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In Drosophila melanogaster, we cloned a second PCNA cDNA that differs from that encoded by the gene mus209 for convenience called DmPCNA1 in this article.. The second PCNA cDNA DmPCNA2 e

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antigen (PCNA2) from Drosophila melanogaster

Tatsushi Ruike1, Ryo Takeuchi1, Kei-ichi Takata1,2, Masahiko Oshige1,3, Nobuyuki Kasai1,

Kaori Shimanouchi1, Yoshihiro Kanai1, Ryoichi Nakamura1, Fumio Sugawara1 and

Kengo Sakaguchi1

1 Department of Applied Biological Science, Faculty of Science and Technology, Tokyo University of Science, Japan

2 University of Pittsburgh Cancer Institute, Hillman Cancer Center, PA, USA

3 Department of Biochemistry and Molecular Biology, Indiana University School of Medicine, IN, USA

In eukaryotes, proliferating cell nuclear antigen

(PCNA), a trimeric and ring-shaped protein, is involved

in various nuclear events During chromosomal DNA

replication, PCNA is loaded onto DNA by the

repli-cation factor C complex and acts as a DNA sliding

clamp for DNA polymerase d [1] and DNA polymerase

e [2] PCNA also participates in the DNA repair

machinery with multiple binding partners such as

Xero-derma pigmentosumG (XP-G), apurinic⁄ apyrimidinic

(AP) endonucleases, DNA glycosylases, and translesion

DNA synthesis polymerases [3] Other studies have

demonstrated the interaction of PCNA with proteins

that contribute to cell cycle regulation [4], DNA

methy-lation [5] and chromatin remodeling [6]

In Drosophila melanogaster, DmPCNA1 is encoded

by the gene mus209 [7] Most mus209 mutants show

nonconditional lethality However, some mus209 mutant alleles show a temperature-sensitive phenotype, and are hypersensitive to methyl methanesulfonate (MMS) and ionizing radiation, reflecting the participa-tion of DmPCNA1 in DNA repair [8] In addiparticipa-tion, DmPCNA1 gene expression is controlled by the DNA replication-related element (DRE)⁄ DRE-binding factor (DREF), or DRE⁄ DREF system [9], which is respon-sible for activating the promoters of the 180 and

73 kDa subunits of DNA polymerase a and cyclin A, among others Therefore, like other eukaryotic PCNAs, DmPCNA1 is also closely linked to chromo-somal DNA replication and cell cycle progression Recently, two or three types of PCNA have been identified in archaeans such as Aeropyrum pernix, Pyrococcus furiosus and Sulfolobus solfataricus [10–12]

Keywords

DNA repair; Drosophila melanogaster;

proliferating cell nuclear antigen; sliding

clamp

Correspondence

K Sakaguchi, Department of Applied

Biological Science, Faculty of Science and

Technology, Tokyo University of Science,

2641 Yamazaki, Noda-shi, Chiba-ken 278,

Japan

Fax: +81 471 23 9767

Tel: +81 471 24 1501

E-mail: kengo@rs.noda.tus.ac.jp

(Received 09 August 2006, revised 14

Sep-tember 2006, accepted 18 SepSep-tember 2006)

doi:10.1111/j.1742-4658.2006.05504.x

The eukaryotic DNA polymerase processivity factor, proliferating cell nuc-lear antigen, is an essential component in the DNA replication and repair machinery In Drosophila melanogaster, we cloned a second PCNA cDNA that differs from that encoded by the gene mus209 (for convenience called DmPCNA1 in this article) The second PCNA cDNA (DmPCNA2) enco-ded a 255 amino acid protein with 51.7% identity to DmPCNA1, and was ubiquitously expressed during Drosophila development DmPCNA2 was localized in nuclei as a homotrimeric complex and associated with Drosophila DNA polymerase d and e in vivo Treatment of cells with methyl methanesulfonate or hydrogen peroxide increased the amount of both DmPCNA2 and DmPCNA1 associating with chromatin, whereas exposure to UV light increased the level of association of only DmPCNA1 Our observations suggest that DmPCNA2 may function as an independent sliding clamp of DmPCNA1 when DNA repair occurs

Abbreviations

GST, glutathione-S-transferase; MMS, methyl methanesulfonate; PCNA, proliferating cell nuclear antigen; S2 cells, Drosophila Schneider 2 cells.

