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Tiêu đề Interactions of HIPPI, a Molecular Partner of Huntingtin Interacting Protein HIP1, with the Specific Motif Present at the Putative Promoter Sequence of the Caspase-1, Caspase-8 and Caspase-10 Genes
Tác giả P. Majumder, A. Choudhury, M. Banerjee, A. Lahiri, N. P. Bhattacharyya
Người hướng dẫn N. P. Bhattacharyya
Trường học Saha Institute of Nuclear Physics
Chuyên ngành Structural Genomics
Thể loại báo cáo khoa học
Năm xuất bản 2007
Thành phố Kolkata
Định dạng
Số trang 14
Dung lượng 446,3 KB

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interacting protein HIP1, with the specific motif present at the putative promoter sequence of the caspase-1, caspase-8 and caspase-10 genes P.. It was observed that the C-terminal ‘pseu

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interacting protein HIP1, with the specific motif present at the putative promoter sequence of the caspase-1, caspase-8 and caspase-10 genes

P Majumder1, A Choudhury2, M Banerjee1, A Lahiri2and N P Bhattacharyya1

1 Structural Genomics Section, Saha Institute of Nuclear Physics, Bidhan Nagar, Kolkata, India

2 Department of Biophysics, Molecular Biology and Genetics, University of Calcutta, Kolkata, India

It has been known for more than 13 years that

increased CAG repeats beyond position 36 in exon1 of

the Huntingtin (Htt) gene causes Huntington’s disease

[1], resulting in increased apoptosis in a specific region

of the brain [2] Among various interacting partners of

the protein Htt [3–5], Huntingtin interacting protein 1

(HIP1), identified in the yeast two-hybrid assay [6] and

subsequently characterized as an endocytic adaptor

protein with clatharin assembly activity, binds to

various cytoskeleton proteins [7] In the search for interacting partners of HIP1, a novel protein HIPPI (HIP1 protein interactor) has recently been identified HIPPI does not have any known domains except for a

‘pseudo’ death effector domain (pDED) and a myosin-like domain Interaction of HIPPI with HIP1 takes place through the pDED present in both proteins The HIPPI–HIP1 heterodimer recruits procaspase-8, and activates the initiator caspase and its downstream

Keywords

caspase; HIPPI; motif; pDED; transcription

regulation

Correspondence

N P Bhattacharyya, Structural Genomics

Section, Saha Institute of Nuclear Physics,

1 ⁄ AF Bidhan Nagar, Kolkata 700 064, India

Fax: +91 033 2337 4637

Tel: +91 033 2337 5345

E-mail: nitai_sinp@yahoo.com

(Received 11 April 2007, revised 1 June

2007, accepted 5 June 2007)

doi:10.1111/j.1742-4658.2007.05922.x

To investigate the mechanism of increased expression of caspase-1 caused

by exogenous Hippi, observed earlier in HeLa and Neuro2A cells, in this work we identified a specific motif AAAGACATG () 101 to ) 93) at the caspase-1 gene upstream sequence where HIPPI could bind Various muta-tions in this specific sequence compromised the interaction, showing the specificity of the interactions In the luciferase reporter assay, when the reporter gene was driven by caspase-1 gene upstream sequences () 151 to ) 92) with the mutation G to T at position ) 98, luciferase activity was decreased significantly in green fluorescent protein–Hippi-expressing HeLa cells in comparison to that obtained with the wild-type caspase-1 gene

60 bp upstream sequence, indicating the biological significance of such binding It was observed that the C-terminal ‘pseudo’ death effector domain of HIPPI interacted with the 60 bp () 151 to ) 92) upstream sequence of the caspase-1 gene containing the motif We further observed that expression of caspase-8 and caspase-10 was increased in green fluores-cent protein–Hippi-expressing HeLa cells In addition, HIPPI interacted

in vitrowith putative promoter sequences of these genes, containing a sim-ilar motif In summary, we identified a novel function of HIPPI; it binds to specific upstream sequences of the caspase-1, caspase-8 and caspase-10 genes and alters the expression of the genes This result showed the motif-specific interaction of HIPPI with DNA, and indicates that it could act as transcription regulator

Abbreviations

DED, death effector domain; EMSA, electrophoretic mobility shift assay; GFP, green fluorescent protein; GST, glutathione S-transferase;

HD, Huntington’s disease; HIP1, Huntingtin interacting protein 1; HIPPI, Huntingtin interacting protein 1 protein interactor; Htt, Huntingtin; IOD, integrated optical density; pDED, ‘pseudo’ death effector domain; TSS, transcription start site.

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apoptotic cascades [8,9] It has been shown earlier that

the interaction of HIP1 with normal Htt (a protein with

fewer than 36 Gln) is stronger than that observed with

the mutated Htt (a protein with more than 36 Gln

resi-dues) [10] On the basis of this observation, it has been

proposed that the weaker interaction of HIP1 with

mutated Htt in Huntington’s disease (HD) may

increase the amount of freely available HIP1 and

enhance the propensity for the HIP1–HIPPI

heterodi-mer to form The increased amount of HIP1–HIPPI

may in turn lead to the increase in cell death observed

in HD [8] A role of HIPPI in apoptosis regulation has

also been inferred from other studies Apoptin, a

chicken anemia virus-encoded protein, has been shown

to colocalize with HIPPI in the cytoplasm of normal

cells, whereas in tumor cells the two proteins localize

separately in the nucleus and cytoplasm It has been

proposed that the HIPPI–apoptin interaction may

suppress apoptosis [11] The bifunctional apoptosis

inhibitor, which regulates neuronal apoptosis, also

interacts with HIPPI, although the functional relevance

of this interaction remains unknown [12] Very recently,

it has been reported that HIPPI interacts with the

postsynaptic scaffold protein Homer1c and regulates

apoptosis in striatal neurons [13] All these studies

show that HIPPI, through its interacting partner,

regulates apoptosis Even though the exact function of

HIPPI remains unknown, it has been shown, using

knockout mouse (Hippi–⁄ –), that HIPPI is involved the

Sonic hedgehog signaling pathway [14]

