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Báo cáo khoa học: Syndecan-4 is a signaling molecule for stromal cell-derived factor-1 (SDF-1)/ CXCL12 pptx

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We show that upon stimulation of HeLa cells by CXCL12, CXCR4 becomes tyrosine phosphorylated as expected, while syndecan-4 but not syndecan-1, syndecan-2 or beta-glycan also undergoes su

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factor-1 (SDF-1)/ CXCL12

Nathalie Charnaux1,2*, Se´verine Brule1,2*, Morgan Hamon1, Thomas Chaigneau1, Line Saffar1, Catherine Prost1, Nicole Lievre1and Liliane Gattegno1,2

1 Laboratoire de Biologie Cellulaire, Biothe´rapies Be´ne´fices et Risques, UPRES 3410 Universite´ Paris XIII, Bobigny, France

2 Hoˆpital Jean Verdier, Bondy, France

Chemokines are low molecular mass proteins mediating

several functions such as hematopoiesis regulation,

leu-kocyte maturation, angiogenesis, T and B lymphocytes

trafficking, homing and lymphoid tissues development

[1–3] Stromal cell-derived factor-1 (SDF-1)⁄ recently

renamed CXCL12 [4], is the only known ligand for CXCR4 [5,6] SDF-1 and CXCR4 are constitutively expressed in various tissues [7] and are implicated in several diseases CXCR4 is involved in HIV infection and pathogenesis [5,8] SDF-1 and CXCR4 also regulate

Keywords

CXCR4; proteoglycan; SDF-1⁄ CXCL12;

syndecan-4

Correspondence

L Gattegno, Laboratoire de Biologie

Cellulaire, Biothe´rapies Be´ne´fices et

Risques, UPRES 3410 Universite´ Paris XIII,

74, rue Marcel Cachin, 93017, Bobigny,

France, Hoˆpital Jean Verdier, 93017, Bondy,

France

Fax: +33 1 48026503

Tel: +33 1 48387752

E-mail: liliane.gattegno@jvr.ap-hop-paris.fr

*These authors contributed equally to this

work.

(Received 18 January 2005, accepted 21

February 2005)

doi:10.1111/j.1742-4658.2005.04624.x

Stromal cell-derived factor-1 (SDF-1)⁄ CXCL12, the ligand for CXCR4, induces signal transduction We previously showed that CXCL12 binds to high- and low-affinity sites expressed by primary cells and cell lines, and forms complexes with CXCR4 as expected and also with a proteoglycan, syndecan-4, but does not form complexes with syndecan-1, syndecan-2, CD44 or beta-glycan We also demonstrated the occurrence of a CXCL12-independent heteromeric complex between CXCR4 and syndecan-4 However, our data ruled out the glycosaminoglycan-dependent binding of CXCL12 to HeLa cells facilitating the binding of this chemokine to CXCR4 Here, we demonstrate that CXCL12 directly binds to syndecan-4

in a glycosaminoglycan-dependent manner We show that upon stimulation

of HeLa cells by CXCL12, CXCR4 becomes tyrosine phosphorylated as expected, while syndecan-4 (but not syndecan-1, syndecan-2 or beta-glycan) also undergoes such tyrosine phosphorylation Moreover, tyrosine-phos-phorylated syndecan-4 from CXCL12-stimulated HeLa cells physically coassociates with tyrosine phosphorylated CXCR4 Pretreatment of the cells with heparitinases I and III prevented the tyrosine phosphorylation of syndecan-4, which suggests that the heparan sulfate-dependent binding of SDF-1 to this proteoglycan is involved Finally, by reducing syndecan-4 expression using RNA interference or by pretreating the cells with hepari-tinase I and III mixture, we suggest the involvement of syndecan-4 and heparan sulfate in p44⁄ p42 mitogen-activated protein kinase and Jun N-ter-minal⁄ stress-activated protein kinase activation by action of CXCL12 on HeLa cells However, these treatments did not modify the calcium mobil-ization induced by CXCL12 in these cells Therefore, syndecan-4 behaves

as a CXCL12 receptor, selectively involved in some transduction pathways induced by SDF-1, and heparan sulfate plays a role in these events