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and in higher plants such as carrots [13] In contrast, it

is known that several sequences homologous to PCNA

are present in mammalian genomes, although they are

reportedly pseudogenes [14,15]

In the present study, we identified and characterized

a second Drosophila PCNA (DmPCNA2) DmPCNA2

was present as a 29 kDa protein product and localized

in nuclei as a homotrimer in a similar fashion to

DmPCNA1 Both MMS and hydrogen peroxide

(H2O2) treatments increased the level of DmPCNA2

associating with chromatin, suggesting that

DmPCNA2 may be another sliding clamp involved in

the repair of MMS- and H2O2-induced DNA lesions

Results

Molecular cloning of Drosophila PCNA2

The studies on PCNA in archaeans and higher plants

suggest that some organisms may have several PCNA

proteins [10–13] A search of the Drosophila genome

sequence database [16] identified a gene, listed as

CG10262 in FlyBase, that has homology to

DmPCNA1, the original Drosophila PCNA encoded by

mus209 [7] According to the genome sequence

data-base, this PCNA-like gene is located at 37F2 on the

long arm of chromosome 2 and is composed of two exons and one intron In comparison, the DmPCNA1 gene is located at 56F11 on the short arm of chromo-some 2 and is composed of two exons and one intron

We cloned the cDNA of this PCNA-like gene, design-ated as DmPCNA2 in this study, by RT-PCR ampli-fication and determined the 5¢- and 3¢-termini of the gene by 5¢- and 3¢-RNA ligase mediated rapid amplifi-cation of cDNA elements (RLM-RACE) analysis The cDNA of the DmPCNA2 gene was 1019 bp in length, and had a Drosophila consensus sequence for transla-tion initiatransla-tion, 5¢-(C ⁄ A)AA(A ⁄ C)ATG, and a putative poly(A) addition signal sequence, 5¢-AATAAA [17,18]

It encoded a predicted product of 255 amino acids with a molecular mass of 28.5 kDa, and showed 51.7% sequence identity with DmPCNA1 Addition-ally, it showed 44.7% sequence identity to the human PCNA and 40.7% to Schizosaccharomyces pombe PCNA, whereas DmPCNA1 shows 70.7% and 49.6% identity, respectively The nucleotide sequence data

of DmPCNA2 cDNA have been submitted to the DDBJ⁄ EMBL ⁄ GenBank nucleotide sequence data-bases (accession number: AB195794)

We carried out a multiple sequence alignment of DmPCNA2 and DmPCNA1 to identify conserved structural domains in the two proteins (Fig 1)

Fig 1 Amino acid sequence alignment of Drosophila melanogaster proliferating cell nuclear antigen 2 (DmPCNA2) and DmPCNA1 Identical and similar amino acid residues are boxed in black and gray, respectively The interdomain connecting loop and the C-terminal tail, known to

be important for interaction of PCNA-binding proteins, are indicated The DmPCNA2 polypeptide lacked amino acid residues from positions

190 to 194 of DmPCNA1, which corresponds to part of the D2E2loop.

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Eukaryotic PCNA proteins have an interdomain

connecting loop that interacts with proteins such as

DNA polymerase d, flag endonuclease 1 (FEN-1), and

XP-G, and also a C-terminal tail that interacts with

DNA polymerase e and replication factor C [3] These

regions are conserved in both DmPCNA2 and

DmPCNA1, but a small region of the D2E2 loop is

absent in DmPCNA2 [19] According to previous

stud-ies, PCNAs from several archaeans (A pernix,

P furiosusand S solfataricus) also lack the D2E2loop

[10–12] The biophysical role of this loop is still

unknown

Analysis of DmPCNA2 expression during

Drosophila development

In Drosophila, DmPCNA1 is highly transcribed in

pro-liferating tissues [20], and its transcription is controlled

by the transcription factors DREF and early region 2

transcription factor (E2F) [9,21] These transcription

factors regulate the expression of DNA replication- and

cell proliferation-related genes To investigate the

biolo-gical role of DmPCNA2, we first performed northern

hybridization experiments on a range of Drosophila

developmental stages A high level of expression of

DmPCNA1was detected in embryos at 0–2 and 8–12 h

of development; moderate expression was present in

unfertilized eggs, 4–8 and 12–16 h embryos, and adult

females, and in Kc cells (Fig 2A) Similar results were

found in a previous study [20] In contrast to the

expres-sion pattern of DmPCNA1, it was difficult to detect a

DmPCNA2signal at any developmental stage (Fig 2A)

