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Báo cáo khoa học: Light-induced gene expression of fructose 1,6-bisphosphate aldolase during heterotrophic growth in a cyanobacterium, Synechocystis sp. PCC 6803 ppt

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The increases in the protein level of FbaA and fbaA gene expression observed in wild-type cells under LAHG conditions were greatly inhibited in the deletion mutant.. Results Growth of Sy

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1,6-bisphosphate aldolase during heterotrophic growth

in a cyanobacterium, Synechocystis sp PCC 6803

Yosuke Tabei, Katsuhiko Okada, Nobuaki Makita and Mikio Tsuzuki

School of Life Sciences, Tokyo University of Pharmacy and Life Sciences, Japan

In photosynthetic organisms, light activates various

signal transduction pathways regulating the growth

rate, the expression of genes involved in various

meta-bolic processes and the activation of enzymes related

to energy processes In higher plants, various

pheno-mena concerning photogermination, phototropism and

photoperiodism, including flower initiation, are

regu-lated by light as a signal via phytochromes and⁄ or

other photoreceptors [1,2] In cyanobacteria, resetting

of the circadian rhythm [3] and phototaxis [4] have

been analyzed at the gene expression level In the light, cyanobacteria assimilate CO2 via the reductive pentose phosphate pathway using ATP and NAD(P)H gener-ated through photosynthesis to produce glycogen and other organic compounds In the dark, glucose resi-dues derived from glycogen are catabolized via glycoly-sis, the oxidative pentose phosphate pathway (OPPP) and the incomplete tricarboxylic acid cycle, leading to the production of NAD(P)H and biosynthetic inter-mediates for maintenance and growth [5,6] Both

Keywords

cyanobacteria; glucose degradation; light;

signal transduction; Synechocystis

Correspondence

K Okada, School of Life Sciences, Tokyo

University of Pharmacy and Life Sciences,

Horinouchi, Hachioji, Tokyo 192-0392, Japan

Fax: +81 42 676 6721

Tel: +81 42 676 6716

E-mail: kokada@ls.toyaku.ac.jp

(Received 8 August 2008, revised 18

October 2008, accepted 30 October 2008)

doi:10.1111/j.1742-4658.2008.06772.x

Synechocystis sp PCC 6803 exhibits light-activated heterotrophic growth (LAHG) under dark conditions with glucose as a carbon source The light activation is remarkable at a late period of photoautotrophic preculture, such as the late-linear and stationary growth phases To understand the physiological effects of light irradiation and glucose under LAHG condi-tions, their effects on the expression of soluble proteins were analyzed by means of 2D-PAGE Various soluble proteins, which were minimal under photoautotrophic preculture conditions, were observed clearly under LAHG conditions, suggesting that proteins were synthesized actively under these conditions Fructose 1,6-bisphosphate aldolase, one of the glycolytic enzymes, was found to be induced under LAHG conditions on 2D-PAGE The activity of fructose 1,6-bisphosphate aldolase, which had decreased during photoautotrophic preculture, also increased under LAHG condi-tions, similar to the mRNA level of the encoding gene, fbaA In addition,

we found that a deletion mutant of sll1330, a putative gene containing a helix-turn-helix DNA-binding motif, could not grow under LAHG condi-tions, whereas it could grow photoautotrophically The increases in the protein level of FbaA and fbaA gene expression observed in wild-type cells under LAHG conditions were greatly inhibited in the deletion mutant These results suggest that the regulation of fbaA gene expression by way of sll1330 is one of the important processes in Synechocystis sp PCC 6803 under light pulse LAHG conditions

Abbreviations

EMSA, electrophoretic mobility shift assay; FBA, fructose 1,6-bisphosphate aldolase; G6PD, glucose 6-phosphate dehydrogenase; GAPDH, glyceraldehyde 3-phosphate dehydrogenase; GK, glucokinase; HTH, helix-turn-helix; LAHG, light-activated heterotrophic growth; OPPP, oxidative pentose phosphate pathway; PGI, glucose 6-phosphate isomerase; PK, pyruvate kinase.