Interactions of several transcription factors with Htt

and alterations of a large number of genes observed in

microarray studies support the hypothesis that the

pathology of HD is mediated through alterations in

transcription [15] In several studies using cellular and

animal models of HD (where the mutated full-length

Htt gene or exon1 are expressed by knockin), the

expression of the caspase-1, caspase-3, caspase-2,

caspase-6 and caspase-7 genes is increased [16,17] How

the expression of these genes is altered is not known

We have previously shown that exogenous

expres-sion of Hippi increases various apoptotic markers In

the course of this study, it was also observed that the

endogenous expression of caspase-1, caspase-3 and

caspase-7 is upregulated in green fluorescent protein

(GFP)–Hippi-expressing cells, whereas the

mitochond-rial genes ND1 and ND4 and the antiapoptotic gene

Bcl-2 are downregulated [9] Recently, we have also

shown that HIPPI can directly interact with the

ca-spase-1 gene upstream 60 bp sequence () 151 to ) 92)

in vitro and in vivo [18] In the present investigation,

we identified and characterized a motif within this

60 bp sequence of the caspase-1 gene where HIPPI

could bind specifically In addition, we observed that a similar motif was present at the putative promoter sequences of the caspase-8 and caspase-10 genes; the expression of these genes was also increased in GFP– Hippi-expressing HeLa cells In vitro experiments showed that HIPPI also interacted with the promoter sequences of these genes

Results

Specific motif at the upstream sequences

of the caspase-1 gene

To search for the specific DNA sequence motif where HIPPI might interact, we analyzed 1 kb upstream regions of the caspase-1, caspase-3 and caspase-7 genes using four different motif prediction algorithms, i.e meme, alignace, bioprospector and mdscan The motifs predicted using the different methods, parame-ters and sequence sets (masked⁄ unmasked) were then assembled and compared, and the redundant motifs were discarded (data not shown) The motif pre-dicted using the methods mentioned was 5¢-AA AGA[CG]A[TA][GT]-3¢ We investigated whether any similar motif was present within the 60 bp stretch of the caspase-1 gene upstream sequence where HIPPI actually interacted [18] It was observed that the motif 5¢-AAAGACATG-3¢ () 101 to ) 93) was present in the positive strand of the caspase-1 gene upstream sequence This motif was conserved in promoters of caspase-1 orthologs from Pan troglodytes (DOOP ID:

83123145,) 245 to ) 253) and Macaca mulatta (DOOP ID: 94252893, ) 245 to ) 253) The motif sequences

of the caspase-3 gene (5¢-AAAGAGATG-3¢, ) 828 to ) 820) and the caspase-7 gene (5¢-AAAGACATA-3¢, ) 245 to ) 253) were present in the positive strand In subsequent studies, we tested whether HIPPI could interact with the 5¢-AAAGACATG-3¢ () 101 to ) 93) motif present in the putative promoter of the caspase-1 gene

Interactions of HIPPI with AAAGACATG and various mutants of this sequence at the caspase-1 gene upstream sequence The specific sequence AAAGACATG identified within the 60 bp upstream sequence was used to test whether HIPPI interacted with this motif The results of a typical electrophoretic mobility shift assay (EMSA) experiment carried out using the above-mentioned sequence and its mutants (mutations at the fourth, fifth and sixth positions) are shown in Fig 1A A mobility shift of the band corresponding to [32P]ATP[cP]-labeled

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dsDNA, AAAGACATG, in the presence of

gluta-thione S-transferase (GST)–HIPPI (Fig 1A, panel I,

lane 3) indicated interaction of the purified protein

with the motif No shift was observed in the presence

of GST protein only (lane 2)

EMSA with mutants of the 9 bp motif AAAGA

CATG indicated that AAAGAGATG (mutation of

the sixth nucleotide, C to G) interacted with the GST–

HIPPI, as is evident from the mobility shift of the

band corresponding to radiolabeled dsDNA in the

presence of purified protein (Fig 1A, panel II, lanes 3

and 4) However, mutation at the fourth nucleotide

(G to T) and fifth nucleotide (A to C) affected the

interaction In both cases, there was no shift of the

probe, as shown in lane 2 and lane 6, indicating that

GST–HIPPI did not interact with these mutated

motifs

A similar result was also obtained in the

fluores-cence quenching study (Fig 1B, panel I) With

AAAGAGATG), the fluorescence (kemission¼ 340 nm,

kexcitation¼ 295 nm) of GST–HIPPI protein was

reduced and reached a plateau The value of the

dissociation constant, determined from the plateau

region, obtained with AAAGACATG was calculated

to be 1.2 nm (Fig 1C, panel I) A similar result was

obtained with AAAGAGATG, with a dissociation

constant of 0.3 nm (Fig 1C, panel II) A fluorescence

quenching assay with the DNA AAAGACACG (point

mutation at the eighth position T to C of the predicted

motif mentioned above) revealed a decrease in the

intrinsic fluorescence of GST–HIPPI protein,

indica-ting binding of the protein with this mutated motif

(Fig 1B, panel II) The apparent dissociation constant

(Kd) of this binding was 4 nm (Fig 1C, panel III)

