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Characterization of isocitrate dehydrogenase from the green sulfurA carbon dioxide-fixing enzyme in the reductive tricarboxylic acid cycle Tadayoshi Kanao, Mineko Kawamura, Toshiaki Fuku

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Characterization of isocitrate dehydrogenase from the green sulfur

A carbon dioxide-fixing enzyme in the reductive tricarboxylic acid cycle

Tadayoshi Kanao, Mineko Kawamura, Toshiaki Fukui, Haruyuki Atomi and Tadayuki Imanaka

Department of Synthetic Chemistry and Biological Chemistry, Graduate School of Engineering, Kyoto University, Yoshida-Honmachi, Sakyo-ku, Kyoto, Japan

Isocitrate dehydrogenase (IDH) catalyzes the reversible

conversion between isocitrate and 2-oxoglutarate

accom-panied by decarboxylation/carboxylation and

oxidoreduc-tion of NAD(P)+cofactor While this enzyme has been well

studied as a catabolic enzyme in the tricarboxylic acid (TCA)

cycle, here we have characterized NADP-dependent IDH

from Chlorobium limicola, a green sulfur bacterium that fixes

CO2through the reductive tricarboxylic acid (RTCA) cycle,

focusing on the CO2-fixation ability of the enzyme The gene

encoding Cl-IDH consisted of 2226 bp, corresponding to a

polypeptide of 742 amino acid residues The primary

struc-ture and the size of the recombinant protein indicated that

Cl-IDH was a monomeric enzyme of 80 kDa distinct from

the dimeric NADP-dependent IDHs predominantly found

in bacteria or eukaryotic mitochondria Apparent Michaelis

constants for isocitrate (45 ± 13 lM) and NADP+

(27 ± 10 lM) were much smaller than those for

2-oxoglut-arate (1.1 ± 0.5 mM) and CO2(1.3 ± 0.3 mM) No signif-icant differences in kinetic properties were observed between Cl-IDH and the dimeric, NADP-dependent IDH from Saccharomyces cerevisiae(Sc-IDH) at the optimum pH of each enzyme However, in contrast to the 20% activity of Sc-IDH toward carboxylation as compared with that to-ward decarboxylation at pH 7.0, the activities of Cl-IDH for both directions were almost equivalent at this pH, suggesting

a more favorable property of Cl-IDH than Sc-IDH as a

CO2-fixation enzyme under physiological pH Furthermore,

we found that among various intermediates, oxaloacetate was a competitive inhibitor (Ki ¼ 0.35 ± 0.04 mM) for 2-oxoglutarate in the carboxylation reaction by Cl-IDH, a feature not found in Sc-IDH

Keywords: isocitrate dehydrogenase; reductive tricarboxylic acid cycle; CO2-fixing enzyme

The reductive tricarboxylic acid (RTCA) cycle is a carbon

dioxide (CO2) fixation pathway distinct from the

well-known reductive pentose phosphate cycle (Calvin–Benson

cycle) in plants, algae, and various bacteria In this pathway,

four molecules of CO2are fixed to produce one molecule of

oxaloacetate in one cycle It has been suggested that the

RTCA cycle functions in anaerobic bacteria Chlorobium [1]

and Desulfobacter [2], thermophilic bacteria

Hydrogeno-bacter [3] and Aquifex [4], and also in the thermophilic

archaeon Thermoproteus [4] The key enzymes of the RTCA

cycle are ATP-citrate lyase, and four CO2-fixing enzymes:

pyruvate synthase, phosphoenolpyruvate carboxylase,

2-oxoglutarate synthase, and isocitrate dehydrogenase

(IDH) As IDH is not specific for the RTCA cycle and is

widely distributed as a member of the tricarboxylic acid (TCA) cycle, this enzyme has been extensively characterized

in terms of its contribution to the TCA cycle in various species, including aerobic bacteria [5], facultative anaerobic bacteria [6], archaea [7], yeast [8], plants [9], and mammalian tissues [10] [11]