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metabolic processes occur in the same compartment in

prokaryotic cells [7]

Synechocystis sp PCC 6803 (hereafter referred to as

Synechocystis), a unicellular cyanobacterium, is a

use-ful model species for research on biological responses

to the environment because its whole genome sequence

has been determined [8] and molecular techniques are

available, including transformation and homologous

recombination Exhaustive analyses of gene expression

(such as of the transcriptome and proteome) are now

possible for this organism For example, new insights

into the role of thioredoxin in the regulation of cellular

processes and the function of the cell membrane in

cyanobacteria have been obtained through proteomic

analysis [9] Moreover, Synechocystis can grow

hetero-trophically on glucose Light irradiation, however, is

required for heterotrophic growth, which occurs even

with a low light intensity at which photosynthesis can

scarcely proceed The cells can grow even with

occa-sional light pulses (e.g for 5 min every 24 h) [10]

Therefore, so far, this phenomenon has been

desig-nated as light-activated heterotrophic growth (LAHG)

Although hik8 and sigE have been reported to be

necessary for LAHG [11,12], the exact mechanism

underlying LAHG has not yet been determined

Genome sequencing for several cyanobacteria has

revealed the presence of all the genes required for

glu-cose metabolism, and biochemical evidence of the

functional roles of the gene products has been

obtained [8,13] The genes and⁄ or enzymes involved in

glycolysis and the OPPP, as studied to date in some

detail in cyanobacteria, include glucose 6-phosphate

dehydrogenase (G6PD) [14], 6-phosphogluconate

dehy-drogenase [15], glyceraldehyde 3-phosphate

dehydroge-nase (GAPDH; EC 1.2.1.12) [16–18], pyruvate kidehydroge-nase

(PK; EC 2.7.1.40) [19], phosphoenolpyruvate

carboxyl-ase [20], fructose 1,6-bisphosphate aldolcarboxyl-ase (FBA; EC

4.1.2.13) [21] and phosphofructokinase [6,22]

How-ever, the regulation of glucose metabolism under dark

conditions and the coordination of its control in

cyanobacteria remain poorly understood It is

impor-tant to note that the reductive pentose phosphate

path-way as well as the glycolysis and gluconeogenesis

pathways function in the same compartment of the

cyanobacterial cells In addition, cyanobacterial

thyla-koid membranes harbor both photosynthetic and

respiratory electron transport chains, and the same

components are shared by the two processes [23]

Therefore, it is important to strictly regulate the

direc-tion of reacdirec-tions in the anabolic and catabolic

path-ways in response to environmental conditions

For characterization of LAHG, the analysis of gene

expression involved in carbon metabolism that is

induced by light, especially of glycolytic enzymes, is important In the present study, we provide clear evidence of LAHG with cells at the late-linear and stationary growth phases of photoautotrophic precul-ture In addition, we show that, under LAHG condi-tions FBA, a glycolytic enzyme, is regulated by light and glucose via sll1330, a putative gene containing a helix-turn-helix (HTH) DNA-binding motif

Results

Growth of Synechocystis and its glucose utilization under heterotrophic growth conditions Photoautotrophically grown cells at the late-linear growth phase were cultured heterotrophically with or without short periods (5 min) of light every 3 h, which

is considered as LAHG in the present study The cells grew with approximately 30 and 66 h of doubling time

on culture with or without light pulses, respectively They grew to a two-fold higher level with 10 mm glu-cose (6.0· 108cellsÆmL)1) than with 5 mm glucose in approximately 1 week (2.8· 108cellsÆmL)1) (Fig 1) However, in continuous darkness (dark heterotrophic conditions), the cells did not grow so much, even in the presence of either 5 or 10 mm glucose Without glucose, the cells could not grow either with or without the light pulses Whereas glucose in the medium was almost completely consumed under LAHG conditions

in 8 days, glucose remained in the medium even after cell growth had ceased under dark heterotrophic con-ditions (Fig 1B) These results suggest that the supply

of glucose in the medium was the sole carbon and energy source for the cells to grow and that the cells could not fully utilize glucose until they were exposed

to light pulses

During culture, the amount of chlorophyll a in the cells grown photoautotrophically decreased under both LAHG and dark heterotrophic conditions from 3.0 to 0.9· 10)14gÆcell)1 in 8 days The amount of soluble protein was maintained at approximately 2.0· 10)14gÆcell)1 under LAHG conditions, but decreased to 0.8· 10)14gÆcell)1 in 8 days under dark heterotrophic conditions The results obtained suggest that soluble protein synthesis continued at a normal level under LAHG conditions, but not in the dark

Dependence of LAHG on the cell conditions for photoautotrophic preculture

The cell conditions for photoautotrophic preculture greatly affected the subsequent LAHG and heterotro-phic growth profiles (Fig 2) The cells harvested at the