We therefore carried out an RT-PCR screen for

DmPCNA2 expression in the different stages of

Dro-sophila development Expression levels were compared

in the linear range of RT-PCR amplification As shown

in Fig 2B, a DmPCNA2 cDNA-specific band was

vis-ible ubiquitously throughout Drosophila development

To determine whether the putative DRE and E2F

sites found in DmPCNA1 were present in the

5¢-upstream region of DmPCNA2, we isolated genomic

DNA from adult Drosophila and cloned the

5¢-upstream region (approximately 1000 bp) of the

DmPCNA2gene We searched this 1000 bp nucleotide

sequence using genetyx-mac v 9 processing software

but did not find either a DRE site (5¢-TATCGATA-3¢)

or an E2F site (5¢-TATCCCGC-3¢) in the 5¢-upstream

region of the DmPCNA2 gene

Next, we sought to detect endogenous DmPCNAs

by antibodies raised against peptides unique to either

DmPCNA2 or DmPCNA1 Using specific antibodies

for DmPCNA2 or DmPCNA1, protein bands of

approximately 29 or 35 kDa, respectively, were

observed in western blots of Drosophila Schneider 2 (S2) cells (Fig 2C) In contrast, no significant staining was detectable with preimmune rabbit IgG Further-more, using anti-Flag serum, protein bands of approxi-mately 30 or 36 kDa, respectively, were also observed

in western blots of S2 cells that have stable expression

of Flag-tagged DmPCNA2 or Flag-tagged DmPCNA1 (Fig 2C)

Analysis of trimer formation by DmPCNA2 and DmPCNA1

As PCNA forms a ring-shaped homotrimer with a central cavity [19], we analyzed the homotrimeri-zation of DmPCNA2 and its heterotrimerihomotrimeri-zation with DmPCNA1 We first produced recombinant proteins and purified these to near homogeneity The purified DmPCNA2⁄ T7-(His)6 eluted as a single peak with a calculated molecular mass of 100 kDa in a Sephacryl S-300 gel filtration column, as also did DmPCNA1⁄ T7-(His)6 (Fig 3A) This result suggests that DmPCNA2 is able to form a homotrimer We therefore simulated the three-dimensional structures of DmPCNA2 and DmPCNA1, using the data from human PCNA (Fig 3B) The possible structures of the DmPCNA2 homotrimer resemble that of the DmPCNA1 homotrimer, except for the small region of the D2E2 loop This loop in DmPCNA2 was shorter than that in DmPCNA1

The simulation of the possible structure of the DmPCNA2 homotrimer suggests that the sizes of the homotrimers of DmPCNA2 and DmPCNA1 are sim-ilar We therefore investigated whether DmPCNA2 could form a heterotrimer complex with DmPCNA1

We performed a glutathione-S-transferase (GST) pull-down experiment using DmPCNA2⁄ GST or DmPCNA1⁄ GST and DmPCNA2⁄ T7-(His)6 or DmPCNA1⁄ T7-(His)6 The indicated GST fusion pro-teins and T7-(His)6-tagged proteins of DmPCNAs were mixed in NaCl⁄ Pi (lanes 1–5 in Fig 4A), incubated at

4C for 12 h, and precipitated with GST Sepharose-4B beads Under these conditions, however, we were unable even to find an interaction of DmPCNA1 with itself (lane 3 in Fig 4A) Unsurprisingly, therefore, we could not detect an interaction between DmPCNA2 and DmPCNA1 (lanes 4 and 5 in Fig 4A) It is poss-ible that both DmPCNA2 and DmPCNA1 might already have been present as homotrimers prior to mixing and that they could not exchange monomers under the experimental conditions used Therefore,

we sought to reconstitute the trimeric forms of DmPCNAs When the proteins were forced to disso-ciate to the monomeric state by incubation at 4C for

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6 h in NaCl⁄ Pi containing 0.1% Tween-20, followed

by dialysis at 4C for 6 h in NaCl ⁄ Pi, DmPCNA2

could form a heterotrimeric complex with DmPCNA1

in vitro(lanes 9 and 10 in Fig 4A)

Next, we used an immunoprecipitation assay to

determine whether DmPCNA2 and DmPCNA1 could

form a heterotrimer in vivo As we could not detect

endogenous DmPCNA2 in the crude extracts from S2

cells unless SuperSignal West Femto Maximum was used as the chemiluminescence reagent (Fig 2C), we considered that further analyses of endogenous DmPCNA2 with anti-DmPCNA serum were impracti-cal Therefore, using the Drosophila Expression Sys-tem, we carried out an immunoprecipitation using S2 cells that stably expressed V5-tagged DmPCNA1 and Flag-tagged DmPCNA1, V5-tagged DmPCNA2 and

