

respectively

For both substrates, hexokinase exerted the highest

negative control on the ATPout⁄ ADPout ratio

(Table 3) The remainder of the control was distributed

among the respiratory-chain modules, ATP synthesis,

and the ANT, with negligible negative control exerted

by the proton leak Similarly to the control of the

ATPin⁄ ADPin ratio, the distribution of the control of

the ATPout⁄ ADPout ratio within the respiratory chain

depended on the substrate used Comparing the two

substrates, ATP synthesis exerted less control over the

ATPout⁄ ADPout ratio in the case of succinate

oxida-tion Palmitoyl-CoA increased the control of the

ATPout⁄ ADPout ratio by ATP synthesis and proton

leak, and decreased the control by the Q-reducing

module with both respiratory substrates, and the

con-trol by the QH2-oxidizing module and hexokinase with

succinate The control of the ATPout⁄ ADPout ratio by the ANT increased by 56% and 113% with succinate and glutamate plus malate as substrate, respectively

Partial integrated responses to palmitoyl-CoA Table 4 summarizes integrated elasticities to palmitoyl-CoA and partial integrated responses of system fluxes and intermediates to palmitoyl-CoA mediated through each module of oxidative phosphorylation With both respiratory substrates, the ANT had the largest elasti-city to palmitoyl-CoA, in agreement with the finding that, under our experimental conditions, the ANT is the main target of palmitoyl-CoA in oxidative phos-phorylation As a consequence, the response mediated through the ANT contributed most to the overall response of the system fluxes and intermediates to palmitoyl-CoA, i.e the response through the ANT was responsible for 68% of the decrease in Jo, 68% of the decrease in Jp, 56% of the increase in the QH2⁄ Q ratio, 70% of the increase in Dw, 72% of the increase

in the ATPin⁄ ADPinratio, and 59% of the decrease in the ATPout⁄ ADPout ratio with succinate as substrate Similar results were obtained when glutamate plus malate was used as substrate: the response through the ANT contributed 75% of the reduction in Jo, 76% of the reduction in Jp, 68% of the increase in Dw, 88% of the increase in the ATPin⁄ ADPinratio, and 69% of the reduction in the ATPout⁄ ADPout ratio The exception was the QH2⁄ Q ratio, where the response through the

Table 4 Contribution of individual modules of oxidative phosphorylation to the overall response of system variables to palmitoyl-CoA The partial integrated responses (IR) of each module to 5 l M palmitoyl-CoA were calculated using control coefficients (Tables 2 and 3) and integ-rated elasticity coefficients (Ie) of modules to palmitoyl-CoA as described in [21] Values are mean ± SEM from three (succinate) or four (glu-tamate plus malate) experiments (indicated as subscript) Modules: 1, Q reducing; 2, QH 2 oxidizing; 3, proton leak; 4, ATP synthesis;

5, ANT; 6, hexokinase p-CoA, Palmitoyl-CoA; OR, overall response.

pCoA iIRJp

pCoA iIRQH2 =Q

pCoA iIRDpCoA i IRATPin =ADP in

pCoA iIRATPout =ADP out

pCoA Ie i

pCoA

Succinate

Glutamate plus malate

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ANT contributed only 29% of the overall increase in

the QH2⁄ Q ratio, most of the rest of the increase

stem-ming from stimulation of the Q-reducing module

(52%)