IDH in the TCA cycle catalyzes the oxidative decarb-oxylation of isocitrate to 2-oxoglutarate coupled with the reduction of NAD(P)+ The IDH reaction is not only an oxidation step in the cycle for generation of reducing power but also provides 2-oxoglutarate as an important inter-mediate for glutamate biosynthesis Indeed, deficiency of this enzyme in Escherichia coli resulted in the auxotrophy for glutamate [12] IDH also comprises the branching point between TCA cycle and glyoxylate cycle along with isocitrate lyase In E coli and related bacteria grown on C2 carbon sources, IDH is phosphorylated by the function

of IDH kinase/phosphatase, that leads to inactivation of the enzyme and consequent switch of the carbon flux from TCA cycle to glyoxylate cycle [13] [14]

There are two kinds of IDH with different cofactor dependency, NAD- and NADP-dependent IDHs Eukary-otes possess both IDH isozymes, where NAD-dependent enzymes are a4b4heterooctamers localized in mitochondria

to function in the TCA cycle, while NADP-dependent IDH activities have been detected in the cytosol, peroxisomes, and mitochondria It has been suggested that the eukaryotic NADP-IDHs provide NADPH and 2-oxoglutarate for biosynthesis of fatty acids and amino acids [9] In contrast,

Correspondence to T Imanaka, Department of Synthetic Chemistry

and Biological Chemistry, Graduate School of Engineering,

Kyoto University, Yoshida-Honmachi, Sakyo-ku, Kyoto 606-8501,

Japan Fax: + 81 75 7534703, Tel.: + 81 75 7535568,

E-mail: imanaka@sbchem.kyoto-u.ac.jp

Abbreviations: RTCA cycle, reductive tricarboxylic acid cycle; IDH,

isocitrate dehydrogenase; idh, the gene encoding isocitrate

dehydro-genase; Cl-IDH, isocitrate dehydrogenase from Chlorobium limicola;

Sc-IDH, NADP-dependent isocitrate dehydrogenase from

Sacchar-omyces cerevisiae; IPTG, isopropyl thio-b- D -galactoside.

Enzyme: isocitrate dehydrogenase (EC 1.1.1.42).

(Received 11 December 2001, revised 18 February 2002, accepted 20

February 2002)

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bacteria possess only NADP-dependent IDH These

bacte-rial and eukaryotic NADP-dependent IDHs are usually

dimeric in structure, consisting of identical subunits with

molecular masses ranging from 40 to 57 kDa [9] [15] In

addition to these enzymes, a limited number of monomeric

IDHs with molecular masses of  80 kDa have been

identified from Azotobacter vinelandii [16], Vibrio

parahaemolyticus [17], Rhodomicrobium vannielii [18],

Desulfobacter vibrioformis [19], and Corynebacterium

glutamicum [20] Psychrophilic Vibrio sp strain ABE-1

possesses structurally distinct IDH isozymes of

homodi-meric (IDH-I) and monohomodi-meric (IDH-II) structures [21] The

genes of monomeric IDHs have been cloned and sequenced

from Vibrio sp ABE-1 [22] and Cr glutamicum [23], and

putative monomeric IDH genes have been identified on the

chromosomes of Chlorobium tepidum, Pseudomonas

aeru-ginosa, Mycobacterium leprae, and Neisseria meningitidis

Comparison of the primary structures revealed little

overall similarity between these two types of

NADP-dependent IDHs [20] [23]

We have previously isolated the green sulfur bacterium

Chlorobium limicolastrain M1, and have characterized one

of the key enzymes of the RTCA cycle, ATP-citrate lyase

[24] The results demonstrated the heteromeric structure of

this enzyme and its role in regulating the direction and flux

of the RTCA cycle For further understanding of the RTCA

cycle, we are carrying out detailed investigations of each

member of the cycle With respect to IDH, although the

activities have been detected in some autotrophic organisms

utilizing the RTCA cycle, no biochemical analysis of the

enzyme has been reported Furthermore, the catalytic

properties of IDH for the reductive carboxylation are much

less studied in comparison with those for the oxidative

reaction

In this report, we isolated the gene encoding IDH from

C limicola (Cl-IDH) and characterized the recombinant

Cl-IDH as a CO2-fixing enzyme, and compared the catalytic

properties of Cl-IDH with those of dimeric

NADP-depen-dent IDH from Saccharomyces cerevisiae having different

physiological functions

M A T E R I A L S A N D M E T H O D S

Bacteria, plasmids, and media

The green sulfur bacterium C limicola strain M1 was grown

phototrophically at 30°C as described previously [24]