C

Fig 2 Expression of Drosophila melanogaster PCNA2 (DmPCNA2) during Drosophila development (A) Northern hybridization analysis 3¢-UTRs of DmPCNA2 and DmPCNA1 cDNAs (33.6% nucleotide sequence homology) were used as specific probes RP-49 mRNA served

as a loading control (B) RT-PCR analysis of DmPCNA2 Expression of Act5C was used as an internal control; expression of DmPCNA1 was also analyzed to ensure that RT-PCR reflected the results of the northern hybridization The cycle numbers used are indicated NC is the neg-ative control (C) Western blotting analysis of endogenous DmPCNAs Crude extracts from Drosophila Schneider 2 (S2) cells were separated

by 12.5% SDS⁄ PAGE and blotted with preimmune rabbit IgG (left panel) serum, DmPCNA2 serum (second panel from the left), or anti-DmPCNA1 serum (middle panel) The 29 kDa protein band of DmPCNA2 and the 35 kDa protein band of anti-DmPCNA1 are indicated by arrows Crude extracts from S2 cells expressing Flag-tagged DmPCNA2 (second panel from the right) or Flag-tagged DmPCNA1 (right panel) were separated by 12.5% SDS ⁄ PAGE and blotted with anti-Flag serum The 30 kDa protein band of Flag-tagged DmPCNA2 and the 36 kDa pro-tein band of Flag-tagged DmPCNA1 are indicated by arrows The sizes of the molecular mass markers are indicated on the left.

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Flag-tagged DmPCNA2, or V5-tagged DmPCNA1

and Flag-tagged DmPCNA2 We detected interactions

between DmPCNA1 molecules and between

DmPCNA2 molecules with V5 and Flag tags, but

found no evidence of an interaction between

DmPCNA2 and DmPCNA1 (Fig 4B) These data

sug-gest that DmPCNA2 can only form a homotrimer

in vivo, and that the heterotrimerization in vitro may

be an artificial event

Association of DmPCNA2 with Drosophila DNA

polymerases d and e

PCNA was originally identified as a DNA sliding

clamp for DNA polymerases [22] In humans, PCNA

associates with the p120 catalytic subunit of DNA

polymerase d through interaction with the p66 third

subunit [23] In Schizosaccharomyces pombe, PCNA

interacts with the Pol2p catalytic subunit of DNA polymerase e [24] We therefore tested whether DmPCNA2 could associate with the catalytic subunits

of Drosophila DNA polymerase d and DNA poly-merase e We carried out an immunoprecipitation assay using crude extract from S2 cells that had stable expression of V5-tagged DmPCNA2 As shown in Fig 5, both DNA polymerase d and DNA polymerase

e are precipitated with anti-V5 serum, indicating that DmPCNA2 can associate with DNA polymerase d and DNA polymerase e in vivo

Properties of binding of DmPCNA2 and DmPCNA1 to chromatin damaged by various mutagens

As described earlier, PCNA is involved in DNA repair [3] In humans, the amount of PCNA binding to

A

B

Fig 3 Homotrimer formation of Drosophila melanogaster proliferating cell nuclear anti-gen 2 (DmPCNA2) (A) Gel filtration chroma-tography analysis Two hundred micrograms

of purified DmPCNA2 ⁄ T7-(His) 6 or DmPCNA1 ⁄ T7-(His) 6 was loaded onto a Sephacryl S300 gel filtration column The cir-cle indicates the position of the maximum peak at which DmPCNA2 (left panel) or DmPCNA1 (right panel) was found Molecu-lar mass standards (open squares) used were ferritin (440 kDa), aldolase (158 kDa), albumin (67 kDa), ovalbumin (43 kDa) and ribonuclease A (13.7 kDa) (B) Building of a model of a ring-shaped, three-dimensional structure of DmPCNA2 (left panel) and DmPCNA1 (right panel): upper panel, back view; lower panel, side view In the dia-grams for DmPCNA1, purple balls represent amino acid residues from 190 to 194 that are present in DmPCNA1 but absent from DmPCNA2.

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chromatin increases in cells treated with mutagens such

as MMS [25], H2O2 [26] and UV light [27] We

there-fore examined the association of DmPCNA2 and

DmPCNA1 with chromatin following treatment with

DNA-damaging agents First, we visualized the

sub-cellular localization of V5-tagged DmPCNA2 and

Flag-tagged DmPCNA1 in S2 cells using

immunofluo-rescence microscopy We found that both DmPCNA2

and DmPCNA1 were localized in the nucleus

(Fig 6A) Next, we prepared fractions from the

cyto-plasm, the whole chromatin, a high-salt wash and the

core nuclear matrix from S2 cells As controls for the

fractionation procedure, we used western blotting with

antibodies against b-tubulin (a nonchromatin-bound

protein) and histone H4 (a chromatin-bound protein)

DmPCNA2 and DmPCNA1 were present in the

cyto-plasmic and the whole chromatin fractions (Fig 6B)