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logarithmic growth phase could grow fast

heterotro-phically either with or without light pulses (Fig 2B)

By contrast, those harvested at the stationary growth

phase of the preculture scarcely grew, even in the

pres-ence of glucose in the dark (Fig 2F) Cells harvested

at any phase of the preculture could grow under

LAHG conditions, although the induction period was

longer with a longer preculture period (Fig 2C–E)

Therefore, the difference in cell growth between

LAHG and dark heterotrophic conditions was obvious

at a late period of culture, such as the late-linear growth phase, where reactivation of some processes by light pulses may occur under LAHG conditions Cells harvested on day 8 of photoautotrophic preculture (Fig 2E) were used for subsequent experiments

Proteome analysis of cells grown under photoautotrophic preculture, LAHG and dark heterotrophic conditions

The compositions of soluble proteins on culture under LAHG, dark heterotrophic and the respective precul-ture conditions were analyzed by 2D-PAGE Under photoautotrophic preculture and LAHG conditions (Fig 3A,B), over 90 protein spots were observed, whereas less than half this number was observed under heterotrophic conditions These results imply that some

of the proteins appearing during photoautotrophic pre-culture disappeared under dark heterotrophic condi-tions We also found that 32 of the spots observed were thicker for LAHG than the corresponding spots for photoautotrophic preculture, suggesting a greater syn-thesis of the respective proteins with the addition of glucose Moreover, 20 of these 32 spots were thicker than the corresponding spots under dark heterotrophic conditions, suggesting a greater synthesis of the respec-tive proteins with light in the presence of glucose The putative genes and their products for individual spots that were increased by the glucose supply with and without the short periods of light were determined from the molecular weights of fragments by means of MALDI-TOF MS (Table 1) Protein syntheses with various categories of genes in relation to metabolism, transport and the machinery of gene expression were enhanced under LAHG conditions The proteins involved in cellular processes, GroEL1 (spot 6), Tig (8) and GreP (32), were induced under LAHG conditions HtpG (spot 3), DnaK2 (4) and GroEL2 (5, 7) appeared under both LAHG and dark heterotrophic conditions Rps1a (spot 20) and Tsf (26) involved in the translation machinery were induced under LAHG conditions, whereas Fus (spot 2), Tuf A (14) and Rpl12 (31) were induced under dark heterotrophic conditions These results suggest that cellular processes and translation machinery function differently with or without light in the presence of glucose AtpB (spot 9), NatB (10), UrtA (11), RbcL (17) and CpcB (29), formerly regarded as representing peripheral membrane proteins [24], were abundant in the soluble fraction of the cells grown under LAHG conditions They might have been extracted dur-ing our sample preparation due to good solubilization,

or the association between the proteins and the membrane might change with growth conditions

0

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1.5

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B

Time (days)

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0

2

4

6

8

10

Time (days)

Fig 1 Growth of Synechocystis under heterotrophic conditions

with (open circles and open squares) or without (filled circles and

filled squares) light pulses for 5 min every 3 h (A) and the glucose

concentration in the medium during culture (B) The cultures grown

photoautotrophically at the late-linear growth phase were incubated

in BG-11 in the presence of 5 m M (open circles and filled circles) or

10 m M (open squares and filled squares) glucose, and in the

absence of glucose (open triangles and filled triangles) at 30 C.

The decrease in the glucose concentration was determined at the

indicated times thereafter Error bars are for three separately grown

cultures.

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2D-PAGE also revealed that some proteins, including

RbcL (spot 17), Gap2 (24) and Prk (19) in

photosyn-thetic carbon metabolism, and FbaA (18) in glucose

metabolism, were synthesized to a greater extent under

LAHG conditions than under any of the other

condi-tions The reason why photosynthetic genes were

induced by glucose was probably a result of the higher

protein-synthetic activity Enzymes involved in

glycoly-sis and the OPPP other than FbaA were not included in

Table 1, probably due to their low contents or to them

being less changeable in their amounts The increase in

the protein level of FbaA under LAHG conditions

com-pared to under dark heterotrophic conditions suggested

that glucose degradation was induced by light and

glu-cose in Synechocystis

The activity of FBA, which decreased from 88 to

46 unitsÆmg)1 protein during autotrophic preculture,

was determined for both LAHG and dark

heterotro-phic cultures (Fig 4) The FBA activity increased

under LAHG conditions, whereas, under dark

hetero-trophic conditions, it remained constant for 4 days

and then decreased gradually This finding is consistent

with the protein level of FBA, which was increased by

light pulses in the presence of glucose

Possible enhancement of glucose metabolism during LAHG

When 5 mm d-[14C(U)]glucose was supplied to cells that had been incubated in continuous darkness with

