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The in silico GOGAT mutant showed a similar behaviour; its ammonium flux JN was clearly much lower than that of the wild type at low ammonium concentrations, irrespective of the a-KG leve

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assimilation of Escherichia coli: dissection using an

in silico replica

Frank J Bruggeman1, Fred C Boogerd1and Hans V Westerhoff1,2,3

1 Molecular Cell Physiology, Institute of Molecular Cell Biology, CRBCS, Vrije Universiteit, Amsterdam, the Netherlands

2 Mathematical Biochemistry, SILS, Universiteit van Amsterdam, the Netherlands

3 Stellenbosch Institute for Advanced Studies, Stellenbosch, South Africa

Many unicellular organisms exhibit enormous

plasti-city towards sudden changes in their physico-chemical

environment Much of the adaptation capacity derives

from the ‘emergent’ properties of biochemical works composed of signal-transduction, metabolic,and gene-expression regulatory levels [1] Most of the

net-Keywords

ammonium assimilation; systems biology;

glutamine synthetase; robustness; silicon

cell

Correspondence

H.V Westerhoff, Molecular Cell Physiology,

Institute of Molecular Cell Biology, CRBCS,

Vrije Universiteit, de Boelelaan 1085,

NL-1081, HV Amsterdam, the Netherlands

Fax: +31 20 598 7229

Tel: +31 20 598 7230

E-mail: hw@bio.vu.nl

Note

The mathematical model described here has

been submitted to the Online Cellular

Sys-tems Modelling Database and can be

accessed free of charge at http://jjj.

biochem.sun.ac.za/database/Bruggeman/

index.html

(Received 7 October 2004, revised 31

Janu-ary 2005, accepted 23 FebruJanu-ary 2005)

doi:10.1111/j.1742-4658.2005.04626.x

Ammonium assimilation in Escherichia coli is regulated through multiplemechanisms (metabolic, signal transduction leading to covalent modification,transcription, and translation), which (in-)directly affect the activities of itstwo ammonium-assimilating enzymes, i.e glutamine synthetase (GS) andglutamate dehydrogenase (GDH) Much is known about the kinetic proper-ties of the components of the regulatory network that these enzymes are part

of, but the ways in which, and the extents to which the network leads tosubtle and quasi-intelligent regulation are unappreciated To determine whe-ther our present knowledge of the interactions between and the kinetic prop-erties of the components of this network is complete) to the extent thatwhen integrated in a kinetic model it suffices to calculate observed physiolo-gical behaviour) we now construct a kinetic model of this network, based

on all of the kinetic data on the components that is available in the literature

We use this model to analyse regulation of ammonium assimilation at ous carbon statuses for cells that have adapted to low and high ammoniumconcentrations We show how a sudden increase in ammonium availabilitybrings about a rapid redirection of the ammonium assimilation flux fromGS⁄ glutamate synthase (GOGAT) to GDH The extent of redistributiondepends on the nitrogen and carbon status of the cell We develop a method

vari-to quantify the relative importance of the various regulavari-tors in the network

We find the importance is shared among regulators We confirm that the nylylation state of GS is the major regulator but that a total of 40% of theregulation is mediated by ADP (22%), glutamate (10%), glutamine (7%) andATP (1%) The total steady-state ammonium assimilation flux is remarkablyrobust against changes in the ammonium concentration, but the fluxesthrough GS and GDH are completely nonrobust Gene expression ofGOGAT above a threshold value makes expression of GS under ammonium-limited conditions, and of GDH under glucose-limited conditions, sufficientfor ammonium assimilation

ade-Abbreviations

a-KG, a-ketoglutarate; ATase, adenylyltransferase; GDH, glutamate dehydrogenase; GOGAT, glutamate synthase; GS, glutamine synthetase; NRI, response regulator of two-component signal transduction couple NRI ⁄ NRII; NRII, sensor of two-component signal transduction couple NRI ⁄ NRII; UTase, uridylyltransferase.