Abbreviations

dsRNA, double-stranded RNA; FBS, fetal bovine serum; GAG, glycosaminoglycan; HS, heparan sulfate; JNK ⁄ SAPK, Jun N-terminal ⁄ stress-activated protein kinase; MAPK, mitogen-stress-activated-protein kinase; PFA, paraformaldehyde; PMA, phorbol 12-myristate-13-acetate; PG, proteoglycan; Ptyr, tyrosine phosphorylated; SDF, stromal cell-derived factor; SD, syndecan.

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embryonic development [9] Much of the heparan

sulfate (HS) at the cell surface is derived from the

syndecan (SD) family of transmembrane proteoglycan

(PG) [10] The SDs bind a variety of growth factors,

cytokines, proteases, antiproteases and cell adhesion

molecules [10,11]; they are individually expressed in

dis-tinct cell-, tissue-, and development-specific patterns

[12], and show cell-specific variations in the structure of

their HS chains [13] SDs may regulate

ligand-depend-ent activation of cell surface growth factor receptors by

several potential mechanisms [10,11,14] SD-4 is one

of the principal HS carrying protein on cell surfaces

[15,16] We recently showed that SDF-1 binds to

high- and low-affinity sites on HeLa cells and forms

complexes on these cells and on human primary

lympho-cytes and macrophages, which comprise CXCR4, as

expected, and also SD-4 [17], but not SD-1, SD-2,

beta-glycan or CD44 ([17] and unpublished data) Moreover,

we recently demonstrated the occurrence of an

SDF-1-independent heteromeric complex on the plasma

mem-brane of these cells, which comprises CXCR4 and SD-4

but not SD-1, SD-2, CD44 or beta-glycan [17] This

suggested that SDF-1 may bind both the PG SD-4 and

its G-protein-coupled receptor (GPCR), CXCR4

How-ever, our previous data have shown that while

glycos-aminidases pretreatment of primary macrophages

decreases the binding of SDF-1 to CXCR4, such

treat-ment had no effect on the chemokine binding to

CXCR4 expressed by the HeLa cell line [17] This has

suggested that while SD-4 may serve as a binding

anchor for SDF-1 on primary macrophages to enable

the chemokine to interact with CXCR4, this was not

true if HeLa cells were tested

The present study was designed to test whether

SD-4 functions as a specific SDF-1 signaling molecule

Therefore, we first determined whether SDF-1 directly

binds SD-4 and the glycosaminoglycan

(GAG)-dependency of this binding Because protein

phos-phorylation plays a critical role in the generation of

intracellular signals in response to external stimuli,

we then investigated whether SD-4 becomes tyrosine

phosphorylated (Ptyr) upon SDF-1 stimulation of

HeLa cells, and whether, in these conditions,

tyrosine-phosphorylated SD-4 is physically coassociated with

tyrosine-phosphorylated CXCR4, and what the

GAG-dependency of these events is Finally, we asked

whe-ther SD-4 is involved in owhe-ther biochemical signals

induced by SDF-1 By specifically reducing SD-4

expression using RNA interference, or by reducing the

HS expressed at the plasma membranes of HeLa cells

by the use of heparitinases I and III, we analyzed the

respective roles of SD-4 and HS in transduction

path-ways induced by SDF-1 on these cells

Results SDF-1 directly binds to SD-4 The HeLa cells used in the present study express CXCR4, SD-2, beta-glycan (data not shown) [17,18], CD44, SD-1 and SD-4 (Fig 1A), as assessed by flow cytometry analysis after indirect immunofluorescence

A

B

c

Fig 1 PGs on HeLa cells (A) Cell surface expression of SD-1, SD-4 and CD44 on HeLa cells HeLa cells (5 · 10 5