5 mm glucose for 6 days, most of the radioactivity incorporated was found in phosphate esters and a slight amount in glutamate at 1 h after the supply of

d-[14C(U)]glucose (data not shown) Thus, we pre-sumed that even the cells cultured in continuous dark-ness metabolized it to phosphorylated sugars, but to a lesser extent to other organic compounds

2D TLC of a cell extract with detection with ninhy-drin revealed that glutamate was a major amino acid

in cells incubated under both LAHG and dark hetero-trophic conditions, but that the amount under the former was much higher than that under the latter (see Fig S1) The l-glutamate contents in the cells at 0 and

8 days under LAHG, and at 8 days in continuous darkness, were 0.13, 0.20 and 0.05· 10)11gÆcell)1, respectively Considering that glutamate is synthesized from 2-oxoglutarate via the tricarboxylic acid cycle by way of an aminotransferase reaction, we could deduce that the glucose metabolism is more active under

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Time (days)

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12d

8d

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Fig 2 Effects of pre-culture conditions on the heterotrophic growth of Synechocystis Growth of Synechocystis on photoautotrophic precul-ture (A) Growth of Synechocystis under the heterotrophic conditions (B–F) with (open circles and open squares) or without (filled circles and filled squares) light pulses for 5 min every 3 h The cultures were carried out in BG-11 in the presence of 5 m M glucose (open circles and filled circles) and in the absence of glucose (open squares and filled squares) (B–F) Growth when the cells started to be cultured in the pres-ence of glucose at 4, 5, 7, 8 and 12 days, respectively, in (A) The data are representative of three separate cultures.

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LAHG conditions than under dark heterotrophic

conditions

Changes in some enzymatic activities on glucose

metabolism

The maximum enzymatic activites of glycolytic

enzymes under dark heterotrophic and LAHG

condi-tions for 8 days were determined in the presence of

dithiothreitol (Table 2) The activities of glucokinase

(GK; EC 2.7.1.2) and PK were constantly maintained under the three sets of conditions The glucose 6-phos-phate isomerase (PGI; EC 5.3.1.9) and FBA activities were relatively higher than those of the other enzymes The total activity of FBA under LAHG conditions was higher than the initial level, whereas that under dark heterotrophic conditions was lower The activity

of GAPDH was increased by the addition of glucose Therefore, we concluded that FBA was enhanced at both the protein level and with respect to its activity

kDa

C

E

D

250

75

50

25

p I 4

Autotrophic conditions

1 3

6 2

18 9 7 8 10 11

26 25 27

29

31 30

19 20

17

Fig 3 Proteome analyses of the soluble protein fraction of Synechocystis under various conditions The soluble proteins were extracted from Synechocystis cultured under photoautotrophic preculture (A), LAHG (B) and dark heterotrophic (C) conditions for 8 days Equivalent amounts of proteins were separated by 2D-PAGE and stained with Coomassie brilliant blue The profile shown in (E) is identical to (B) with circles and numbers for annotation purposes The soluble proteins of Dsll1330 cultured under LAHG conditions for 8 days (D) were also analyzed The positions of molecular size markers are indicated in kDa on the left FBA is indicated by an arrow.

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under LAHG conditions compared to in continuous

darkness This result is consistent with the

enhance-ment of fbaA gene expression by light pulses in the

presence of glucose [25]

Changes in the transcript level of fbaA during

heterotrophic culture

Figure 5 shows the changes in the mRNA level of

fbaAunder LAHG and dark heterotrophic conditions

Considering that the cells at 0 days in Fig 5 had been

grown under photoautotrophic conditions, and that the mRNA level of fbaA increased under LAHG con-ditions, we deduced that the increase in the mRNA level of fbaA was induced by both light pulses and glucose On the other hand, the mRNA level of fbaA under dark heterotrophic conditions increased slightly until 6 days, and then decreased gradually The level under the dark heterotrophic conditions was approxi-mately one-tenth of that under LAHG conditions after

8 days These results suggested that light irradiation was required for the expression of fbaA

Table 1 Proteins were observed under LAHG conditions to a 1.5-fold greater extent than under autotrophic conditions in Synechocystis.