However, a similar assay with AAATACATG and

AAAGCCATG did not alter the GST–HIPPI

fluores-cence significantly (Fig 1B, panel I), which further

supported the results of EMSA with the same DNA

sequences, discussed before (Fig 1A, panel II) Further

point mutations at the second (A to G), third (A to

G), seventh (A to C) and ninth (G to A) nucleotides

of the 9 bp motif AAAGACATG and a subsequent

fluorescence quenching study indicated no significant

quenching of fluorescence of GST–HIPPI in the

pres-ence of these mutants This result revealed that GST–

HIPPI did not interact with these mutated sequences

of the 9 bp motif (Fig 1B, panel II)

To explore the nature of the interactions of GST–

HIPPI with AAAGACATG, we increased the

concen-tration of NaCl from 50 mm (normally used in all

binding assays) to 1000 mm As is evident from Fig 2,

with the increasing concentrations of NaCl, the

fluor-escence intensities of GST–HIPPI increased, indicating

a lesser extent of interactions of GST–HIPPI with AA AGACATG This result indicated that the interaction

of GST–HIPPI with AAAGACATG was electrostatic

in nature, although other possibilities cannot be ruled out

The above results showed that purified GST–HIPPI interacted with the 9 bp motif AAAGACATG present

at the upstream sequence () 101 to ) 93) of the cas-pase-1 gene, and that mutation at the sixth and eighth positions of the motif did not affect this binding, as is evident from the significant quenching of GST–HIPPI protein fluorescence observed with the respective sequences (Fig 1B, panels I and II) A summary of the results is shown in Table 1 From the experimental studies described above with the various mutant motifs and their interactions in vitro with HIPPI, the consen-sus HIPPI-binding motif AAAGASAHK, i.e AAAG A[GC]A[ATC][TG], was derived

Reduction of the promoter activity of the 60 bp ()151 to ) 92) caspase-1 gene upstream sequence

by mutation at position) 98 (G to T) to the specific motif AAAGACATG ()101 to ) 93) in GFP–Hippi-expressing cells

We have earlier shown that the 717 bp () 700 to + 17) and 60 bp () 151 to ) 92) sequences can act as the promoter in the luciferase reporter assay in HeLa

as well as in Neuro2A cells It has been shown that the luciferase activity of pGL3 when driven by the 717 bp caspase-1 gene upstream sequence is higher than that obtained with the 60 bp-driven construct [18] This has been attributed to the presence of binding sites for other factors within these flanking sequences [19] As shown above, the 60 bp upstream sequence contains the motif AAAGACATG () 101 to ) 93), and muta-tion at posimuta-tion ) 98 (G to T) abolished the interaction

of HIPPI To check whether this mutation also decrea-ses the expression of the reporter gene driven by this mutated 60 bp caspase-1 gene upstream sequence

in vivo, we carried out the luciferase assay after cloning both the wild-type 60 bp sequence and the mutated

60 bp sequence in pGL3 The luciferase activity, seen

in GFP–Hippi-expressing HeLa cells when the lucif-erase gene was driven by the 60 bp region with a mutation at position ) 98 (G to T), was decreased (Fig 3) significantly (P¼ 0.01) in comparison with that obtained with the wild-type 60 bp sequence The result of this experiment is shown in Fig 3, and indi-cates that mutation of the specific site of the binding motif at the putative promoter sequence of the caspase-1 gene, where HIPPI can bind, decreased the

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promoter activity of the 60 bp upstream sequences

sig-nificantly As shown above, the interaction of HIPPI

with the mutated 9 bp motif (G to T at the fourth

position of the motif) was abolished, whereas the

60 bp sequence with the mutated motif exhibited

sub-stantial promoter activity This could be due to

addi-tional transcription regulator-binding sites within the flanking sequence of the motif It has been shown that p53 can bind within this region [19] The luciferase activity of the pGL3 driven by the mutated 60 bp caspase-1 gene upstream sequence in GFP–Hippi-expressing HeLa cells was similar (3.0 ± 1.1) to that