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adaptation phenomena remain to be explained

mechanistically in terms of the network topology and

the kinetic properties of the molecular components of

the network One possible approach to finding these

explanations is through calculation of the properties of

(parts of) such cellular networks from the

experiment-ally determined properties of the macromolecules

within them, for those cases where these properties are

known sufficiently (e.g [2–5]) Such detailed kinetic

models of parts of living cells have been called ‘silicon

cells’ or ‘silicon replicas’ ([6], see also http://www

siliconcell.net and http://www.jjj.bio.vu.nl) Silicon cells

can be used: (a) to test whether the

molecular-biologi-cal knowledge can account for observed physiologimolecular-biologi-cal

behaviour; (b) to analyse behaviour accounted for; and

(c) to predict behaviour not observed experimentally

(e.g [2–4,7]) Here, we present a silicon cell for the

biochemistry underlying the metabolic regulation of

ammonium assimilation in Escherichia coli

A classical example of a hierarchical regulatory

net-work is the glutamine synthetase (GS) adenylylation

cascade involved in the regulation of ammonium

assimilation of E coli [8–13] It is composed of two

ammonium-assimilatory routes: one through GS⁄

glu-tamate synthase (GOGAT) and one through GDH

(glutamate dehydrogenase) Both lead to the net

reduc-tive addition of ammonium to a-ketoglutarate (KG)

Whereas GDH accomplishes this in a single reaction,

the GS⁄ GOGAT pathway constitutes two reactions

that additionally hydrolyse ATP The affinity of GS

for ammonium (i.e  0.1 mm) is a factor of  10

higher than the affinity of GDH for ammonium (i.e

 1 mm) [14,15] GS ⁄ GOGAT is essential for growth

at low (< 1 mm) ammonium concentrations, when

GDH appears to be redundant GDH might function

in ammonium assimilation when free energy limits

growth and sufficient ammonium is available [16,17]

Furthermore, GDH has been implicated in

osmotoler-ance and pH homeostasis [18]

While growing on glucose and ammonium, as sole

carbon and nitrogen source, respectively, the carbon

skeleton of both glutamate (GLU) and glutamine

(GLN) is derived from catabolism, i.e from a-KG (a

tricarboxylic acid cycle intermediate), and the nitrogen

atom is obtained directly from incorporating

ammo-nium Glutamine (the product of GS) and GLU (the

product of GDH and GOGAT) serve as precursors for

the synthesis of a diverse range of metabolites, i.e

(almost all) amino acids, purine and pyrimidine

nucleotides, glucosamine-6-phosphate, and NAD+

[11] This central role of GLU and GLN at the

inter-section of catabolism and anabolism in E coli led

physiologists and enzymologists to perform detailed

studies on the regulation of the regulatory networkconnected to ammonium assimilation (reviewed in[11–13]) This network proved to harbour a stunningcomplexity, comprising at least five different regulatorymechanisms dedicated to the regulation of ammoniumassimilation through direct effects on the activity ofand amount of GS One mechanism resides in the dif-ference in affinity of GS and GDH for ammonium,rendering GDH more important at high ammoniumconcentrations [15,19] A second mechanism operatesthrough the cumulative feedback control of GS byvarious end products of the GLN- and GLU-demandpathways [20] The third mechanism involves the aden-ylyltransferase (ATase) catalysed inactivation of GSthrough a progressive adenylylation of its 12 subunits[21] The net rates of (de) adenylylation depend on: (a)the concentration of GLN [22]; and (b) the uridylyla-tion state and the a-KG-binding state of the trimericproteins PII [23] and GlnK [24,25] The latter two pro-teins act as substrates for the ambiguous enzyme uri-dylyltransferase (UTase) that can (de) uridylylate allthree subunits of PII [26] and also those of GlnK[24,25] GlnK has recently been shown to be importantunder conditions of nitrogen starvation whereas PII isfunctional at higher concentrations of ammonium [27].All activities of UTase⁄ UR are sensitive to the GLNconcentration Additionally, PII can bind one a-KGmolecule per subunit each having different effects onthe signalling role of PII The fourth mechanisminvolves the transcriptional stimulation of the glnALGoperon, which codes for GS, NRII, and NRI, by thedoubly phosphorylated dimeric response-regulatorNRI The dimeric protein NRII acts as the cognatesensor of the two-component regulatory system NRI-NRII When it binds PII complexed with one molecule

of a-KG, NRII catalyses the dephosphorylation ofphosphorylated NRI [12,28] The fifth mechanism is byregulation of the concentration of GS through proteinturnover (reviewed in [11])

The network as a whole has been postulated to rate and decide upon information concerning the phy-siological carbon and nitrogen status through itssensitivities for ammonium, a-KG, and GLN [12,22,29]

integ-A silicon cell that includes all known kinetic properties

of the macromolecules involved in the five regulatorymechanisms might prove to be the only way to under-stand such complex regulation Provided that the kin-etic properties of the molecules are represented correctly

in the replica, the latter should behave in the same way

as the real pathway With this challenge in mind, wenow construct a silicon cell version of the regulation

of the GS adenylylation cascade, based exclusively onwhat is known about the molecular constituents, i.e on