) were stained for FACS analysis with anti-(SD-1) DL-101 mAb (a), anti-(SD-4) 5G9 mAb (b) or anti-CD44 mAb (c) (thick lines) Reactivity was compared to an isotype-matched control monoclonal antibody (a,b,c, dotted lines) (B) Immunoblot analysis of PGs from HeLa cells HeLa cells were lysed in the presence of Triton X-100 and urea PGs (from 2 · 10 6

cells per lane) were enriched by DEAE Sephacel anion exchange chromatography and then treated with heparitinases I, III, and chondroitinase ABC mixture, electroblotted and revealed with 3G10 mAb (lane 1) or the isotype, IgG2b (lane 2) The respective immunoreactivity with (SD-1) DL-101, anti-(SD-4) 5G9, anti-CD44 mAbs, or anti-(SD-2) Igs are represented by arrows Data are representative of three individual experiments.

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labeling The core proteins of most PGs enriched from

HeLa cells lysates were analyzed [17] after heparitinase

I and III and chondroitinase ABC treatment to detect

their apparent molecular masses Proteins of 32 kDa

and 50–58 kDa, immunoreactive with anti-SD-4 5G9

and 3G10 mAbs, were observed (Fig 1B) The 50–

58 kDa proteins may represent, in accordance with

other studies, homo- or hetero-oligomers of the SD-4

core protein, which is a 32 kDa protein [19] Other

PGs were also detected: 34 kDa proteins

immunoreac-tive with both anti-SD-2 mAbs and mAb 3G10,

45- and 90 kDa proteins immunoreactive with

anti-SD-1DL-101 and 3G10 mAbs (the 90 kDa ones

probably being dimers of the 45 kDa ones), and

60 kDa proteins immunoreactive with anti-CD44 and

3G10 mAbs (Fig 1B) All these apparent molecular

masses are close to the predicted ones [9] These PGs

were glycanated, as mAb 3G10 reacts with an epitope

including a terminal unsaturated uronic acid residue,

which is unmasked after HS removal by heparitinases

treatment [20]

Native PGs may migrate in a diffuse high molecular

mass distribution on SDS⁄ PAGE Using the respective

specific Abs, glycanated PGs migrate as follows: SD-4

as a 100–250 kDa broad smear, SD-1 as a single

98 kDa band, CD44 as a 110 kDa band, SD-2 as a

50 kDa protein Beta-glycan migrates as two broad

bands of 55 and 100 kDa, respectively (Fig 2, lanes

1–5) No immunoreactivity was detected with the

iso-types (data not shown) The fact that all these PGs

were also immunoreactive with anti-HS mAb 10E4,

but not with its isotype, demonstrates their glycana-tion (Fig 2, lane 6 and data not shown) Biotinylated SDF-1a bound to the broad smear of 100–250 kDa, characterized as glycanated SD-4, but did not bind to SD-1, SD-2, beta-glycan or CD44 (Fig 2, lane 7 vs 1–5) Heparitinase I and III, and chondroitinase ABC pretreatment of the strips abolished the binding of electroblotted PGs to anti-HS mAb 10E4 (Fig 2, lane

8 vs 6), and strongly decreased that of biotinylated SDF-1a to SD-4 (Fig 2, lane 9 vs 7), but did not change SD-4 binding to anti-SD-4 mAb 5G9 (specific for the core protein of SD-4)(data not shown) This demonstrated that (a) the heparitinases treatment was efficient; (b) SD-4 was still present on the polyvinylid-ene difluoride membrane (data not shown); and (c) the direct binding of SDF-1 to SD-4 was GAG dependent