E coliDH5a and pUC118 were used for DNA

manipu-lation and sequencing E coli BL21(DE3) (Stratagene, La

Jolla, CA, USA) was used as a host for an expression

plasmid derived from pET21a(+) (Novagen, Madison, WI,

USA) These strains were cultivated in Luria–Bertani

medium at 37°C When necessary, 50 lgÆmL)1ampicillin

was supplied into the medium to maintain plasmids

Isolation of the IDH gene (idh) from C limicola

Construction of a genomic DNA library of C limicola M1

has been described previously [24] A partial DNA fragment

of idh was amplified from C limicola genomic DNA by

PCR using two primers corresponding to highly conserved

regions among monomeric IDHs One primer (5¢-CAYC

TSAARGCNACSATGATG-3¢, N:A/T/G/C, Y:C/T,

S:G/C, R:A/G) was designed from HLKATMM from position 251–257, and the other primer (5¢-AAYTGYTG NACRTGYTTNGGNGC-3¢) was a complementary sequence of MAQKAEE from position 409–415 in mono-meric IDH from Cr glutamicum, respectively A phage clone carrying the complete Cl-idh gene was screened from the genomic library by plaque hybridization using the amplified DNA fragment as a probe A BamHI and SalI restriction fragment containing the idh gene and its flanking regions (6.0 kbp) was subcloned into pUC118

DNA manipulation and sequencing DNA manipulation was carried out according to the methods described by Sambrook & Russell [25] Prepara-tion of plasmid DNA was performed with Plasmid Mini-and Midi-Kits (Qiagen, Hilden, Germany) along with the alkaline extraction method [25] Nucleotide sequences of both DNA strands were determined using a BigDye Terminator Cycle Sequencing FS Ready Reaction Kit and

a Model 310 capillary DNA sequencer (Applied Biosystems, Foster City, CA, USA) The multiple alignment of protein sequences and the identity and similarity between sequences were obtained with the programALIGNcontained within the

CLUSTALWprogram provided by DNA Data Bank of Japan (DDBJ) The sequence data was analyzed usingGENETYX

software package (Software Development, Tokyo, Japan) The nucleotide sequence data of Cl-idh will appear in the EMBL, GenBank, and DDBJ nucleotide sequence data-bases under accession no AB076021

Expression ofC limicola idh gene and purification

of the recombinant enzyme

In order to construct an expression vector for Cl-idh, two oligonucleotides (sense, 5¢-AAAAACATATGGCAAGCA AATCGACCATCATCTACAC-3¢, and antisense, 5¢-AAA AAGGATCCCGGCTGAAAACCGGGCTGCATTA-3¢) were designed for amplification of idh flanked with NdeI and BamHI sites (underlined) After confirming the nucle-otide sequence, an NdeI–BamHI fragment of the amplified idhgene was ligated with pET21a(+) at the corresponding sites The expression vector, named pET-IDH, was intro-duced into E coli BL21(DE3), and the recombinant cells were cultured in Luria–Bertani medium containing

50 lgÆmL)1ampicillin at 37°C Expression of idh in the recombinant cells under the control of T7 promoter was induced for 3 h at 37°C after the addition of 0.1 mM

isopropyl thio-b-D-galactoside (IPTG) when D660 ¼ 0.4 The cells harvested from a 3-L culture were washed twice with 0.1M potassium phosphate buffer (pH 7.2), and resuspended in the same buffer The cells were disrupted

by sonication on ice, and then centrifuged for 15 min at

15 000 g to remove cell debris The soluble fraction was applied onto a Resource Q anion exchange column (Amer-sham Pharmacia Biotech, Uppsala, Sweden) by using an A¨KTA explorer 10S apparatus (Amersham Pharmacia Biotech) After equilibrating and washing with 20 mM

potassium phosphate buffer (pH 7.2), Cl-IDH was eluted

by a linear gradient of KCl (0–0.5M) in the same buffer with

a flow rate of 2 mLÆmin)1 The active fraction was concentrated and further applied onto a Superdex200 HR10/30 gel-filtration column (Amersham Pharmacia