Following exposure to DNA-damaging agents, both

DmPCNA2 and DmPCNA1 showed increased levels

of association with chromatin, with a time-dependent relationship (Fig 6C) The level of DmPCNA2 in the whole chromatin fraction reached a maximum at 5–8 h after MMS treatment and at 3 h after H2O2treatment (Fig 6C) In contrast, the amount of DmPCNA1 in this fraction continued to increase up to 8 h after MMS treatment and 5 h after H2O2 treatment (Fig 6C) UV light treatment increased the level

of DmPCNA1 associating with chromatin but not of DmPCNA2 Mitomycin C did not alter the levels

of either DmPCNA2 or DmPCNA1 associating with chromatin We also investigated the binding of DmPCNA2 to chromatin after treatment with various doses of DNA-damaging agents (Fig 6D) MMS-trea-ted S2 cells were collecMMS-trea-ted 5 h after treatment, and S2 cells treated with H2O2, UV light or mitomycin C were harvested at 3 h The amounts of DmPCNA2 in the whole chromatin fractions increased in a dose-depend-ent fashion after MMS and H2O2treatments, but were

A

B

Fig 4 Interaction of Drosophila

melano-gaster proliferating cell nuclear antigen 2

(DmPCNA2) and DmPCNA1 (A) In vitro

interaction of DmPCNA2 and DmPCNA1.

Lanes 1–5: the indicated proteins were

mixed in NaCl ⁄ P i at 4 C for 12 h Lanes

6–10: the indicated proteins were mixed in

NaCl⁄ P i containing 0.1% Tween-20 at 4 C

for 6 h, and this was followed by dialysis in

NaCl⁄ P i at 4 C for 6 h The proteins bound

to GST Sepharose-4B beads were analyzed

by western blotting with anti-T7 or anti-GST

serum (B) In vivo interaction between

DmPCNA2 and DmPCNA1 Drosophila

Schneider 2 (S2) cells expressing the

indica-ted DmPCNAs were harvesindica-ted and lysed.

The lysates were immunoprecipitated (IP)

with anti-V5 serum The washed

immuno-precipitates were separated by 12.5%

SDS ⁄ PAGE and blotted for either Flag or V5

(left panel) The lysates were

immunoprecip-itated with anti-Flag serum and blotted

sequentially for V5 or Flag (right panel).

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not influenced by UV light or mitomycin C treatments

(Fig 6D)

Discussion

In this study, we identified a second PCNA cDNA

from Drosophila melanogaster This PCNA, which we

call here DmPCNA2, had two conserved regions, an

interdomain connecting loop and a C-terminal tail

DmPCNA2 formed homotrimers and associated with

DNA polymerase d and DNA polymerase e in vivo In

addition, DmPCNA2, as well as DmPCNA1, was

present in the whole chromatin fraction of cellular

proteins Taken together, these results suggest that

DmPCNA2 can act as a DNA sliding clamp for these

DNA polymerases

Yamaguchi and colleagues reported that the

expres-sion of DmPCNA1 is controlled by the transcription

factors DREF and E2F, which are abundant in tissues

such as the ovary and in unfertilized eggs and early

embryos [9,21] Thus, DmPCNA1 mRNA is highly

expressed in proliferating tissues and decreases rapidly

during development [20] In contrast to DmPCNA1,

there was no evidence for putative binding sites for DREF and E2F in the 5¢-upstream region of DmPCNA2 Moreover, DmPCNA2 was constantly expressed even in pupae in which few cells are pro-liferating These data suggest that expression of DmPCNA2might not be related to cell proliferation

We found different patterns of binding to chromatin between DmPCNA2 and DmPCNA1 in S2 cells trea-ted with DNA-damaging agents MMS and H2O2 induced a more rapid association of DmPCNA2 with chromatin than of DmPCNA1 UV light induced the association of DmPCNA1 with chromatin, but not of DmPCNA2 These results suggest that each DmPCNA functions independently when DNA is damaged It has been reported that PCNA cannot load itself onto DNA in vitro and requires a clamp loader protein to achieve this association [28,29] Therefore, the patterns

of association of DmPCNA2 and DmPCNA1 with chromatin might reflect differential loading onto dam-aged DNA by clamp loaders DmPCNA1 probably functions in the repair of MMS-, H2O2- and UV light-induced lesions in a similar manner to other eukaryotic PCNAs In eukaryotes, base excision repair is known

to be the major pathway for repair of MMS- and

H2O2-induced DNA lesions and is often initiated by several DNA glycosylases [30] In S pombe, PCNA and Rad9⁄ Rad1 ⁄ Hus1 differentially participate in base excision repair through interaction with the DNA gly-cosylase MutY homolog [31] Although the precise function of DmPCNA2 remains unclear, one hypothe-sis is that DmPCNA2 might participate in the base excision repair pathway through interaction with some

of the Drosophila DNA glycosylases Another possibil-ity is that DmPCNA2 might simply support DmPCNA1 in the repair of MMS- and H2O2-induced DNA damage