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all the kinetic data We then analyse the effects of

chan-ges in the ammonium level and in the carbon status

(a-KG) on the transient and short-time steady-state

properties of the ammonium-assimilation flux by the

network When considering such relatively short time

scales, regulation through gene expression can be

assumed to be negligible (e.g [30]) allowing one only to

consider metabolic regulatory processes We devise and

apply a method that determines the relative importance

of the various regulators during transient regulation of

the rate of GS Finally, we alter gene expression of

GDH, GOGAT, and GS and calculate the effects on

the ammonium assimilation flux We observe that the

regulatory network gives rise to a number of regulatory

phenomena that are not present in the constituent

indi-vidual molecules, yet may exemplify much of the basis

for the quasi-intelligent response of the living cell to

changes in its environment

The mathematical model described here has been

sub-mitted to the Online Cellular Systems Modelling

Data-base and can be accessed at http://jjj.biochem.sun.ac.za/

database/Bruggeman/index.html free of charge

Results

The ammonium assimilation network in silico:

biochemical and physiological aspects

The silicon cell version of the ammonium assimilation

network in E coli was constructed from existing

litera-ture data on the kinetic and physicochemical properties

of its components (Experimental procedures) The

inter-action network is shown in Fig 1 The model

incorpor-ates the kinetic data known for the central proteins

(GS, GOGAT, GDH, ATase, UTase, PII) The kinetic

parameter values derive from in vitro measurements in

cell-free extracts or with purified proteins, except for

the kinetic parameters of ATase The latter parameters

were obtained from fitting them to adenylylation states

of GS as function of GLN and a-KG levels in a

recon-stituted system containing only ATase, UTase, PII and

GS (with constant concentrations of a-KG and GLN)

(Experimental procedures) We emphasize that we did

not fit to systemic behaviour as a whole: all behaviour

we calculate here results from the properties of the

com-ponents rather than from a fit Also the physiological

boundary conditions, e.g moiety conserved totals, were

obtained from the literature The silicon cell employed

simple modular kinetics for the reactions outside the

ammonium assimilation pathway itself, such as amino

acid synthesis of amino acids derived from GLU and

GLN A detailed description of the kinetic model can

be found in the Supplementary material

The three gln regulatory genes are expressed tively at a low level [13], suggesting that the intracellularconcentrations of PII, UTase and ATase are independ-ent of nitrogen status Accordingly, the amount of theregulatory protein PII and the activities of UTase, andATase were fixed at levels normally encountered in wildtype E coli cells The expression levels of the genesglnA, gltBD, and gdhA, encoding GS, GOGAT, andGDH, respectively, do depend on the physiological state

constitu-of E coli (e.g [31]) Time-dependent gene expressionwas not taken into account: the replica was meant toreconstruct the short-term metabolic regulation only.Furthermore, the kinetics of the anabolic modules werechosen such that: (a) the net ammonium assimilationfluxes (JN¼ 25–41 mmÆmin)1) were consistent withintermediate specific growth rates of E coli (0.3–0.5 h)1); and (b) the flux via the GLU demand routewas approximately eight times higher than the flux viathe GLN demand route [32] The maximal rates for GS,GOGAT, and GDH used in the calculations below weredetermined with wild type E coli growing at a specificgrowth rate of 0.3 h)1 in an ammonium-limited or aglucose-limited chemostat (Table 1)

The ammonium assimilation network in silico –partial validation

No comprehensive physiological studies of the nium assimilation network under controlled conditionsthat could serve as a full validation of the model could

ammo-be found in the literature Therefore, we choose tocompare the in silico behaviour of the wild type andmutants (obtained by removing the correspondingreactions) to the reported physiology of the corres-ponding real wild type and mutant strains Unfortu-nately, the type of physiological experiments carriedout to determine the physiology of mutants is semi-quantitative at best In the cases used in this sectionnone of them included measurements of the maximalrates at the used physiological conditions This meansthat the physiological behaviour of the mutants in vivoand in silico can be compared in a qualitative senseonly The steady states of the in silico wild type andmutants were calculated for four different ‘physiologi-cal’ conditions, i.e at a low (0.05 mm; Table 2) and at

a high (1.0 mm; Table 3) intracellular ammonium centration, each for two a-KG concentrations (0.2 and1.0 mm) These a-KG concentrations represent the lowand high end of the reported physiological range ofintracellular concentrations [31]

con-The following experimentally obtained physiologicaldata (a–d) are qualitatively consistent with the simula-ted in silico data shown in Tables 2 and 3 (a) Under all