Spot no on 2D-PAGE

Light induciblea

sll1363 Ketol-acid reductoisomerase (IlvC) 21

chaperone (HtpG)

3

sll0170 70 kDa heat shock protein (DnaK2) 4

Photosynthesis and respiration,

energy metabolism

slr0009 Ribulose bisphosphate carboxylase

large subunit (RbcL)

sll1342 Glyceraldehyde 3-phosphate

dehydrogenase (Gap2)

sll0018 Fructose 1,6-bisphosphate

aldolase (FbaA)

Transport and binding proteins slr0559 Periplasmic binding protein of ABC

transporter for natural amino acids (NatB)

sll1447 Periplasmic protein, ABC-type urea

transporter system substrate binding protein (UrtA)

11

sll1450 Nitrate ⁄ nitrite transporter system

substrate binding protein (NrtA)

13 DNA replication, restriction, modification,

recombination, and repair

sll8006 Type I restriction-modification

system S subunit

sll1749 50s ribosomal protein L12 (Rpl12) 31

a Genes enhanced under LAHG conditions to a 1.5-fold greater extent than under dark conditions are indicated (s).

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LAHG and the protein composition of

Dsll1330, encoding a two-component system

response regulator

Because many transcriptional factors contain the HTH

DNA-binding motif, there is a possibility that some

HTH DNA-binding proteins may be involved in the

fbaAgene expression induced by light and glucose We

have searched the Synechocystis genome sequence

databank and Cyanobase, and identified 57 ORFs

encoding putative HTH motif-containing

transcrip-tional factors Among these candidates, we successfully

mutated the sll1330 gene encoding a putative

two-component response regulator by means of targeted

mutagenesis with a spectinomycin resistance cassette

A resultant sll1330 deletion mutant, Dsll1330, could grow under photoautotrophic and mixotrophic (i.e under continuous light illumination with glucose) con-ditions as fast as the wild-type (Fig 6A,B) However, Dsll1330 did not grow well either under LAHG or dark heterotrophic conditions compared to the wild-type (Fig 6C,D) This can be explained by a deficiency

in the ability to use glucose as a carbon source for growth

Proteome analysis of Dsll1330 showed relatively lower contents of various proteins [e.g Gap2 (spot 24) and Tsf (spot 26)] The FbaA protein (spot 18; Fig 3, arrow) was also less in Dsll1330 (Fig 3B,D) and was

as high as that in wild-type cells incubated under dark conditions The FbaA protein appeared to be more stable than its mRNA In any case, these results, when taken together with those obtained previously [25], suggest that one of the reasons for the inability of LAHG by Dsll1330 is a lack of enhancement of the protein level of FBA with light pulses in the presence

of glucose

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80

60

40

20

0

Time (days) Fig 4 The FBA activities of Synechocystis under LAHG and

het-erotrophic conditions in BG-11 containing 5 m M glucose Cells were

incubated under LAHG (white bars) and dark heterotrophic (black

bars) conditions for 2, 4, 6 and 8 days (0 days indicates the activity

of FBA on photoautotrophic preculture on day 8) The error bars

represent three separately grown cultures.

Table 2 Glycolytic enzyme activities of cells grown under dark heterotrophic and LAHG conditions for 8 days.

Activity (mUÆmg)1protein ± SE) Initial

(0 days)

Dark heterotroph (8 days)

LAHG (8 days)

a Class-II was inhibited by the addition of 1 m M EDTA.

fbaA rRNA

(days)

Fig 5 Northern analysis of fbaA gene expression in Synechocystis under LAHG and dark heterotrophic conditions in BG-11 containing

5 m M glucose RNA was isolated from cells grown photoautotrophi-cally on day 8 (0 days) and cells incubated under LAHG and dark heterotrophic conditions for 2, 4, 6 and 8 days Total RNA (10 lg) was then subjected to northern hybridization with a probe specific for the fbaA gene The lower panel shows rRNA stained with ethi-dium bromide as a control The data are representative of three independent experiments.