Our next task in the near future will be to elucidate how DmPCNA2 functions in the DNA repair system The analysis of flies with mutation of DmPCNA2 will help us to understand its biophysiologic roles as well

as enable identification of the DmPCNA2 binding partners

Experimental procedures

Cloning of DmPCNA2

Total RNA from Kc cells was reverse transcribed using the SuperScript First-Strand Synthesis System (Invitrogen, Car-lsbad, CA) with an oligo-(dT)12)18primer Amplification of the DmPCNA2 cDNA was performed using ExTaq thermo-stable DNA polymerase (TaKaRa, Ohtsu, Japan) and the following primers: forward, 5¢-ATGCTCGAGGCGCGTT

Fig 5 Association of Drosophila melanogaster proliferating cell

nuclear antigen 2 (DmPCNA2) with DNA polymerase d (Dmpol d)

and Dmpol e Drosophila Schneider 2 (S2) cells expressing

V5-tagged DmPCNA2 were harvested and lysed The lysates were

immunoprecipitated (IP) with anti-V5 serum The washed

immuno-precipitates were separated by 5% SDS ⁄ PAGE and analyzed by

western blotting with anti-Dmpol d, anti-Dmpol e or anti-V5 serum.

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A B

D C

Fig 6 Chromatin-binding patterns of Drosophila melanogaster proliferating cell nuclear antigen 2 (DmPCNA2) and DmPCNA1 in response to DNA-damaging agents (A) Immunofluorescent analysis of the localization of V5-tagged DmPCNA2 and Flag-tagged DmPCNA1 DmPCNA2 is shown in red, DmPCNA1 in green, and DNA in blue after DAPI staining Bar represents 5 lm (B) Fractionation of DmPCNA2 and DmPCNA1 Drosophila Schneider 2 (S2) cells expressing V5-tagged DmPCNA2 and Flag-tagged DmPCNA1 were extracted to obtain cyto-plasmic, whole chromatin, high-salt-wash and core nuclear matrix fractions The fractions were analyzed by western blotting with the indica-ted antibodies (C) Chromatin binding of DmPCNA2 and DmPCNA1 in response to DNA-damaging agents [0.02% methyl methanesulfonate (MMS), 1.5 m M H2O2, 35 JÆm)2UV light and 0.02% mitomycin C (MMC)] S2 cells were collected at the indicated post-treatment intervals (D) Chromatin binding of DmPCNA2 after various doses of DNA-damaging agents S2 cells were treated with MMS (concentration range 0.01–0.1%), H 2 O 2 (concentration range 0.5–2.5 m M ), UV light (dose range 15–70 JÆm)2) or MMC (concentration range 0.01–0.1%) The chro-matin fractions were analyzed by western blotting with anti-V5 serum.

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TGAG-3¢; and reverse, 5¢-CTAGAAATCGGGGTCATT

CA-3¢ The amplified cDNA was cloned into the pGEM-T

vector (Promega, Madison, WI) To identify the 5¢- and

3¢-termini of the gene, 5¢- and 3¢-RLM-RACE was

per-formed in accordance with the manufacturer’s

recom-mended protocol (FirstChoice RLM-RACE kit; Ambion,

Austin, TX)

Northern hybridization and RT-PCR analysis

Total RNAs were extracted using Trizol (Invitrogen) from

unfertilized Drosophila eggs, embryos, larvae, adult flies

and from Kc cells Northern hybridization was carried out

as described previously [32] The 3¢-UTR of DmPCNA2

cDNA (nucleotides 863–1019) or that of DmPCNA1

(nucle-otides 873–997) was used as the specific probe Full-length

ribosomal protein 49 (Rp-49) cDNA was used as a control

sources described above) were treated with DNase I

(TaKaRa) to remove traces of genomic DNA

contamin-ation, and purified with phenol⁄ chloroform First-strand

cDNA was synthesized from 1 lg of total RNA using

the SuperScript First-Strand Synthesis System (Invitrogen)