A

B

C

shifted

1 2 3

1 2 3 4 5 6 band

Probe

1.00E+008

AAAGAGATG

AAGGACATG AAAGACCTG

AAAGACATG

K d =1.2 nM

AAAGAGATG

K d =0.29 nM AAAGACACG

K d =4 nM

AAAGACACG AAAGACATA AGAGACATG

AAAGACATG AAAGCCATG AAATACATG

8.00E+007 6.00E+007 4.00E+007 2.00E+007 0.00E+000

14 16

12 10 8

6 4 0.00 0.01 0.02 0.03 0.04 0.05 0.00 0.02 0.04 0.06

[DNA] µM [DNA] µM

1.50E-008 1.40E-008

1.28E-008 1.26E-008

0.105 0.100 0.095 0.090 0.085 0.080

1.20E-008 1.10E-008 1.00E-008

F 340

F 340

0 25 50 75 100

1/[DNA] µM

20 25 30 35 40 45 50

1/[DNA] µM

0 11 22 33 44 55

1/[DNA] µM

0.08

Probe (9 bp) AAAGACATG

II I

I

shifted band

Fig 1 In vitro binding assay of putative HIPPI-binding motif AAAGACATG and its mutant (A) EMSA of binding of the end-labeled 9 bp motif AAAGACATG and two of its mutants with purified GST–HIPPI protein Panel I Lane1: probe (200 n M of [ 32 P]ATP[cP]-labeled 9 bp motif AAAGACATG) only Lane 2: probe + 4 l M GST protein Lane 3: probe + 1.7 l M GST–HIPPI Panel II Typical results of similar analysis with the same 9 bp DNA with mutation at the fourth, fifth or sixth base and GST–HIPPI protein are shown Lane 1: 200 n M [32P]ATP[cP]-labeled AAATACATG (probe only) Lane 2: 200 n M same probe + 3.8 l M GST–HIPPI protein Lane 3: band corresponding to 200 n M [ 32 P]ATP[cP]-labeled AAAGAGATG (probe only) Lane4: 200 n M probe + 3.8 l M GST–HIPPI protein Lane 5: AAAGCCATG (probe only) Lane 6: result obtained with 200 n M same probe + 3.8 l M GST–HIPPI protein (B) Quenching of intrinsic fluorescence of GST–HIPPI (0.8 l M ) at 340 nm (kexc¼ 295 nm) in the presence of the 9 bp putative motif sequence and six of its mutants Panel I Fluorescence quenching of GST–HIPPI protein due to addition of AAAGACATG (red line) and its mutants: AAAGAGATG (black line), AAAGCCATG (green line), AAATACATG (blue line) Inset: Curves representing wavelength scan of each point of quenching experiment with the 9 bp motif sequence AAAGACATG Fluor-escence intensities were measured in a Fluoromax 3 spectrofluoremeter Panel II Study of any quenching of intrinsic fluorFluor-escence of GST– HIPPI due to addition of point-mutated sequences of the 9 bp potent HIPPI-binding motif, namely: AAGGACATG (black line), AGAGACATG (red line), AAAGACCTG (green line), AAAGACACG (blue line) and AAAGACATA (sky blue line) Positions of point mutations are indicated by underlines (C) Linear plot of 1 ⁄ DF versus 1 ⁄ c, where as DF is the change in fluorescence with respect to the intrinsic fluorescence of GST– HIPPI due to addition of DNA with concentration c (l M ) Kdvalues were calculated from such plots In panel I, DF is of GST–HIPPI versus c

of 9 bp motif sequence AAAGACATG In panel II and panel III, DF is of GST–HIPPI versus c of mutated products of 9 bp sequence: AAAGA GATG and AAAGACACG, respectively.

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observed in HeLa cells (without any detectable HIPPI

expression) when the luciferase gene was driven by the

60 bp wild-type sequence (1.2 ± 1.3) The difference

was not statistically significant (P¼ 0.4) Furthermore,

there was no significant difference (P¼ 0.6) between

the luciferase activities in HeLa cells expressing pGL3

driven either by the 60 bp wild-type sequence

(1.2 ± 1.3) or the 60 bp mutated (1.7 ± 0.9) sequence

Thus, these luciferase activities could be due to the

presence of promoter-binding site(s) within the 60 bp

caspase-1 gene upstream sequence other than for

HIPPI This indicated that, due to point mutation

at position 98 (G to T), HIPPI could not bind to the

caspase-1 gene upstream to transcribe the downstream

gene; this was manifested by about a two-fold decrease

in luciferase acitivity Thus, the results of promoter

assay experiments further confirmed the in vitro result

that mutation of the motif abolished the binding of

HIPPI to the specific sequence of the caspase-1 gene

upstream sequence, and the increased expression of

caspase-1 in GFP–Hippi-expressing cells was due to interaction of HIPPI with this motif

Interaction of pDED of HIPPI with upstream sequences of the caspase-1 gene

To check which portion of HIPPI was responsible for this interaction, a cDNA portion corresponding to the two termini of HIPPI, i.e the N-terminal portion com-prising amino acid residues 10–334 (NCBI protein ID NP_060480) and the C-terminal pDED region (amino acids 335–429), were cloned and expressed in bacteria, and the proteins were purified Interactions of the puri-fied 6X(HN)-pDED and the N-terminal domains of HIPPI [also tagged with 6X(HN)] were studied in vitro

by EMSA and fluorescence quenching The results revealed that the 6X(HN)-pDED domain of HIPPI interacted with the 60 bp upstream sequence of the caspase-1 gene (Fig 4A, panel II, lanes 1 and 3) In contrast, the N-terminal region of HIPPI did not inter-act with the upstream sequence of the caspase-1 gene (Fig 4A, panel I, lane 3) This result showed that the C-terminal end containing the pDED domain of HIPPI could interact with the upstream sequence of the caspase-1 gene

16000000

GST-Hippi 25µg + AAAGACATG 0.05 µM

R2=0.92422 14000000

12000000

10000000

8000000

6000000

4000000

2000000

0

Fig 2 (A) Sigmoidal curve (R 2 ¼ 0.924) showing gradual increase

in fluorescence intensity of GST–HIPPI (0.8 l M ) at 340 nm (k exc ¼

295 nm) at saturation level of binding with the 9 bp motif

AAAGA-CATG with increasing salt (NaCl) concentrations ranging from

50 m M to 1 M

Table 1 Summary of binding study with the putative HIPPI-binding

motif and its mutants ND, not determined.

Fluorescence quenching Result Average Kd(n M )

8

p=0.01

7 6 5

4 3 2 1 0

Fig 3 The caspase-1 gene upstream 60 bp and a point mutation (G to T) incorporated in the same sequence at position ) 98, cloned

in the pGL3 enhancer plasmid (60 M ) and transfected (4 lg each) in GFP–Hippi-expressing cells Cells expressing GFP–Hippi were mon-itored by the presence of GFP under a fluorescence microscope About 80–90% of cells expressed GFP after 20 h of transfection with GFP–Hippi Transfected cells are denoted as 60_Hi and

60 M _Hi, respectively The corresponding average fold increase (n ¼ 3) in luciferase activities compared to control (cell expressing only pGL3 without any insert) are given in bar diagrams P-values

of significance are mentioned above the bar diagram in each of the cases studied.