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Interaction of the Sll1330 protein with the fbaA

pro-moter region was additionally examined by means of

the electrophoretic mobility shift assay (EMSA) using

DNA fragments of the upstream region of fbaA (see

Fig S2) The DNA fragment comprising )331 to

)186 bp from the putative transcription start point of

the fbaA gene was found to bind with Sll1330, which was overexpressed in Escherichia coli (see Fig S2) These results suggest that Sll1330 binds to this putative promoter region of the fbaA gene in PCC 6803 cells

Discussion

In the present study, the effects of light on heterotro-phic growth of Synechocystis were precisely investi-gated First, we confirmed that Synechocystis could not grow in complete darkness, as reported previously [10] However, the cells at the logarithmic growth phase could grow heterotrophically even without illu-mination This would be because glucose-degrading machineries were active in the photoautotrophic pre-culture at relatively early stages The total FBA activ-ity in the late-linear growth phase was lower than that

in the exponential growth phase (Table 2) This is consistent with the fact that the mRNA levels of some glycolytic genes were suppressed at the stationary growth phase compared to at the exponential growth phase [26] Physiological changes occur at different growth phases with respect to the accumulation of inhibitory metabolites [27,28] and gene expression [29] The expression of 10% of the genes was different in the linear growth phase compared to in the logarithmic growth phase [30] Considering the close correlation between nitrogen and carbon metabolism [13], we assume the decrease in gene expression during growth

is due to the lower level of nitrogen in the medium Alternatively, because of the higher concentration of cells during photoautotrophic preculture, the amount

of light absorbed by each cell decreased in these condi-tions In any case, when using cells precultured at a late period of the preculture (i.e after 8 days of cul-ture), an effect of light on the heterotrophic growth was clearly observed Therefore, LAHG might be due

to reactivation of some biochemical activities

We have attempted proteome analysis using the com-bination of 2D-PAGE and MALDI-TOF MS of tryptic digests Considerable amounts of soluble proteins were found in the cells under LAHG conditions compared to those after 8 days of photoautotrophic preculture Con-sidering that various kinds of proteins were present at higher levels under LAHG conditions than under dark heterotrophic conditions, we deduced that the light pulses triggered the transcription and translation of a whole set of proteins essential for growth with glucose

In this respect, the transcriptional levels of molecular chaperones groESL and cpn60 are known to be signifi-cantly increased by light irradiation in Synechocystis [30] Moreover, the DnaK2 protein is one of the abun-dant soluble proteins, with dnaK gene expression having

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B

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Fig 6 Growth of the wild-type (circles) and Dsll1330 (triangles)

under photoautotrophic (continuous light; A), mixotrophic

(con-tinuous light + 10 m M glucose; B), LAHG (light pulses + 10 m M

glucose; C) and dark heterotrophic (dark + 10 m M glucose; D)

conditions Error bars indicate the SD for three independent

experiments.

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been reported to obey up-regulation with the lights on

and down-regulation with the lights off (i.e in the

man-ner of a circadian rhythm) [31], which is consistent with

the results shown in Fig 3 DnaK2 and rehydrin may

protect the cells from continuous light irradiation and

facilitate the functional assembly of photosynthetic

machinery proteins [32] The SodB protein (Spot 29)

cat-alyzes the dismutation of O2)to H2O2and O2, in which

sodBgene and SodB protein expression are induced by

continuous light irradiation [33] Light induction of

putative 30S ribosomal protein S1 (sll1356) and

elonga-tion factor Ts (sll1261), which are involved in

transla-tion processes, suggests that protein synthesis is

enhanced during cell growth under LAHG conditions

This is supported by the appearance of more spots on

2D-PAGE of cells under LAHG conditions than under

heterotrophic conditions

In the present study, the expression of GroEL1, Tig

and GreP was also up-regulated under LAHG

condi-tions compared to under both photoautotrophic and

dark heterotrophic conditions These results suggest

the higher activities of cellular processes (e.g protein

synthesis and metabolic processes) under LAHG

con-ditions FbaA, one of the components of the

glucose-metabolism machinery, was also up-regulated by light

under glucose-utilizing conditions The protein level of

FbaA was high compared to that of other glycolytic

enzymes The increase in the maximum Fba activity in

8 days (Fig 4) under LAHG conditions, but not under

dark heterotrophic conditions, suggested the light

acti-vation of Fba synthesis This is also supported by the

higher content of glutamate in the cells Therefore,

cells under LAHG conditions may be more active than

without light

We found also that, in the sll1330 deletion mutant

(Dsll1330), which could not grow heterotrophically

(Fig 6), the protein level of FbaA was repressed

(Fig 3D), even under LAHG conditions, and the

increases in the mRNA levels of five glycolytic genes,

including fbaA, were repressed by light and glucose [25]