with random hexamers, and then amplified using the

GGGGTCATTCA-3¢; DmPCNA1 – forward, 5¢-ATGTTC

GAGGCACGCCT-3¢, and reverse, 5¢-TTATGTCTCGTT

TCCCGACA-3¢, and reverse, 5¢-ATCCCGATCCTGAC

TCTT-3¢ The PCR conditions were: DmPCNA2 – 94 C

for 5 min, 94C for 45 s, 55 C for 45 s, 72 C for 1 min,

24 cycles, 5 min extension at 72C; DmPCNA1) 94 C

for 5 min, 94C for 45 s, 55 C for 45 s, 72 C for 1 min,

21 cycles, 5 min extension at 72C; Act5c) 94 C for

5 min, 94C for 45 s, 55 C for 45 s, 72 C for 1 min 30 s,

17 cycles, 5 min extension at 72C PCR products were

visualized by staining with SYBR Gold nucleic acid gel

stain (Molecular Probes, Eugene, OR) after agarose gel

electrophoresis

Generation of antibodies to DmPCNA2 and

anti-DmPCNA1

A keyhole limpet haemocyanin (KLH)-conjugated

syn-thetic peptide with an extra cysteine on the N-terminus

DmPCNA2) or (CKLAQTGSVDKEEEA, amino acids

181–194 of DmPCNA1) was used for inoculation into

rab-bits (Bio Matrix Research, Kashiwa, Japan) For detection

of endogenous DmPCNA2, anti-DmPCNA2 serum or

pre-immune rabbit IgG diluted to 0.5 lgÆmL)1 served as

pri-mary antibodies Horseradish peroxidase-conjugated goat

anti-(rabbit IgG) (Vector Laboratories, Burlingame, CA)

diluted to 2 ngÆmL)1 served as the secondary antibody

Chemiluminescence was detected with SuperSignal West Femto Maximum (Pierce, Rockford, IL) For detection of endogenous DmPCNA1, anti-DmPCNA1 serum diluted

to 1 lgÆmL)1 and horseradish peroxidase-conjugated goat anti-(rabbit IgG) diluted to 50 ngÆmL)1 served as primary and secondary antibodies, respectively Chemiluminescence was detected with enhanced chemiluminescence (ECL) western blotting detection reagents (Amersham Pharmacia Biotech, Piscataway, NJ)

Animals were fed water and standard rabbit food and maintained on a 12 h light/dark cycle Polyclonal antiserum

to the peptide was raised in rabbits by subcutaneous injec-tion of 0.15 mg of the peptide emulsified in Freund’s com-plete adjuvant Two weeks after the primary injection, boosts of 0.3 mg of the peptide in Freund’s incomplete adju-vant were injected every 2 weeks The rabbits were bled one week after the final boost under anesthesia The rabbits were treated in accordance with procedures approved by the Ani-mal Ethics Committee of the Science University of Tokyo

Purification of recombinant DmPCNA2 or DmPCNA1 proteins

The DmPCNA2 coding region was cloned into pET21a (Novagen, Darmstadt, Germany) or pGEX-6P-1 vectors

over-expressed in Escherichia coli BL21 (DE3) (Novagen) and purified with His-Bind Resin according to the manufacturer’s

GST) protein was overexpressed in E coli BL21 (DE3) and purified with Glutathione Sepharose-4B (Amersham

DmPCNA1⁄ T7-(His)6protein and DmPCNA1⁄ GST protein were carried out as described above for DmPCNA2

Gel filtration column chromatography

DmPCNA1⁄ T7-(His)6 proteins were dialyzed against

pH 8.0, 5 mm 2-mercaptoethanol, 10% glycerol) containing 0.2 m NaCl A 200 lg sample of each protein was sepa-rately loaded onto a gel filtration column (Sephacryl S-300 gel column; Amersham Pharmacia Biotech) equilibrated with the same buffer The molecular mass was estimated from a calibration curve using ferritin (440 kDa), aldolase (158 kDa), albumin (67 kDa), ovalbumin (43 kDa) and ribonuclease A (13.7 kDa)

Three-dimensional structure model building

The predicted structure of the human PCNA protein was used to set the parameters for constructing models

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of DmPCNA2 and DmPCNA1 We used the swiss-model

program [33–35] to generate three-dimensional models of

the DmPCNA2 and DmPCNA1 proteins

GST pull-down assay

Equal amounts of purified GST fusion proteins and

puri-fied T7-(His)6-tagged proteins were mixed in NaCl⁄ Piand

incubated at 4C for 12 h, or mixed in NaCl ⁄ Picontaining

0.1% Tween-20 and incubated at 4C for 6 h The

mix-tures were then dialyzed in NaCl⁄ Piat 4C for 6 h GST

Sepharose-4B beads (Amersham Pharmacia Biotech) were

added to the samples, which were then incubated at 4C

for 1 h After being washed six times with 0.8 mL of

NaCl⁄ Pi, the bound proteins were eluted with TEMG

buf-fer containing 10 mm reduced glutathione and analyzed by

western blotting with mouse monoclonal antibody T7

(Novagen) and rabbit polyclonal anti-GST serum

Cell culture, plasmid construction, and

transfection

S2 cells were cultured in Schneider’s Drosophila Medium

(Invitrogen) containing 10% heat-inactivated fetal bovine

serum at 25C The expression vector for V5-tagged

DmPCNA2 was constructed by cloning the DmPCNA2

coding region into pAc5.1⁄ V5-His C (Invitrogen)