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As 6X(HN)-pDED of HIPPI does not contain any

tryptophan, a 280 nm excitation filter was used, and

the fluorescence (characteristics of tyrosine and

phe-nylalanine) was measured at 305 nm A decrease in

the fluorescence intensity of 6X(HN)-pDED due to

the addition of the 60 bp region of the caspase-1 gene

upstream sequence was observed Addition of the

caspase-1 gene upstream 60 bp sequence could also quench the intrinsic fluorescence of 6X(HN)-pDED of HIPPI from 6.997 to 1.802 (Fig 4B, panel I) with an apparent binding constant (Kd) 0.34 nm; a double reciprocal plot is shown in Fig 4B, panel II However, addition of the upstream sequences of the caspase-1 gene (717 bp) to the N-terminal domain (without the pDED domain) of HIPPI did not decrease the fluorescence intensities determined by exciting either at 295 nm (kem¼ 340 nm; fluorescence intensity changed from 15.62 to 14.42 due to addition

of 0.5 lm DNA) or 280 nm (kem¼ 305 m; fluores-cence intensity changed from 8.77 to 7.59) This result also showed that pDED of HIPPI actually interacted with the caspase-1 gene upstream sequences We recently observed that pDED of HIPPI could also interact in vivo with the caspase-1 gene upstream sequence (data not shown)

Increase in caspase-1 gene expression and induction of apoptosis by C-terminal pDED

of HIPPI The role played by pDED of HIPPI in alteration of caspase-1 gene expression in HeLa cells was monitored

by western blot analysis using antibody to caspase-1 (Fig 5, middle panel) The band intensities were measured using image master vds software The aver-age integrated optical density (IOD) of three different experiments is shown in Table 2 The results indicated that caspase-1 expression, as detected by western blot

A

B

shifted

labeled

band

Casp1

ups 717 bp

shifted

labeled

band

Casp1ups

II I

C1ups 717bp (HIPPI-pDED)

C1ups 60bp (6XHN-HIPPI_pDED)

Kd=0.34n M

C1ups 717bp (HIPPI-Nterm)

C1ups 60bp (HIPPI-pDED)

9

7

5

4

2

0

0.00 0.01 0.02

0.03 0.04

0.18 0.19 0.20 0.21

0.17

0 20 40 60 80100 120 140

60 bp

Fig 4 (A) In vitro binding assay of pDED of HIPPI with the

ca-spase-1 gene upstream sequences In panel I, typical results of

EMSA with the 717 bp caspase-1 probe and 6X(HN)-pDED of Hippi

and 6X(HN)-tagged N-terminal domain of Hippi protein are shown.

Lane 1 shows the result with the probe only (400 n M ) Lanes 2 and

3 show results obtained when 400 n M probe was allowed to

inter-act with 2.7 l M 6X(HN)-pDED of HIPPI and 5.2 l M 6X(HN)-tagged

N-terminal domain of HIPPI, respectively In panel II, 500 n M 60 bp

caspase-1 gene upstream sequence ( ) 151 to ) 92) labeled with

[32P]dCTP[aP] was used as probe Lanes 1 and 2 show results

obtained with probe only and probe + 4.8 l M BSA (nonspecific

pro-tein), respectively Lane 3 shows the result when 500 n M probe

was allowed to react with 1.6 l M 6X(HN)-pDED of HIPPI, and lane

4 shows the result obtained when 500 n M labeled 60 bp probe was

allowed to react with 1.6 l M 6X(HN)-pDED protein in the presence

of 500 n M unlabeled 60 bp caspase-1 gene upstream sequence (B)

Panel I, quenching of intrinsic fluorescence of 6x(HN)-tagged pDED

of HIPPI (pDED-HIPPI, 2 l M ) at 305 nm in presence of the 717 bp

(squares) and 60 bp (triangles) upstream sequences of the

ca-spase-1 gene (denoted as C1ups 717 bp and C1ups 60 bp,

respect-ively) and any change in intrinsic fluorescence of 6x(HN)-tagged

N-terminal domain of HIPPI (HIPPI-Nterm, 1 l M ) at 305 nm in the

presence of 717 bp upstream sequence of the caspase-1 gene,

denoted by circles Panel II shows a linear plot of 1 ⁄ DF versus 1 ⁄ c

where, DF represents the decrease in intrinsic fluorescence of

6x(HN)-tagged HIPPI-pDED protein in the presence of the 60 bp

upstream sequence of the caspase-1 gene; c, concentration (l M ).

The apparent binding constant (K d ) was calculated from this plot

and is given with the graph. Fig 5 Role of exogenous pDED of HIPPI in alteration of caspase-8

and caspase-1 activation in HeLa cells Western blot analysis using antibodies to caspase-8 (upper panel) and caspase-1 (middle panel) with total protein isolated from HeLa cells (H), HeLa cells expres-sing GFP-tagged N-terminus of HIPPI containing Myosin-like domain (HiN), and that expressing GFP-tagged pDED of HIPPI (HiD) The upper bands of the upper panel correspond to proca-spase-8 (57 kDa), and the lower bands represent the 12 kDa activa-ted caspase-8; the upper bands of the middle panel correspond to procaspase-1 (45 kDa), and the lower bands correspond to the

20 kDa activated caspase-1 The lowermost panel shows the level

of b-actin (14.4 kDa).