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conditions, the calculated wild type steady-state GLNconcentration (0.6–1.0 mm) proved to be at least oneorder of magnitude lower than the calculated GLUconcentration (4.0–21 mm) This reproduces the con-centration ranges and the relationship that has beenobserved frequently in vivo [31,33–35] (b) As expectedfor the wild type, at glucose limitation the in silico GSwas adenylylated to a higher degree than for the condi-tions mimicking ammonium limitation Accordingly,ammonium assimilation ran predominantly via GS dur-ing ammonium limitation whereas GDH dominatedduring glucose limitation The ammonium assimilation

Fig 1 Reaction scheme of the metabolic ammonium-assimilation network in E coli Subnetworks (UTase, ATase, metabolism), defined such that there is no mass flux between them, are enclosed in dashed boxes Metabolites are denoted in upper case letters Boundary metabolites (with concentrations held constant) are denoted

by white letters in grey boxes Dashed arrows portray the regulatory interconnec- tions between the subnetworks governed

by the communicating intermediates that are displayed outside of the dashed boxes Full arrows represent the rates, which are further characterized by vj’s (where j denotes the enzyme abbreviation) Activa- tors and inhibitors are depicted in bold and plain format below or above the process rates they regulate ATPase stands for the cellular free-energy pathways that re-phos- phorylate ADP The following abbreviations were used: UT, uridylyl transfer; UR, uridylyl removal; DEAD, deadenylylation; AD, ade- nylylation; GS, glutamine synthetase; GDH, glutamate dehydrogenase; GOGAT, gluta- mate synthase; GLNDEM, glutamine demand; GLUDEM, glutamate demand; NH, ammonium; KG, a-KG; GLU, glutamate; GLN, glutamine; MET GLN , metabolite derived from glutamine; and METGLU, meta- bolite derived from glutamate.

Table 1 Measured maximal rates of GS, GOGAT and GDH

deter-mined for E coli K12 growing at a dilution rate of 0.3 h)1 in an

ammonium-limited and glucose-limited chemostat All maximal

rates are in m M Æmin)1.

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fluxes are comparable under the two conditions (this

illustrates growth at comparable growth rates) (c)

Experimental cells lacking GOGAT show unimpaired

growth at high ammonium concentrations Only under

nitrogen-limitation they grow more slowly [36] The

in silico GOGAT mutant showed a similar behaviour;

its ammonium flux (JN) was clearly much lower than

that of the wild type at low ammonium concentrations,

irrespective of the a-KG level At the higher

ammo-nium concentration the silicon GOGAT deletion cells

did assimilate ammonium at a substantial rate, again

consistent with the experimental result (d) Mutants

lacking GDH have no obvious growth impairment

when both free energy and carbon are available in

excess [17,32] In agreement with this experimental

observation, the silicon GDH deletion mutant

sus-tained a high ammonium-assimilation flux during

ammonium-limited growth (e) Cells of Salmonella

typhimurium devoid of ATase and induced for GS

expression accumulate GLN to high levels under high

ammonium conditions, even after the initially depleted

GLU pool has been restored [37,38] This is indeed

cal-culated for the in silico pathway for the case of glucose

limitation (f) Experimental mutants lacking UTaseexhibit a high adenylylation state of GS independent ofthe absence or presence of ammonium in the medium[39,40]; they are not able to sense changes in the nitro-gen status (they sense nitrogen all the time) Likewise,

GS was adenylylated to a substantial extent in the

in silicoUTase mutant growing at two limitations

An in silico PII mutant was not included, because theinterpretation of the phenotypes of experimental PIImutants is confounded by the presence of the PII para-logue, GlnK, in these mutants [41] The in silico mutantstrain deficient in GS did engage in ammonium assimil-ation but its GLN production flux was zero (Tables 2and 3) In reality such a mutation is indeed lethal due tothe fact that GS is the sole enzyme capable of producingGLN

Steady-state response to changes in ammoniumconcentration

The effects of the external nitrogen and internal carbonand nitrogen status on the metabolic regulation ofthe ammonium assimilation flux were investigated The

Table 2 Calculated steady-state in silico physiology of wild type and of mutant E coli strains in the presence of 0.05 m M ammonium (ammonium-limited chemostat) and 0.2 (A) or 1.0 (B) m M a-KG The values for the maximal rates were 360 m M Æmin)1(GDH), 600 m M Æmin)1(GS), and 85 m M Æmin)1(GOGAT).