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Biotech) at a flow rate of 0.35 mLÆmin)1 All purification

steps were carried out at 4°C The active fractions were

examined for apparent homogeneity by SDS/PAGE

Pro-tein concentration was determined by a Bio-Rad ProPro-tein

Assay system (Bio-Rad, Hercules, CA, USA) with bovine

serum albumin as a standard

Enzyme assays

Activities of Cl-IDH and NADP-dependent dimeric IDH

from S cerevisiae (Oriental Yeast, Osaka, Japan) were

determined spectrophotometrically at 25°C In the

decarb-oxylic reaction, the assay mixture contained 0.4 mM

triso-diumDL-isocitrate, 0.2 mM NADP+, 40 mM MgCl2, and

enzyme solution in 1 mL of 100 mM

2-(cyclohexylamino)-ethanesulfonic acid (Ches) buffer (pH 9.0) The increase of

NADPH was detected by absorbance at 340 nm, and one

unit of activity was defined as 1 lmol of NADPH formed

per min In the carboxylation reaction, the mixture was

composed of 8 mM sodium 2-oxoglutarate, 0.16 mM

NADPH, 40 mM MgCl2, 35 mM NaHCO3, and enzyme

solution in 1 mL of 100 mM

N-2-hydroxyethylpiperazine-N¢-2-ethanesulfonic acid (Hepes) buffer (pH 7.0) In order

to accurately quantify NaHCO3, 0.5M stock solution of

NaHCO3in the buffer was preincubated for 1 h before use

in an adequately sealed bottle to avoid equilibration with

atmospheric CO2 After addition of the NaHCO3 stock

solution to the reaction mixture in a sealed cuvette, further

incubation at 25°C for 5 min was carried out for

equili-bration before addition of the enzyme solution The

consumption of NADPH was monitored at 340 nm, and

one unit of activity was defined as 1 lmol of NADPH

oxidized per min For determination of optimum pH in each

reaction, 2-(N-morpholino)ethanesulfonic acid (Mes)

buf-fers with pH values from 5.0 to 7.0, Hepes bufbuf-fers with pH

values from 7.0 to 8.5, N,N-bis(2-hydroxyethyl)glycine

(Bicine) buffers with pH values from 8.0 to 9.0, and Ches

buffers with pH values from 8.7 to 10.0 were used for the

assay

R E S U L T S

Isolation of theidh gene from C limicola

In the cell-free extract of C limicola strain M1, we could

detect NADP-dependent IDH activity toward isocitrate

with a specific activity of 0.85 UÆmg)1, as previously shown

in the closely related green sulfur bacterium, C

thiosulfato-philum[1] Steen et al have recently reported the presence

of IDH in a related thermophile C tepidum by activity

staining after SDS/PAGE, in which the active band

corresponded in size (80 kDa) to monomeric IDH from

Desulfobacter vibrioformis[19] We therefore supposed that

IDH from C limicola is likely to be a monomeric enzyme

Two primers were designed from conserved regions among

known monomeric IDHs (See Materials and methods), and

PCR with the primers and genomic DNA from strain M1

gave successful amplification of a 1-kbp DNA fragment

The complete idh gene was isolated from C limicola

genomic library by using the amplified fragment as a probe

DNA sequencing analysis revealed that the Cl-idh gene

consisted of 2226-bp and encoded a protein with a

molecular mass of 80 465 Da Putative rho-independent

terminator was located 27-bp downstream of the stop codon However, typical consensus sequences for ribosome binding and for a promoter were not identified in the 5¢-flanking region of Cl-idh No open reading frames were found in the immediate vicinity of the gene