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analysis, was increased in GFP–pDED-expressing cells

by 4.4 ± 0.7-fold as compared to that in parental

HeLa cells However, this increase in the N-terminal

part of HIPPI-expressing cells was only 1.4-fold The

increase in caspase-1 expression was again 6.2 ±

1.1-fold in pDED HIPPI-expressing cells as compared to

the N-terminal part of HIPPI-expressing cells

To test whether the C-terminal pDED of HIPPI

could induce apoptosis more efficiently than the

N-ter-minal domain in our system, these two domains cloned

in pEGFP C1 vectors were transfected into HeLa cells

After 32 h, when 80–90% of cells were expressing

GFP-tagged protein, we determined the nuclear

frag-mentation as an indication of apoptosis induction and

caspase activation GFP–pDED-expressing cells

exhib-ited nuclear fragmentation in 32.5 ± 1.8% of the total

cell population, whereas this value in the GFP-tagged

N-terminal domain of HIPPI-expressing cells was only

17.6 ± 1.9% This difference was statistically

signifi-cant (P¼ 0.0006) Thus, GFP–pDED of HIPPI was

more effective in inducing apoptosis in HeLa cells

Fluorometric determination of caspase-1 activity by a

commercially available kit indicated that, in GFP–

pDED of HIPPI-expressing cells, caspase-1 activity

was 1.6-fold higher (P¼ 0.02) than that observed in

the GFP–N-terminal domain of HIPPI-expressing

HeLa cells Fluorometric determination of caspase-8

activity indicated that in HeLa cells expressing GFP–

pDED of HIPPI, caspase-8 activation was also 1.6-fold

higher in comparison to that obtained in the

GFP–N-terminal domain of HIPPI-expressing cells This value

was also statistically significant (P¼ 0.047, n ¼ 3)

Activation of caspase-1 and caspase-8 in

GFP–pDED-expressing cells was further supported by western blot

analysis (Fig 5) using total protein isolated from HeLa

cells expressing pDED and the N-terminal domain of

HIPPI It is evident from Fig 5 that ectopic pDED

expression in HeLa cells induced cleavage of proca-spase-8 (Fig 5, upper panel) and procaspase-1 (Fig 5, middle panel) proteins more efficiently as compared to that of the N-terminal domain of HIPPI A similar higher activation (2.1-fold, P¼ 0.03) of caspase-3 was observed in GFP–pDED of HIPPI-expressing cells in comparison to that observed in GFP-–N-terminal HIPPI-expressing HeLa cells These results are shown

in Table 2

Presence of the motif and the putative promoter sequences of caspase-8 and caspase-10 increased expression of the genes in GFP–Hippi-expressing HeLa cells

The derived motif AAAGASAHK, i.e AAAGA[GC] A[ATC][TG], was used to search for the presence of the motif at the 1000 bp upstream sequences of the caspase-8 and caspase-10 genes using motiflocator (http://www.esat.kuleuven.ac.be/dna/BioI/Software html) These genes are supposed to be involved in HD The results for similar motifs identified in the caspase-1 (for reference) caspase-3, caspase-7, caspase-8 and caspase-10 genes are shown in the Table 3 In Table 3, the start and end positions of the motifs are indicated

by distance from the transcription start site (TSS) The position upstream of the TSS of any gene is denoted

by ‘–’ followed by the distance from the TSS In the caspase-8 gene, the putative upstream sequence motifs AAAGAGAAC () 955 to ) 963) in the positive strand, and AAAGAAAAG () 418 to ) 410) and AA AGACATA () 800 to ) 808) in the negative strand, were observed (variants are underlined) As shown above, mutation at the last base, G to A, abolished the interaction of HIPPI, so the last motif would not interact with HIPPI The other two motifs might be the target of HIPPI In the upstream sequence of the

Table 2 Comparison of apoptosis induction and alteration in caspase-1 gene expression in GFP-tagged pDED of HIPPI and N-terminal domain of HIPPI-expressing HeLa cells.

GFP–pDED

of HIPPI (fold) P-values

GFP–N-terminus

of HIPPI (fold) P-values

Fold increase: pDED versus N-terminal domain (P-values) Caspase-1

expression

8.9 ± 2.6 54.9 ± 2.1

(6.2-fold)

(0.0005) Nuclear

fragmentation

2.4 ± 0.9 32.5 ± 1.8

(13.5-fold)

(7.3-fold)

0.0006 Caspase-8

activation

9.2 ± 2.0 23.1 ± 1.3

(2.5-fold)

(0.047) Caspase-1

activation

40.4 ± 3.6 90.2 ± 11.1

(2.2-fold)

(0.02) Caspase-3

activation

1.5 ± 0.3 10.8 ± 2

(7.2-fold)

(3.4-fold)

(0.03)

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caspase-10 gene, four variant motifs were identified.

Among them, AAACAGATG () 254 to ) 262) is

present in the positive strand, and the sequences AA

AGAAAAG () 651 to ) 643), AAAGAAAAG () 725

to) 717) and GAAGACATT () 849 to ) 857) are

pre-sent in the negative strand

Given that the caspase-8 and caspase-10 genes

har-bor similar motifs as that in the caspase-1 gene and

increase caspase-1 expression, we first tested the

expression of the caspase-8 and caspase-10 genes in

GFP–Hippi-expressing cells by the semiquantitative

RT-PCR described previously [18] The numbers of

PCR cycles and the amount of total RNA were chosen

so that the yield of RT-PCR products was in the linear range The IOD value of the RT-PCR product obtained with RNA isolated from GFP–Hippi-expres-sing HeLa cells was increased 2.5-fold in comparison

to the value obtained when RNA from the HeLa cells was used This increase was statistically significant (P¼ 0.0004) A similar significant increase in the IOD value of the RT-PCR products for the caspase-10 gene (1.8-fold, P¼ 0.0002) was detected A bar diagram showing the mean IOD of bands corresponding to caspase-8 and caspase-10 gene-specific products run on 1.5% agarose gel is shown in Fig 6A) A representa-tive photograph of the RT-PCR products run on

Table 3 Summary of the presence of similar motifs in caspase-1, caspase-3, caspase-7, caspase-8 and caspase-10 gene upstream sequences.