Flag-tagged DmPCNA2 was constructed by cloning the

pAc5.1⁄ V5-His C from which the V5-His tag had been

removed Expression vectors for V5-tagged DmPCNA1 and

Flag-tagged DmPCNA1 were constructed as described

above for DmPCNA2 All transfections and establishment

of the stable cell lines were performed in accordance with

the manufacturer’s protocols (Invitrogen)

Immunoprecipitation experiments

Aliquots of 1· 107S2 cells were washed in NaCl⁄ Pi and

suspended in TEMG buffer containing 0.15 m NaCl, 0.01%

NP-40, and the protease inhibitors phenylmethanesulfonyl

fluoride (1 mm), leupeptin (1 mm) and pepstatin A (1 mm)

After sonication, the lysates were rocked at 4C for

30 min, and then centrifuged at 10 000 g for 10 min

(MX-201; TOMY; TMA-29 rotor) The supernatants were

pre-cleared by treatment with protein G Sepharose beads

(Amersham Pharmacia Biotech) at 4C for 1 h Cleared

lysates were immunoprecipitated with protein G Sepharose

beads and a mouse monoclonal V5 antibody (Invitrogen)

or anti-Flag serum (Sigma, St Louis, MO) at 4C for 2 h

Immunoprecipitates were washed three times with the same

buffer, solubilized in SDS⁄ PAGE sample buffer, and

ana-lyzed by western blotting For generation of antibodies

to DNA polymerase d, the purified recombinant DNA

polymerase d fragment (amino acid residues 104–445) was used for inoculation into rabbits The generation of anti-DNA polymerase e was described in a previous report [36]

Immunofluorescence analysis

S2 cells were placed on poly-(l-lysine)-coated coverslips and fixed with 4% paraformaldehyde in NaCl⁄ Pi for

10 min at room temperature After several washes with NaCl⁄ Pi, the cells were treated with methanol for permeabi-lization The samples were incubated with primary antibod-ies, mouse monoclonal anti-V5 serum and rabbit polyclonal anti-Flag serum, at 4C overnight, and then treated for 1 h with the secondary antibodies Alexa546 anti-(mouse IgG) and Alexa488 anti-(rabbit IgG) (Molecular Probes) They were also counterstained with 4¢,6-diamidine-2-phenylindole (DAPI) The preparations were observed under a fluore-scence microscope and the data were collected using a CCD camera (Nikon, Chiyoda, Japan)

Fractionation of cellular proteins

S2 cells were exposed to MMS or mitomycin C for 1 h

or to H2O2 for 15 min The cells were then washed once and incubated prior to sampling UV-irradiated S2 cells were incubated in the dark in order to distinguish the effects of UV irradiation from those of the photoreacti-vating mechanism After incubation, S2 cells were washed three times with ice-cold NaCl⁄ Pi Aliquots of 1· 107

S2 cells were lysed in 500 lL of cytoskeleton buffer (CSK buffer: 10 mm Hepes, pH 7.4, 100 mm NaCl, 300 mm

2-mercapto-ethanol, 1 mm phenylmethanesulfonyl fluoride, 1 mm leu-peptin, 1 mm pepstatin A, 0.5% Triton X-100) at 4C for 5 min and centrifuged at 3000 g for 5 min (MX-201; TOMY; TMA-29 rotor) The soluble cytoplasmic fraction was removed, and the pellet was washed once with

500 lL of CSK buffer The pellet was then resuspended

in 200 lL of CSK buffer containing 100 U of RNase-free

sulfate was added to a final concentration of 0.25 m The samples were incubated for 5 min at 4C and centrifuged

as above The soluble chromatin fraction was removed, and the pellet was extracted in CSK buffer with 2 m NaCl for 5 min at 4C After another centrifugation, the

2 m NaCl wash was removed, and the nuclear matrix pel-let was resuspended in 50 lL of SDS⁄ PAGE sample buf-fer For western blot analysis, equal cell equivalents from each fraction were subjected to SDS⁄ PAGE and probed with appropriate antibodies: mouse monoclonal anti-V5 serum, rabbit polyclonal anti-Flag serum (Sigma), mouse monoclonal anti-b-tubulin serum (Chemicon, Temecula, CA), or rabbit polyclonal anti-Histone H4 (Imgenex, San Diego, CA)

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