Genotype

GLN

(m M )

GLU (m M )

n AMP (AMPÆGS)1)

J GS (m M Æmin)1)

J GDH (m M Æmin)1)

J N (m M Æmin)1)

a Initial conditions: PII ¼ 0.003 m M , PIIUMP i ¼ 0.000 m M (i ¼ 1,2,3).

Table 3 Calculated steady-state in silico physiology of wild type and of mutant E coli strains in the presence of 1.0 m M ammonium cose-limited chemostat) and 0.2 (A) or 1.0 (B) m M a-KG The values for the maximal rates where 205 m M Æmin)1(GDH), 110 m M Æmin)1(GS), and 55 m M Æmin)1(GOGAT).

(glu-Genotype

GLN

(m M )

GLU (m M )

n AMP (AMP GS)1)

J GS (m M min)1)

J GDH (m M Æmin)1)

J N (m M Æmin)1)

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external nitrogen and the internal carbon and nitrogen

status were taken to be reflected by the ammonium,

a-KG, and the GLN concentration, respectively

Meta-bolic steady states were computed at internal

ammo-nium concentrations ranging from 0.01 to 1 mm, while

the a-KG concentration was either set to 0.2 or to

1.0 mm The calculations were performed for cells that

had expression levels of GS, GDH, and GOGAT that

mimicked long exposure to ammonium limitation, i.e

identical conditions to those in Table 2 All calculations

involved metabolic steady states that had been reached

within minutes after cells) incubated for generations at

ammonium limitation (i.e 0.05 mm ammonium)) had

been shifted to the ammonium concentration indicated

on the abscissa of Fig 2 The computed steady states

thus reflect metabolic states reached before enzyme

syn-thesis or degradation could have had any effect The

range of a-KG concentrations was again chosen to

mimic the physiological concentrations range [31]

The steady-state relationship between the overall

ammonium-assimilation flux (JN) and the ammonium

concentration for two different a-KG concentrations is

shown in Fig 2A,B Irrespective of the a-KG

concentra-tions, JNincreased sharply with the ammonium

concen-tration as long as the latter stayed below  0.03 mm

Above this ammonium concentration the dependence of

the ammonium assimilation flux on the ammonium

con-centration changed drastically: the ammonium

assimil-ation flux increased only slightly with a further increase

in ammonium concentration Below the threshold, the

metabolic regulation appeared to fail, in view of the

sharp drop in JNwith even a minor decrease in

ammo-nium Our calculations suggest that the expression of

the ammonium transporter AmtB may be necessary to

sustain ammonium assimilation at ammonium

concen-trations below this threshold

To investigate which regulatory mechanism acting on

GS has the highest effect on the dependency of the

ammonium assimilation flux on the ammonium

concen-tration we removed three such mechanisms The

ammo-nium assimilation flux in the insets of Fig 2A,B

corresponds to the three different models in which the

direct regulation of GS is ‘mutated’ by removal of the

terms from the rate equation of GS that correspond to:

(a) thermodynamic regulation; (b) kinetic regulation;

and (c) both thermodynamic and kinetic regulation

Removal of thermodynamic regulation corresponds to

neglecting the inhibitory effect of the backward

reac-tion of GS on the rate of biosynthetic ammonium

assimilotion (by deleting the term [ADP][GLN][Pi]⁄

Keq,GS from Eqn 19a) The kinetic effect was removed

by abolishing both the effect of adenylylation on the

maximal rate of GS (the JGSterm on Eqn 19a and b

was set to 1) and by eliminating the product inhibitionterms, e.g ADP⁄ KADP To enable a fair comparison,the maximal rate of GS in the ‘mutated’ models wascorrected such that the net ammonium assimilation flux(JN) of the mutated and the original model was identi-cal at 0.05 mm of ammonium (i.e 32 and 37 mmÆmin)1,respectively, at 0.2 and 1.0 mm a-KG) Clearly, bothinsets indicate that the effect of the removal of bothregulatory mechanisms (but not of either alone) on theammonium assimilation flux was drastic, i.e at 1.0 mma-KG, JN now increased from 47 at 0.02 mm ammo-nium to 160 mmÆmin)1at 1.0 mm (The value for the JN

at 1.0 mm ammonium in the case for removal of thekinetic and thermodynamic regulation was 69 and