Fig 6 (A) Bar diagrams showing mean of IOD of bands obtained by RT-PCR at caspase-8 and caspase-10 loci, along with error bars calcula-ted on the basis of three independent experiments using mRNA isolacalcula-ted from GFP–Hippi-expressing (gray bar) and parental (white bars) HeLa cells Levels of significance (P-values) are shown on the top of the bars (B) Picture of RT-PCR products run on 1.5% agarose gel and stained with ethidium bromide, representing PCR amplification with RNA isolated from HeLa cells (lane 1:H), GFP–Hippi-expressing HeLa cells (lane 2:Hi), and reaction carried out where no RNA was added (lane 3:ve) The uppermost panel shows the PCR reaction carried out with caspase-8 (164 bp)-specific primers; the middle panel represents PCR amplification using primers specific for caspase-10 (178 bp) genes; and the lowermost panel shows bands (315 bp) corresponding to b-actin (loading control).

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agarose gel is shown in Fig 6B Equally intense signals

for internal control (b-actin gene-specific primers) were

obtained in all the cases (Fig 6B, lowermost panel)

Fluorescence quenching assay to measure the

interactions of GST–HIPPI with the caspase-8 and

caspase-10 gene upstream sequences

Expression of caspase-8 and caspase-10 increased in

GFP–Hippi-expressing cells, as described above, and

DNA sequences similar to the putative HIPPI-binding

motif were present within the 1000 bp upstream

sequences of the caspase-8 and caspase-10 genes

(Table 3) To check interactions of GST–HIPPI with

these upstream regions containing the motifs, the

caspase-8 gene upstream 710 bp () 991 to ) 282) and

caspase-10 gene upstream 768 bp () 914 to ) 147)

regions were PCR-amplified The results, shown in

Fig 7A, indicated quenching of GST–HIPPI intrinsic

fluorescence at 340 nm, due to addition of increasing

concentrations (0.001 lm to 0.05 lm) of the caspase-8

and caspase-10 gene upstream sequences

Average (n¼ 2) Kd values for binding of purified

GST–HIPPI with the caspase-8 gene (0.32 ± 0.13 nm)

and the caspase-10 gene (11 ± 3.8 nm) upstream

sequences were calculated from reciprocal plots as

des-cribed previously [18], and typical cases are shown in

Fig 7B, panel I and panel II, respectively

Discussion

In the present work, we have shown that HIPPI

inter-acted specifically with the motif AAAGACATG () 101

to) 93) present in the upstream region of the caspase-1

gene in vitro Decreased expression of the reporter gene

luciferase when driven by the 60 bp caspase-1 upstream

sequence () 151 to ) 92) containing this motif with a

mutation at position 98 position (G to T) in

compar-ison with the wild-type 60 bp upstream sequence was

observed The same mutation in the motif also

abol-ished the interactions of HIPPI in vitro In addition, we

observed that HIPPI could interact with the putative

promoter sequences of the caspase-8 and caspase-10

genes Expression of caspase-8 and caspase-10, as

detected by semiquantitative RT-PCR, was also

increased in the GFP–Hippi-expressing HeLa cells

The motif derived from bioinformatics analysis and

interaction studies of HIPPI with various mutants of

AAAGACATG present in the caspase-1 gene was

AAAGASAHK, i.e AAAGA[GC]A[ATC][TG] For

the caspase-8 gene, there are three variations in the

motif from that of the motif in the caspase-1 gene

upstream region Our experimental data suggest that

the change of C at the sixth position to G, and of T to

C at the eighth position, did not decrease the interac-tion, whereas a change from G to A at the ninth posi-tion compromised the interacposi-tions (Fig 1B, panel I and panel II) The change at the ninth position of the motif in the caspase-8 gene upstream sequence is G to

C As the caspase-8 gene 710 bp upstream sequence () 991 to ) 282) was shown to interact with HIPPI, we speculated that HIPPI interacted with the motif AAAGAGAAC () 963 to ) 955) We could not exclude the possibility that the other motif AAAG AAAAG () 418 to ) 410) present in the negative strand of the caspase-8 gene promoter interacted with HIPPI Further experiments are necessary to establish this Interaction of HIPPI with the motif AAAGA CATA () 808 to 800) at the positive strand (the vari-ant substitution G to A is underlined) of the caspase-8 gene was not possible, as we showed above that this particular motif did not interact with HIPPI (Fig 1B) The putative HIPPI-binding motifs at the caspase-10

11

A

B

Caspase10 ups + GST-Hippi

Casp8ups (GST-HIPPI)

K d =15 n M

Caspase8 ups + GST-Hippi

10 9 8 7 6

F340 5 4 3 2

0.140 0.145

0.135 0.130 0.125

F 0.15 0.20 0.25

0.10 0.05 0.00

0.00 0.01 0.02

[DNA] µ M

0.03 0.04 0.05

0 10 20

1/[DNA] µ M

1/[DNA] µ M

30 40 50

Fig 7 (A) In vitro binding study of GST–HIPPI with caspase-8 gene ( ) 991 to ) 282) and caspase-10 gene () 914 to ) 147) upstream sequences The upper line (squares) represents a gradual decrease

in the intrinsic fluorescence of GST–HIPPI protein (0.8 M ) at

340 nm (k ex ¼ 295 nm) due to addition of the caspase-10 gene upstream sequence The lower line in the graph (triangles) repre-sents a similar alteration in fluorescence intensity of GST–HIPPI when the caspase-8 gene upstream sequence was added gradually

to it (B) Linear plot of 1 ⁄ DF versus 1 ⁄ c, where DF represents change in intrinsic fluorescence of GST–HIPPI due to addition of upstream sequences from the caspase-8 (panel I) and caspase-10 (panel II) genes, and c represents final concentration (l M ) of DNA allowed to bind with the protein.