We also found binding of Sll1330 with the promoter

region of the fbaA gene Because the Dsll1330 mutant

could grow photoautotrophically with the expression of

fbaA, the sll1330 gene is not required for the expression

of fbaA under photoautotrophic conditions This means

that fbaA gene expression is controlled through two

signal pathways: presumably photosynthetic processes

and light pulses in the presence of glucose Gene

expres-sion of fbaA may be important for survival in various

environments, including both under photoautotrophic

and heterotrophic conditions In the latter case, glucose

induces the expression of several genes, such as those

for GK, phosphofructokinase, phosphoglycerate mutase

and PK, including sll1330 [34] In this respect, glucose degradation as a whole may be regulated by the expres-sion of glycolytic genes via sll1330

Experimental procedures

Algal cells and culture conditions

A glucose tolerant strain of Synechocystis [35] was cultivated photoautotrophically in BG-11 containing 20 mm Tes-KOH (pH 8.2) with continuous illumination by a bank of fluores-cent lamps at 10 WÆm)2and bubbled with 2% (v⁄ v) CO2in glass tubes or flasks [36] The LAHG cultures were incu-bated in the dark with 5 min of light irradiation (5 WÆm)2), eight times a day in the presence of 5 and 10 mm glucose, whereas the heterotrophic cultures were incubated without light irradiation in the presence of glucose Growth and cell density were followed by measuring the absorption at

730 nm with a spectrophotometer (DU640; Beckman Coulter, Fullerton, CA, USA) Cell concentrations were determined with a hemacytometer (Bu¨rker-Turk; Erma Opti-cal Works, Tokyo, Japan) Glucose uptake was assayed by measurement of the concentration of glucose in the medium with a glucose CII kit (Wako Pure Chemical Industries, Osaka, Japan) In the mutant, the wild-type gene for sll1330 was disrupted by the insertion of a spectinomycin resistance cassette [25]

Determination of intracellular chlorophyll a, soluble protein andL-glutamate

Chlorophyll a was measured by the procedure described by Mackinney [37], with some modifications Soluble protein was assayed by measurement of the concentration of a par-ticular protein with a BCA protein assay reagent kit (Pierce Biotechnology, Rockford, IL, USA) Cells were harvested

at a certain time, centrifuged, and then disrupted with a French press at 28 000 p.s.i The lysate was centrifuged and the resulting supernatant was used for the measurement

of soluble protein Intracellular l-glutamate was assayed

by measurement of the concentration of l-glutamate with

a l-glutamate determination kit (Yamasa Corp., Chiba, Japan)

2D-PAGE and in-gel digestion

The materials precipitated from 300 lg of soluble protein were resuspended in 8 m urea, 1% (v⁄ v) Triton X-100, ampholine (pH 3.5–10.0) and 2-mercaptoethanol The mix-ture was centrifuged at 10 000 g for 10 min at 4C The supernatant was applied to a linear immobilized pH gradi-ent strip (pH 4.0–8.0) Isoelectric focusing and subsequgradi-ent SDS⁄ PAGE were then performed Proteins were stained with Coomassie brilliant blue and then scanned using an

Trang 10

image scanner In-gel digestion was performed as described

for an in-gel digest kit (Millipore, Billerica, MA, USA)

The gel pieces were re-swollen by adding a trypsin solution

Samples were incubated overnight at 30C and the protein

fragments were extracted

MALDI-TOF analysis

Peptide extracts were loaded onto the target plate by the

dried droplet method using a-cyano-4-hydroxycinnamic

acid as a matrix MALDI-TOF analysis was performed in

the reflector mode with a Voyager-DE PRO mass

spec-trometer (Applied Biosystems, Foster City, CA, USA)

Database search

Proteins were identified by searching the Synechocystis

database using ms-fit (Protein Prospector; UCSF, San

Francisco, CA, USA) The following criteria were used for

a positive identification in the ms-fit database search: (a)

at least four matching peptide masses; (b) at least 50% of

the measured masses must match the theoretical masses;