47 mmÆmin)1, respectively.)Ammonium assimilation is thought to be associatedwith high activities of GS and GOGAT at low concen-trations of ammonium (< 1 mm) and no activity ofGDH, whereas GDH is presumed to carry the fluxexclusively at higher concentrations of ammonium [11].This has been postulated to be favourable because ofthe additional hydrolysis of one ATP per molecule ofammonium assimilated if the GS⁄ GOGAT pathway isused [17] To investigate whether the shift from GS⁄GOGAT to GDH should actually be expected on thebasis of known kinetics and of metabolic regulationalone, the relative contributions of GS and GDH to thenet ammonium assimilation flux were calculated as afunction of the ammonium concentration, again for thetwo different concentrations of a-KG (Fig 2C,D).Contrary to the expectations, GDH was calculated to

be active at low ammonium concentrations Even at theammonium level that maximally supported GS activity(0.03 mm), GDH activity contributed 12% to theammonium assimilation flux (at 1.0 mm a-KG) Therelative contribution of GS increased strongly withincreasing ammonium concentrations before it wentthrough a maximum of 88% at 0.03 mm ammonium.Hereafter, the contribution of GS decreased, quickly atfirst and then slowly, to settle to a plateau value of 20%(for 1.0 mm a-KG) for ammonium in excess of 1 mm(data not shown) The heights of both the peak in thedependence of the variation of the relative contribution

of the two enzymes on the ammonium concentrationand, to a lesser extent, the minimum plateaus, decreasedwith an increase in the a-KG concentration Remark-ably, Fig 2C shows that, at a low a-KG concentration,even at an ammonium concentration exceeding 1 mm,

GS contributed significantly to the overall ammoniumassimilation (43% at 1.0 mm NH4+and 0.2 mm KG).The strict paradigm of ammonium assimilation fluxthrough GS at low and through GDH at high ammo-nium concentrations should perhaps be replaced by the

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Fig 2 Calculated, steady-state characteristics of the ammonium assimilation network as function of the ammonium concentration at two a-KG concentrations, i.e 0.2 (A, C, E, G), and 1.0 (B, D, F, H) m M ; AB, overall ammonium assimilation flux (J N ); CD, flux ratio of GS and GDH (JGS⁄ J GDH ); EF, apparent maximal rate of GS (V APP

GS ) and the adenylylation state of glutamine synthetase (nAMP); GH, the concentration of PII with one a-KG attached to it (PIIKG 1 ), of PII saturated with both UMP and KG (PIIUMP 3 KG 3 ), and of glutamine (GLN) The numbered lines in the insets of (A) and (B) correspond to the removal of thermodynamic regulation (1), kinetic regulation (2), and both (3) In order to guarantee identical ammonium assimilation fluxes of the original and the mutated model at 0.05 m M ammonium, the fluxes in the insets were calculated with the following values for the maximal rates of GS (in m M min)1), 555 (1, inset A), 160 (2, inset A), 160 (3, inset A), 550 (1, inset B), 140 (2, inset B), 140 (3, inset B).

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subtler picture emerging from what we calculated here

on the basis of the properties of the participating

enzymes The general perception that all ammonium

assimilation at high ammonium concentrations follows

the energetically cheaper route along GDH, is not

sup-ported by the known kinetic properties of the pathway

Indeed it is well known that microorganisms are not

generally efficient free-energy transducers [42]

The contribution of GS to the nitrogen assimilation

flux was smaller at the high a-KG concentration (24%

at 1.0 mm NH4+) This indicates that GS may not

only play a role at low external ammonium conditions

but also at low internal carbon conditions Indeed, not

only does the enzyme couple GS⁄ GOGAT have a

higher affinity for ammonium than GDH, it also has a

higher affinity for a-KG, i.e the KM values of GDH

and GOGAT for a-KG are 0.3 mm and 7 lm,

respect-ively Apparently, GS⁄ GOGAT not only senses the

internal nitrogen status (GLN) but, additionally, the

internal carbon status

The concentrations of GLN and PIIKG1(the form of

the signalling protein PII that binds to the sensor NRII

activating the phosphatase activity of the latter towards

NRIP) increased steadily with the ammonium

concen-tration above 0.03 mm The extent of the increase in the

concentration of PIIKG1 depended on the a-KG

con-centration (Fig 2G,H) At 1.0 mm ammonium and

1.0 mm a-KG, its concentration amounted to 22 nm,

which represented 0.7% of the total amount of PII

pre-sent (3 lm) An increased concentration of PIIKG1

implies an increased rate of NRII-PIIKG1-catalysed

dephosphorylation of NRIP and hence a decrease in the

expression level of GS The physiological concentration

of NRII (assuming it is comparable to the

concentra-tion of NRI) is between 1 and 2 nm for cells grown in

the presence of excess ammonium and it may rise to

> 60 nm in cells grown at low nitrogen conditions

[42a] Therefore, especially at high concentrations of

a-KG, where the contribution of GS to JN was

relat-ively low (Fig 2D), gene expression of GS may be down

regulated by PIIKG1 The concentration of the other

regulatory PII intermediate, i.e PIIUMP3KG3,

decreased with increasing ammonium concentrations,

but increased with increasing a-KG concentrations

These two species reflect the decrease in the overall

uridylylation state of PII as a function of increasing

ammonium concentration (data not shown)