The deduced amino-acid sequence of Cl-IDH was 66.0% and 57.4% identical to monomeric IDHs from Vibrio sp strain ABE-1 (IDH-II) and from Cr glutamicum, respect-ively K253 in IDH from Cr glutamicum had been expected

to be a proton donor during the decarboxylation of isocitrate, and indeed, the site-specific mutagenesis of K253 to Met led to an inactive protein [23] In addition, the alkylation of the adjacent M258 inactivated the IDH from A vinelandii [26] These Lys and Met residues were conserved in Cl-IDH at the position of 256 and 259, respectively In dimeric IDH from E coli (Ec-IDH), K344 and Y345 were interacted with 2¢-phosphate of NADP molecule [23] and the positively charged residues were highly conserved in monomeric IDHs and supposed to contribute to their high specificity toward NADPH K589 and H590 in Cl-IDH were proposed to be equivalent to the residues in Ec-IDH

Expression and purification of IDH from recombinant

E coli

A high level of NADP-dependent IDH activity could be detected in the cell-free extract after induction with IPTG The activity of the recombinant cell-extract (19.5 UÆmg)1) was 100-fold higher than that in the host cells (0.20 UÆmg)1) The homogeneity of the recombinant protein was analyzed with SDS/PAGE (data not shown) and native-PAGE (Fig 1) analyses, and the specific activity of the purified IDH reached 36.0 UÆmg)1(Table 1) The molecular mass of the native enzyme was determined to be 81 kDa by gel-filtration column chromatography and 80 kDa by native-PAGE The results indicated that the recombinant IDH was

a monomeric enzyme with a molecular mass of 80 kDa No IDH activity was detected when NADH was used as a cofactor

Kinetic properties, pH profiles ofCl-IDH and comparison with NADP-dependent IDH fromS cerevisiae

The catalytic properties of IDH from C limicola were investigated for both the oxidative decarboxylation and reductive carboxylation reactions The activity for oxidative decarboxylation of isocitrate was assayed by standard procedures The optimum pH was 9.0 (Fig 2A), and apparent Kmvalues for isocitrate and NADP+at the optimum pH were determined to be 45 ± 13 lM and

27 ± 10 lM, respectively (Table 2) The reductive carboxy-lation activity towards 2-oxoglutarate was determined also

by spectrophotometry As both the monomeric and dimeric IDHs have been reported to accept CO2 molecule as a substrate [27] [28], the reaction mixture was sufficiently equilibrated after addition of NaHCO3 solution prior to assay in a capped cuvette The optimum pH for carboxy-lation was 7.0 (Fig 2A), where the CO2concentration after the equilibration was 17.9% (6.27 mM) of initial bicarbonate concentration (35 mM) Under this reaction condition, Cl-IDH showed normal Michaelis–Menten kinetics also

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for the carboxylation reaction Apparent Km values for

2-oxoglutarate and CO2 were 1.1 ± 0.5 mM and

1.3 ± 0.3 mM, respectively, which were much greater than

the values for isocitrate and NADP+ The kinetic param-eters of monomeric IDHs from C limicola and A vinelan-dii, previously determined by Wicken et al [28], are also shown in Table 2 In addition, we further examined the catalytic properties of NADP-dependent IDH from

S cerevisiae(Sc-IDH) in order to compare the properties

of monomeric IDHs with those of a dimeric enzyme The optimum pH for the decarboxylation and carboxylation activities of Sc-IDH were 8.5 and 6.0 (Fig 2B), and apparent Kmvalues for isocitrate, NADP+, 2-oxoglutarate, and CO2were 20 ± 5 lM, 33 ± 6 lM, 0.85 ± 0.30 mM, and 8.2 ± 1.0 mM, respectively (Table 2) The results suggested that differences in the properties were not so significant among the three enzymes for both the directions However, an interesting difference between Cl-IDH and Sc-IDH was observed in the activities at pH 7.0 The decarboxylic and carboxylic activities of Cl-IDH (46.0 and 41.0 UÆmg)1, respectively) were almost equivalent under physiological conditions (Fig 2A), in contrast to the much higher activity for decarboxylation of Sc-IDH (41.0 UÆmg)1) than that for carboxylation (8.7 UÆmg)1) at

pH 7.0 (Fig 2B)

Fig 1 Native-PAGE of recombinant Cl-IDH The active fraction after

Superdex200 gel-filtration column chromatography was applied to

lane 1 Lane M, molecular markers, thyroglobulin (669 000 Da),

ferritin (440 000 Da), catalase (232 000 Da), lactate dehydrogenase

(140 000 Da), albumin (66 000 Da).