The response of a system variable to an external

effector mediated through a specific module is

deter-mined by the control exerted by that module over a

system variable and the elasticity of that module to the

effector [20,21] Table 4 shows that the overall effects

of palmitoyl-CoA on system fluxes and intermediates

were mainly mediated through the ANT and that the

properties that were controlled most strongly by the

ANT were affected the most

Discussion

We have shown that palmitoyl-CoA induces ROS

pro-duction in actively phosphorylating isolated rat liver

mitochondria Furthermore, it influences the ATPout⁄

ADPout ratio in such a way that these changes result

in increased [AMP]out This is in line with a mechanism

we proposed to underlie the association between

obes-ity and type 2 diabetes [9,12] However, owing to

mul-tiple interactions in living systems, it can be difficult to

differentiate whether all the effects relate to one or

many primary effects To acknowledge this, using

modular kinetic analysis, we established that the

pri-mary cause of the effects of palmitoyl-CoA was

inhibi-tion of the ANT Assessment of the metabolic control

of fluxes and intermediate concentrations by the ANT

then revealed that this enzyme partially controls many

fluxes, concentrations and potentials This then

con-firmed that an increase in AMP concentration and, at

least partly, stimulation of ROS production are effects

of ANT inhibition This study thereby shows how

sys-tems biology methodologies might help in dissecting

the convoluted cause–effect chains in multifactorial

diseases such as obesity and type 2 diabetes

Both starvation and incubation with fatty acids have

been shown to cause a concomitant decrease in

cyto-solic ATP⁄ ADP ratios and an increase in total LCAC

concentrations in perfused rat liver and isolated

hepatocytes, indicating that inhibition of the ANT by

LCACs may be relevant in vivo [22–24] It has been

suggested that modulation of ANT activity by LCACs

might be physiologically significant in the regulation of

gluconeogenesis by fatty acids through effects on the

intramitochondrial ATP⁄ ADP ratio [23]

A decrease in the extramitochondrial concentration

of ATP may result in increased formation of AMP by

adenylate kinase This may subsequently stimulate a

cellular response to stress through activation of

AMP-dependent processes [25] or lead to the breakdown of

AMP to adenosine and extracellular release of the lat-ter [12] The primary mechanism of intracellular adenosine production is hydrolysis of AMP by a cyto-solic 5¢-nucleotidase [26] Increased concentrations of free ADP and AMP in the cytosol are major determi-nants of adenosine production, with extracellular adenosine release correlating linearly with free cyto-solic AMP concentration [27] Exogenous adenosine is

a potent vasodilator (EC50@ 0.1 lm), and, under phy-siological conditions, it facilitates tissue recovery after intensive workload by increasing blood flow and sup-ply of oxygen and metabolic substrates Under patho-logical conditions characterized by inappropriate intracellular triacylglycerol accumulation, a low cyto-solic ATP⁄ ADP ratio may persist because of constant inhibition of the ANT leading to a sustained increase

in extracellular adenosine concentrations, resulting in hyperperfusion, hypertension, increased urate produc-tion, and other abnormalities common to insulin-resist-ant states [12]

We have shown that inhibition of the ANT with palmitoyl-CoA results in a significantly lower ATPout⁄ ADPoutratio With respect to the interrelation between ATPout⁄ ADPout ratios and [AMP]out, we have shown here how [AMP]out increases with decreasing ATPout⁄ ADPout ratio, with larger increases observed at low ratios and smaller changes at high ratios This indi-cates that the effect of LCACs on AMP production will vary depending on the energy state of the cell The theoretical assessment of the correlation was supported

by experimental findings showing that inhibition of the ANT with palmitoyl-CoA leads to a significant palmi-toyl-CoA concentration-dependent decrease in the ATPtotal⁄ ADPtotal ratio and a concomitant increase in [AMP]total On the basis of our findings, we expect that, in intact cells, the absolute cytosolic AMP con-centration will increase moderately in response to a decrease in the cytosolic ATP⁄ ADP ratio in the phy-siologically relevant range However, even at low concentrations of AMP, the relative increase in con-centration would still be substantial and so would the relative effect on the rate of production of adenosine; 5¢-nucleotidase operates in vivo at substrate concentra-tions three orders of magnitude below its Km of 1.2 mm [28]

Inhibition⁄ deinhibition of the ANT depending on LCAC concentration may be relevant in the regulation

of cellular metabolism in vivo via effects on AMP-acti-vated protein kinase (AMPK) Activation of AMPK acts as a switch from anabolic to catabolic metabolism which generates ATP (e.g stimulation of b-oxidation) [25] Thus activation of AMPK would seem to be a desirable effect in obesity, as it would promote the

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consumption of excess fat However, the combination

of persistent ANT inhibition by LCACs with constant

activation of AMPK may have some adverse effects,

because stimulation of b-oxidation in response to

acti-vation of AMPK cannot lead to production of ATP

because of lack of mitochondrial ADP As AMPK

sti-mulates cellular fatty acid uptake [29] and the

availab-ility of circulating fatty acids is increased in obesity,

this may lead to accumulation of intracellular

triacyl-glycerols Furthermore, owing to the decreased flux

through the tricarboxylic acid cycle in the case of

ANT inhibition, b-oxidation-derived acetyl-CoA may

stimulate pyruvate carboxylase, contributing to

increased rates of gluconeogenesis, or may be used for

ketone body synthesis in the liver Indeed, short-term

overexpression of AMPK in mouse liver has been

shown to induce fatty liver and increase ketogenesis

[30]