and (c) 0.01% or better mass accuracy

Assaying enzyme activity

The cells cultivated under LAHG and heterotrophic

condi-tions were harvested by centrifugation The pellets were

resuspended and then lysed by three passages through a

French press at 28 000 p.s.i., followed by clarification by

cen-trifugation at 35 000 g for 10 min The enzyme activities

were measured using previously described procedures

[7,21,38] with some modifications The assay mixtures

com-prised: GK [50 mm Hepes-KOH (pH 8.0), 1 mm

dithiothrei-tol, 10 mm MgCl2, 2.5 mm glucose, 5 mm ATP, 0.5 mm

NAD+and 5 unitsÆmL)1G6PD]; PGI [50 mm Hepes-KOH

(pH 8.0), 1 mm dithiothreitol, 10 mm MgCl2, 1.7 mm

NAD+, 2 mm fructose 6-phosphate and 5 unitsÆmL)1

G6PD]; PFK [50 mm Hepes-KOH (pH 8.0), 1 mm

dith-iothreitol, 10 mm MgCl2, 0.15 mm NADH, 2 mm

fruc-tose 6-phosphate, 2.5 mm ATP, 1 unitÆmL)1 aldolase,

10 unitsÆmL)1 triosephosphate isomerase and 1 unitÆmL)1

glycerophosphate dehydrogenase]; FBA [50 mm Tris–HCl

(pH 7.5), 0.2 mm CoCl2, 0.2 mm NADH, 1 unitÆmL)1

glyc-erol 3-phosphate dehydrogenase, 1 unitÆmL)1

triosephos-phate isomerase and 1 mm fructose 1,6-bisphosphate];

GAPDH [50 mm Tris–HCl (pH 7.5), 5 mm MgCl2, 3 mm

3-phosphoglycerate, 1 mm EDTA, 5 unitsÆmL)1

3-phospho-glycerate kinase, 2 mm ATP and 0.2 mm NADH]; enolase

[50 mm Hepes-KOH (pH 8.0), 1 mm dithiothreitol, 10 mm

MgCl2, 0.15 mm NADH, 3 mm ADP, 3 mm

2-phospho-glycerate, 5 unitsÆmL)1 PK and 6 unitsÆmL)1 lactate

dehydrogenase]; and PK [50 mm Hepes-NaOH (pH 7.0),

30 mm MgCl2, 0.15 mm NADH, 2.5 mm

phosphoenolpyr-uvate, 1 mm ADP and 2 unitsÆmL)1lactate dehydrogenase]

RNA isolation and northern hybridization

Total RNA was extracted and purified by phenol–chloro-form extraction [39] For northern hybridization, the DNA fragments of fbaA were amplified by PCR, using primers 5¢-ATTTCGATCATGCAGGCCG-3¢ and 5¢-GGAAGAAC CGTGCATTACC-3¢, and labeled with [a-32

P]dCTP using a Megaprime labeling kit (Amersham Pharmacia, Piscataway,

NJ, USA) Hybridization signals were detected with a

BAS-2000 bio-imaging analyzer (Fuji Film, Tokyo, Japan)

Expression of the Sll1330 protein in E coli

Overexpression of Sll1330 was carried out as described pre-viously [40] with some modification The sll1330 gene was cloned from PCC 6803 genomic DNA after PCR amplifica-tion using specific oligonucleotides The sll1330 gene was amplified using primers 1330OX-F (5¢-GTCTAGACAT ATGAATCCAG-3¢), comprising nucleotides )10 to +10

of the sll1330 coding region, and 1330OX-R (5¢-CGGGA TCCAGGGTAACAGGTTTCTCCG-3¢), comprising nucle-otides +704 to +730 of the sll1330 coding region NdeI and BamHI sites were introduced into the 1330OX-F and 1330OX-R primers, respectively (underlined)

EMSA

A 135-bp DNA fragment, prom1, corresponding to posi-tions )86 to +49 upstream of the translation initiation site

of the fbaA gene was amplified, using forward primer 5¢-GCAGAAACTAGCCTAAGATG-3¢ and reverse primer 5¢-CCATTTTCCGCCGCATGGTC-3¢ A 121-bp DNA fragment, prom2, corresponding to positions )190 to )70 upstream of the translation initiation site of the fbaA gene was amplified with forward primer 5¢-CTCAGCCATAGA CTAGGGTG-3¢ and reverse primer 5¢-ATCTTAGGCTA GTTTCTGC-3¢ A 126-bp fragment, prom3, corresponding

to positions)311 to )186 upstream of the translation initi-ation site of the fbaA gene was amplified with forward

reverse primer 5¢-CTGAGTTAACCAAGTCCAGG-3¢ A

134 bp DNA fragment, prom4, corresponding to positions )438 to )305 upstream of the translation initiation site of the fbaA gene was amplified with forward primer 5¢-CA

5¢-CCTTAGCGACGGCAATGGTC-3¢ EMSA was carried out as described previously [41]

Acknowledgements

The authors are indebted to Dr S Fujiwara for helpful discussion and Mr N J Halewood for his kind help in the correction of the English They are also indebted

to Mr Masato Sasahara, Ms Yuka Katsuki and

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