Fig 2 Effect of pH on the decarboxylation (open symbols) and carb-oxylation (closed symbols) activities of Cl-IDH (A) and Sc-IDH (B) Assays were performed in each buffer as follows; Mes (r,e), Hepes (j,h), Bicine (m,n), CHES (d,s).

Table 2 Comparison of kinetic properties of IDHs Cl, Chlorobium limicola; Sc, Saccharomyces cerevisiae; Av, Azotobacter vinelandii.

Reaction Properties Cl-IDH Sc-IDH Av-IDH (28)

Decarboxylation K m (l M )

V max (UÆmg)1) 150 ± 6 54 ± 5 130 Carboxylation K m (m M )

2-Oxoglutarate 1.1 ± 0.5 0.85 ± 0.30 0.0139

V max (UÆmg)1) 38 ± 9 16 ± 2 –

Table 1 Purification of Cl-IDH from recombinant E coli IDH activity was measured with carboxylation reaction.

Step

Total protein (mg)

Total activity (U)

Specific activity (UÆmg)1)

Yield (%)

Purification (fold)

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Inhibition of carboxylation activity ofCl-IDH

by oxaloacetate

We further examined the effects of intermediate compounds

in the RTCA cycle on Cl-IDH activity Citrate, pyruvate,

succinate, fumarate, malate, glyoxylate, ATP, and ADP

gave no significant effect on the carboxylation reaction

(data not shown) However, considerable inhibition was

observed when oxaloacetate was added into the mixture

The carboxylation activity decreased to more than half in

the presence of 1 mMoxaloacetate (Fig 3A) In contrast, up

to 5 mMoxaloacetate had no influence on the carboxylation

activity of Sc-IDH The Dixon plot for oxaloacetate with

different concentrations of 2-oxoglutarate displayed typical

competitive inhibition, and a Kivalue of oxaloacetate for

Cl-IDH was determined to be 0.35 ± 0.04 mM (Fig 3B)

Similar to previous reports with IDHs from various sources,

a concerted inhibition with oxaloacetate and glyoxylate was

also observed against Cl-IDH By addition of 0.25 mM

glyoxylate together with the same concentration of

oxaloacetate (0.25 mM), the decarboxylation activity was

decreased to 44%, while relative activity was 77% without

glyoxylate (data not shown)

D I S C U S S I O N

In this paper, we investigated IDH from the green sulfur

bacterium, C limicola, as a CO2-fixing enzyme in RTCA

cycle The enzyme IDH from C limicola was revealed to be

a monomeric enzyme with a molecular mass of 80.5 kDa

The deduced amino-acid sequence of Cl-idh gene showed

high similarities to other monomeric IDHs from Vibrio sp

strain ABE-1 and Cr glutamicum However, no significant

similarity was observed between monomeric and dimeric

IDHs in their primary structures, suggesting that these two

distinct IDHs evolved independently from different

ances-tors

We compared the catalytic properties of Cl-IDH with

those of Sc-IDH Both IDHs exhibited higher affinities to

substrates for decarboxylation (NADP+ and isocitrate)

than those for carboxylation (2-oxoglutarate and CO2), and

the specific activities toward decarboxylation were higher

than those toward the reverse direction at the respective

optimum pH The kinetic parameters of monomeric IDH

from A Vinelandii also showed the same tendency (Table 2) These results indicated that there was not such

a significant difference between Cl-IDH and the counter-parts from aerobic microorganisms These IDHs could catalyze oxidative decarboxylation more efficiently com-pared to reductive carboxylation