Stimulation of ROS production is thought to

con-tribute to dysfunction of many different cell types,

but, in particular, to b-cell dysfunction in

insulin-resistant states through low expression of antioxidant

enzymes in these cells [31] Mitochondrial Dw and the

redox state of coenzyme Q are known to affect ROS

formation [10,11] We have shown that 5 lm

palmi-toyl-CoA caused a substantial increase in Dw (13 mV

with glutamate plus malate and 15 mV with succinate

[16] as substrate, compared with a total state 3–state 4

difference of  25 mV) and induced H2O2 production

in mitochondria respiring on succinate The sensitivity

of the palmitoyl-CoA-induced H2O2 production to

protonophore shows that the process is partly

Dw-dependent This substantiates the part of our

hypothesis suggesting that LCACs bring about ROS

production through an increase in Dw [9] The effect

of palmitoyl-CoA on the QH2⁄ Q ratio with both

res-piratory substrates was less pronounced, casting doubt

on the alternative route by which palmitoyl-CoA may

affect ROS production by the respiratory chain

Effects through the more elusive local ubiquinone

rad-ical remain an option Our results indicate that the

palmitoyl-CoA effect on H2O2 production might be

partly exerted from the matrix side, but the effect is

b-oxidation-independent as the substrate of

b-oxida-tion, palmitoyl-l-carnitine, stimulated H2O2

produc-tion less than did equal amounts of palmitoyl-CoA

Moreover, palmitoyl-CoA did not enhance respiration

directly, as measured by modular kinetic analysis A

possibility remains that palmitoyl-CoA increased the

redox level of intramitochondrial NADH and

flavo-proteins, but it was not able to further stimulate

res-piration because it was already operating at Vmax In

such a case, the most reduced redox potential at the

top of the electron-transfer chain might cause extra ROS production Our observation that atractyloside,

a direct inhibitor of the ANT, caused ROS production that could only partly account for palmitoyl-CoA-induced ROS production indicates that the ANT is only partly involved in this process It is possible that palmitoyl-CoA decreased mitochondrial antioxidant capacity by inhibiting nicotinamide nucleotide trans-hydrogenase [32], an enzyme that provides NADPH for regeneration of two important antioxidant com-pounds, glutathione and thioredoxin, in the mitochon-dria, and in this way contributed to increased ROS production

Our data show that the ANT controls many steady-state concentrations, potentials and fluxes In agree-ment with this, the specific effect of palmitoyl-CoA on the ANT appears to be consistent with its ability to affect many fluxes, concentrations and potentials Table 1 shows that palmitoyl-CoA affects different mitochondrial properties to different extents In the light of these observations, we asked whether Meta-bolic Control Analysis could have served to predict the palmitoyl-CoA effects We showed that the ANT con-trolled Dw and the QH2⁄ Q ratio to the least extent, and indeed it was the least affected by palmitoyl-CoA

Jo, Jp, ATPin⁄ ADPin and ATPout⁄ ADPout ratios were more strongly controlled by the ANT, and again this corresponded to a stronger effect of palmitoyl-CoA

We conclude that the specific effect of palmitoyl-CoA

on the ANT and the varying extent to which the ANT controls various mitochondrial properties at steady-state can largely explain the observed palmitoyl-CoA effects

The relatively weak control of the QH2⁄ Q ratio and

Dw by the ANT is in agreement with the finding that ANT inhibition by palmitoyl-CoA and the resulting increase in Dw can only partly account for the observed increase in ROS production We found that, for Dw and the QH2⁄ Q ratio, their immediate produc-ers and consumproduc-ers, i.e the respiratory-chain compo-nents, exerted the strongest control This indicates that, if an increase in ROS production is brought about by alterations in Dw and the QH2⁄ Q ratio, inter-ference with respiratory-chain function will contribute more than interference with any other component of oxidative phosphorylation

It has been shown that the control of Jo by the ANT is comparable in isolated liver mitochondria [33] and isolated hepatocytes [34], indicating that, at least

to a certain extent, results obtained in isolated mito-chondria can be extrapolated to the intact cell Our results reconfirmed the observation that, in isolated rat liver mitochondria, the ANT has limited control over

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