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gene upstream sequences are AAACAGATG () 254 to

) 262) in the positive strand, and AAAGAAAAG

() 651 to 643), AAAGAAAAG () 725 to ) 717) and

GAAGACATT () 849 to ) 857) in the negative

strand We were unable to exclude any of the motifs

as the target of HIPPI, as we observed that HIPPI

interacted with the putative promoter 768 bp () 914

to ) 147) sequence of the caspase-10 gene (Fig 7B,

panel II) Further experiments are necessary to

deter-mine the specific sequences where HIPPI could interact

at the upstream sequence of this gene

It is interesting to note that even though the initial

motif search revealed that the upstream sequence of the

caspase-7 gene contains the AAAGACATA sequence

present in duplicate within the) 355 to ) 347 and ) 315

to 307 regions, our experiments with this motif revealed

that HIPPI did not interact with it (Fig 1B, panel II)

Thus, the increase in caspase-7 expression in GFP–

Hippicells [9] might not be due to the direct interaction

of HIPPI with the promoter sequence This was further

supported by the observations that purified HIPPI did

not interact with the caspase-7 gene upstream 592 bp

sequence () 1080 to 489) in vitro (by EMSA and

fluor-escence quenching) or in vivo (chromatin

immunopre-cipitation assay using antibody to HIPPI) (data not

shown) We also failed to detect any interactions of

purified HIPPI with the caspase-3 gene upstream 652 bp

sequence () 997 to ) 346) (data not shown), even

though the exact motifs with which HIPPI could

inter-act were present in the negative strand (Table 3) of the

gene The reason behind this still remains obscure;

whether strand bias or the neighboring nucleotides

prevented the interaction remains to be determined

HIPPI does not have any similarity with known

pro-teins having DNA-binding motifs However, it

con-tains the pDED at the C-terminus (amino acid

residues 335–426) and a myosin-like domain The

pDED of HIPPI shows only 34.9% similarity and

21% identity to other known death effector domains

(DEDs), and 39.2% similarity and 26.7% identity with

the pDED of HIP1 It has been shown that the

inter-action of HIPPI with HIP1 is mediated through the

pDED present at HIP1 The pDED differs from its

conformational neighbor DED by the presence of

charged residues at the interacting helices, as opposed

to the hydrophobic ones in the later [8]

DED-contain-ing proteins are known to participate in diverse

cellu-lar functions, including apoptosis through receptor

signaling [20,21] Other DED-containing proteins, such

as DEDD, are known to bind DNA and inhibit RNA

polymerase I activity in vivo [22] Direct evidence that

the DED-containing proteins DEDD and FLAME-3

interact with the transcription factor TFIIIC102 and

thus regulate the transcription of the target genes has been also provided [23] We hypothesized that the pDED of HIPPI might have similar DNA-binding ability to that of its distant relative DEDD.Our find-ings that the purified C-terminal pDED of HIPPI was able to interact with the caspase-1 gene upstream sequence (Fig 4A,B), similar to what was observed with full-length HIPPI [18], and that the exogenous expression of cDNA corresponding to the pDED of HIPPI alone was sufficient to increase caspase-1 expression and apoptosis (Fig 5, Table 2) showed that the C-terminal pDED of HIPPI contributed to the increased expression of caspase-1 and apoptosis HIPPI generally resides in the cytoplasm How this cytoplasmic protein is transported to the nucleus remains unknown In an earlier study, we showed that exogenously expressed Hippi in HeLa cells can be detected in the nuclear fraction [Fig 2(b) in Majumder

et al [9]] It can be seen that there was no detectable endogenous expression of Hippi in HeLa cells, whereas the expression of HIP1 was detected in HeLa cells [Fig 2(c), III, in Majumder et al [9]] Recently, trans-portation of androgen receptor to the nucleus has been reported to be mediated through HIP1 [24] On the basis of this observation, we hypothesized that HIP1 might play similar role in the transport of HIPPI into the nucleus We are presently testing this hypothesis The role of HIPPI in HD, if any, remains unknown Even though the caspase-8 and caspase-10 genes have been implicated in poly-Q-mediated toxicity [25,26], it

is not known whether the expression of these genes is altered The role of HIPPI in the increased expression

of caspase-1 observed in various models and HD patients has to be established We speculated that excess available HIP1 in HD, due to weaker interac-tion of HIP1 with the mutated Htt allele, leads to the formation of more HIPPI–HIP1 heterodimer, which in turn increases caspase-1 expression We were able to immunoprecipitate the caspase-1 gene promoter by antibody to HIPPI after crosslinking DNA protein

in vivo [18] However, we failed to do the same thing with antibody to HIP1 (data not shown), indicating that HIP1 does not directly interact with the putative promoter of the caspase-1 gene Thus, the role of HIP–HIPPI heterodimer formation in the increased expression of caspase-1, caspase-8 and caspase-10 is not clear We speculated that it might be necessary for transporting HIPPI into the nucleus

In summary, together with our earlier observations [9,18], we observed in the present work that HIPPI interacted with the specific motif present in the putative promoters of the caspase-1, caspase-8 and caspase-10 genes and altered the expression of these genes The

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