Transient response to a sudden increase

in ammonium availability

Schutt and Holzer [43] measured a rapid decrease in

the apparent maximal rate of GS (its maximal rate

corrected for its adenylylation state) upon a suddenincrease in the ammonium concentration to cells thathad been adapted to growth on proline, i.e to the vir-tual absence of ammonium They stopped short ofdetermining the actual composite rates of ammoniumassimilation and of confirming that the system shiftedbetween rates as effectively as often hypothesized.Inspired by this work, we subjected the silicon net-work, adapted to ammonium limitation as reflected inthe values of the maximal rates of GS, GDH and GO-GAT and at the reference steady state used previously(i.e an ammonium concentration of 0.05 mm), to asudden increase in the ammonium concentration to1.0 mm To investigate the effect of the carbon status

we performed the calculations at constant trations of both 0.2 and 1.0 mm of a-KG (Fig 3)

concen-At low concentrations of ammonium and a-KG,

in silico ammonium assimilation ran predominantly via

GS⁄ GOGAT (Figs 3A and 2C) Upon the 20-foldincrease in the ammonium concentration at time zero,the rate of GS (and GDH) initially increased rapidly,

as expected from the increase in the concentration ofone of their substrates After a few seconds the ratesbegan to decrease Eventually the (steady-state) GSrate dropped to a level lower than before the addition

of the ammonium, in spite of the 20-fold increasedconcentration of one of its substrates Figure 3C illus-trates that the decrease in the rate of GS correlatedwith a decline in its apparent maximal rate (to  10%

of its preshift value) This in turn correlated with the(rapid) adenylylation of nearly all subunits of GS(from 1.2 to 11 AMP⁄ GS) within 3 min Within a min-ute after the ammonium shift, the GLN concentrationincreased rapidly to finally settle down to a highersteady state than before the ammonium change(Fig 3E) The progressive adenylylation of GS resultedfrom two effects both caused by the rapid increase ofthe GLN concentration Firstly, GLN itself may havedirectly stimulated the ATase-catalysed adenylylationreaction Secondly, GLN interacts with UTase andmay hereby have increased the level of PIIKG1 anddecreased the level of PIIUMP3KG3 (Fig 3E), givingrise to both a further stimulation of the ATase-cata-lysed adenylylation reaction and a release of the stimu-lation of the ATase-catalysed deadenylylation reaction

Effects of mutations on the transient response

of the network

To obtain a more detailed picture of the contribution ofthe different proteins involved in the regulation of theshift from GS- to GDH-dominated ammonium assimil-ation upon an increase in the ammonium concentration,

Trang 9

we removed ATase, UTase, and PII from the model.

We performed these in silico experiments at an a-KG

concentration of 1.0 mm, i.e the conditions where the

shift was most appreciable (Supplementary Figs S1–

S3) These ‘deletions’ took place at the moment of the

addition of ammonium to make sure that the initial

conditions at the moment of the addition were similar

to those in Fig 3B This illustrates the potential power

of silicon cells; here we calculate the outcome of an

experiment not achievable in the laboratory Theremoval of ATase caused an accumulation of GLN (to

67 mm within 5 min after the pulse) (SupplementaryFig S1) Most importantly, in this simulated absence ofthe regulation through ATase, GS contributed 44% tothe ammonium assimilation rate 5 mins after the addi-tion of ammonium Similarly, in order to investigate therole of UTase in regulating the maximal rate of ATase

we removed UTase from the model (Supplementary

Fig 3 Calculated transient response to a sudden increase in the ammonium concentration from 0.05 to 1.0 m M at time zero The a-KG centration was 0.2 m M (panels A, C, and E), or 1.0 m M (panels B, D and F) continuously A, B: rates of glutamine synthetase (vGS), glutam- ate synthase (vGOGAT) and glutamate dehydrogenase (vGDH) C, D: adenylylation state of glutamine synthetase (nAMP) and the ‘apparent’ maximal rate of glutamine synthetase (V APP

con-GS ) E, F: concentrations of glutamine (GLN), PII with one a-KG attached to it (PIIKG1), and PII saturated with UMP and a-KG (PIIUMP3KG3).