However, it is interesting to note that the ratios of carboxylation and decarboxylation activities at pH 7.0, presumably close to the physiological pH, showed a clear difference between Cl-IDH and Sc-IDH The activity of Sc-IDH toward decarboxylation was fivefold higher than that toward carboxylation at pH 7.0 (Fig 2B), suggesting that the decarboxylic reaction was predominant over the carboxylic reaction in vivo This result is consistent with the fact that the NADP-dependent IDH contributes to provide NADPH for reduction of unsaturated fatty acid in

S cerevisiae[29] In contrast, the carboxylation activity of Cl-IDH at pH 7.0 was as high as the decarboxylation activity (Fig 2A) Cl-IDH possessed a more favorable property to fix CO2 than Sc-IDH under physiological conditions

Among the intermediates of RTCA cycle, oxaloacetate affected activities of Cl-IDH More than half of the activity was inhibited by 1 mMoxaloacetate in both directions, and the inhibition for carboxylation was shown to be compet-itive Inhibition by oxaloacetate has been examined for dimeric IDHs and a few monomeric IDHs from

Cr glutamicumand A vinelandii The enzymes displayed low (5–27%), or only trivial (0–5%) levels of inhibition by

1 mM oxaloacetate Although these results were obtained against decarboxylic activity, we confirmed that even 5 mM

oxaloacetate gave no inhibition to the carboxylation activity

of Sc-IDH (Fig 3A) IDHs seemed to be generally insen-sitive against oxaloacetate One exception is the IDH from purple nonsulfur bacterium R vannielii, which showed 44% inhibition with 0.2 mM oxaloacetate [18] This indi-cates that the strong inhibition by oxaloacetate was not a specific property for an IDH which functions in the RTCA cycle

The question remains whether Cl-IDH is actually inhib-ited by oxaloacetate in vivo Malate dehydrogenase is known

to predominantly catalyze the reduction of oxaloacetate to malate, and thereby lowering the possibilities of oxaloacetate accumulation Indeed, when we have analyzed the malate dehydrogenase activity in the cell-free extracts of C

limico-la, 0.95 UÆmg)1activity in the direction of malate synthesis could be detected (data not shown) However, although a closely related strain Chlorobium thiosulfatophilum also harbors the same levels of malate dehydrogenase (0.62 UÆmg)1[1]), previous radiolabeling experiments dem-onstrated a large accumulation of oxaloacetate in the cells, relative to other intermediates [30] In the cells of

C thiosulfatophilumgrown in a medium containing3H2O, the radioactivity of oxaloacetate was 3.6-fold greater than that of malate and 21-fold greater than that of the sum of citrate and isocitrate In addition,14CO2-labeling indicated that oxaloacetate was one of the first stable products of photosynthesis by C thiosulfatophilum [30] These results suggested that oxaloacetate was pooled in Chlorobium cells despite the presence of high malate dehydrogenase activity, and the concentration would sensitively reflect the level of carbon assimilation by the cycle As we previously reported, ATP-citrate lyase from C limicola catalyzes only the

Fig 3 Inhibition of Cl-IDH with oxaloacetate (A) Effect of

oxaloac-etate concentration on the carboxylation activities of Cl-IDH (j) and

Sc-IDH (h) (B) Dixon-plots for oxaloacetate with 3 m M (d), 5 m M

(m), and 10 m M (s) 2-oxoglutarate.

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ATP-dependent cleavage of citrate and the activity was

inhibited at higher ADP/ATP ratios [24] RTCA cycle is

considered to be driven excessively by ATP-citrate lyase

under sufficient energy conditions that might lead to

overaccumulation of oxaloacetate within the cells The

inhibition of Cl-IDH carboxylic reaction by oxaloacetate or

by that concerted with glyoxylate could suppress the cycle in

order to change the carbon flux to other pathways, such as

glutamate biosynthesis, under the condition of excess

turnover of the RTCA cycle Further studies of the enzyme

will clarify the structure, functions, and regulation in the

RTCA cycle

R E F E R E N C E S

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