Trang 10

Fig S2) Removal of UTase led to (relative to the wild

type): (a) an increased steady-state concentration of

GLN; (b) a similar adenylylation state and apparent

maximal rate of GS; and (c) comparable rate changes in

GS, GOGAT and GDH Apparently, GLN can take

over the regulatory role of PIIKG1 and PIIUMP3KG3

after the pulse (Of course, removal of UTase is likely

to have important effects on the regulation of

ammo-nium assimilation due to its second regulatory role, i.e

hierarchical regulation of the activity of the

two-compo-nent signalling network NRI⁄ NRII through its directs

effect on the concentration of PIIKG1, but gene

expres-sion regulation is not considered here)

Do these results hint at PII being redundant for

metabolic ammonium assimilation: can GLN

substi-tute for PII? This we investigated by removing PII

from the model at the moment the 1 mm ammonium

was added (Supplementary Fig S3) PII turned out to

be of major importance; its removal led to an

accumu-lation of GLN and to total deadenylyaccumu-lation of GS

(causing its apparent maximal rate to rise to its

max-imal value of 600 mmÆmin)1) As in the case of the

removal of ATase, PII removal interfered with the

shift from GS⁄ GOGAT- to GDH-dominated

ammo-nium assimilation This may have been due to the

synergistic effect of PIIKG1, PIIUMP3KG3 and GLN

on the rate of ATase (Eqns 15b and 16b)

These results indicate that the interplay between

GS⁄ GOGAT and GDH critically depends on the

sig-nalling cascade composed of both ATase and PII,

UTase being perhaps more important as a hierarchical

regulatory mediator Additionally, the calculated

results of PII removal indicated that ATase alone may

be insufficient for regulating the level of ammonium

assimilation upon an ammonium pulse

Analysis of regulation of the transient response

of the GS rate

The decrease in the rate of GS upon the sudden addition

of ammonium at time zero (Fig 3A,B) is a result of the

regulatory network as a whole For, in the metabolic

subnetwork alone, the rate of GS should have increased

upon the addition of ammonium (as exemplified by the

results obtained in silico after the removal of ATase

(Supplementary Fig S1) The change in the rate of GS

could be caused by the changes in: its state of covalent

modification (nAMP), and the concentrations of

sub-strates (GLU; ATP) and products (GLN; ADP) There

was no method available yet however, to analyse the

relative importance of these various regulatory routes

These regulatory influences could well depend on time,

making such an analysis even more complicated

To test whether the adenylylation of GS is indeedthe most important regulatory event to downregulatethe flux of GS upon a rise in the ammonium level, weset out to develop an in silico method that shouldenable us to quantify the relative strengths of parallelregulatory pathways as a function of time To this aim

we wrote the fractional change in the rate of GS attime t as follows:

dlnvGS

dt ðtÞ¼

X5 i¼1

HvGS

X i ðtÞ ð1Þ

where the sum was taken over the regulatory butions of all five regulators (denoted by Xi) Theregulator with the highest regulatory contribution(HvGS

contri-X i for the regulatory contribution of Xi on therate of GS) at time t has the highest contribution tothe change in the rate of GS at that moment in time.After integrating over the entire steady-state relaxa-tion time, one then obtains for the average regulatorycontribution of Xið HvGS

X i Þ:

1t

Zt 0

d ln vGS

dt ðsÞ ds

¼X5 i¼1

1t

Zt 0

@ln vGS

@ln XiðsÞ d ln Xi

dt ðsÞ ds ¼

X5 i¼1



HvGS

Similarly, the average absolute regulatory contribution

of a regulator Xi to transient regulation of vGS over atime span 0 to t should be given by

H

 vGS

Xi ¼1t

Z t 0

HvGS

Xi ðsÞ

In Supplementary Fig S4 the regulatory contributions

of the five regulators are displayed for the changes inthe rate of GS that were shown in Fig 3 Supplement-ary Fig S4 indicates that initially (seconds) ADP,ATP, GLN, GLU, and nAMP (in decreasing order ofimportance) were important regulators, after that (sec-onds to minute) GLU and nAMP, and at a later stage(minutes) nAMP was most important The integratedregulator contributions can be found in Table 4 In theaverage regulatory contribution up- and downregula-tion are included: negative and positive effects are justsummed up over time A more interesting variable istherefore the average absolute regulatory contribution:here negative effects are integrated, turned into posit-ive values and summed up with positive effects It isnoteworthy that the average regulatory contributions

of ATP and ADP have the same sign, even though theyare an activator and an inhibitor of GS, respectively.This is explained by the definition of the regulatory

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