Confocal microscopy analysis showed that fluores-cently labeled biotinylated SDF-1a colocalizes with SD-4 on the plasma membranes of these cells, as assessed by the yellow (red-green colocalization) stain-ing (Fig 3A, and data not shown) This association was further analyzed by electron microscopy (Fig 3B) Beads at the cell surface were counted and considered

as associated when the distance between them was less than 15 nm Forty per cent of the beads that labeled SD-4 were associated with 45% of the beads that labe-led SDF-1a, while no association of SDF-1a with SD-1 was detected Controls, run without biotinylated SDF-1a or with the isotypes, were not stained (data not shown)

Fig 2 SDF-1 binds to SD-4 HeLa cells were lysed in the presence of Triton X-100 and urea PGs were enriched by DEAE Sephacel anion exchange chromatography, electroblotted and revealed with anti-SD-4 5G9 mAb (lane 1), anti-(SD-1) DL-101 mAb (lane 2), anti-CD44 mAb (lane 3), anti-(SD-2) Igs (lane 4), anti-(beta-glycan) Igs (lane 5), anti-HS 10E4 mAb (lane 6), biotinylated SDF-1a (lane 7) Alternatively, strips were treated with heparitinases I, III mixture and revealed with anti-HS mAb 10E4 (lane 8) or biotinylated SDF-1a (lane 9) Data are represen-tative of three individual experiments.

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SDF-1 induces the tyrosine phosphorylation of

CXCR4 and the homo- or hetero-oligomerization

of this GPCR on HeLa cells

SDF-1-activated or nonactivated HeLa cell lysates

were either immunoprecipitated with anti-CXCR4 mAb

G19 then blots were developed with anti-Ptyr mAb

4G10, or immunoprecipitated with anti-Ptyr mAb 4G10

then blots were developed with anti-CXCR4 mAb

12G5 A protein was observed at 48 kDa, and several

others of apparent molecular masses > 48 kDa All

amounts of these tyrosine-phosphorylated proteins

were significantly increased upon SDF-1 stimulation

of the cells (Fig 4A, lane 2 vs 1, and lane 4 vs 3)

These increases were not significant if the cells were

stimulated with 3 nm SDF-1, and strongly significant

for a cell stimulation with 125 nm SDF-1 These

increases were marginally observed if the cells were

stimulated for 2 min or 30 min in the presence of

125 nm SDF-1 and were strongly significant after

10 min of incubation of the cells with 125 nm of the

chemokine (Fig 4A and data not shown) Among

these tyrosine phosphorylated proteins, those

immuno-reactive with anti-CXCR4 mAb 12G5 probably

repre-sent, respectively, CXCR4 monomers and homo- or

hetero-oligomers (Fig 4A, lane 4) Residual

phos-phorylation of CXCR4 in unstimulated cells was

detected (Fig 4A, lanes 1 and 3), as reported previously [21–23]

SDF-1 also induces the tyrosine phosphorylation

of SD-4 on HeLa cells and tyrosine phosphory-lated SD-4 is physically associated to tyrosine phosphorylated CXCR4

The anti-CXCR4 G19 IP of SDF-1-stimulated cell lysates revealed with anti-Ptyr mAb 4G10, just des-cribed, was also characterized by a 110–200 kDa broad smear, which was marginally revealed if the cells were not stimulated (Fig 4A, lane 2 vs 1) and was not detected if the anti-Ptyr 4G10 IP was revealed with anti-CXCR4 mAb 12G5 (Fig 4A, lane 4 vs 2) This suggests that it represents proteins which are physically associated to CXCR4 and are tyrosine phosphorylated when the cells are stimulated by SDF-1

To characterize these proteins, the SDF-1-unactivated-and SDF-1-activated HeLa cell lysates were immuno-precipitated in parallel with anti-Ptyr mAb 4G10 and blots were developed with several different anti-PG Abs: 4 mAb 5G9, 1 mAb DL-101,

anti-SD-2 Abs or anti-beta-glycan Abs (Fig 4B and data not shown) The tyrosine phosphorylated smear described above was only significantly observed when the anti-Ptyr 4G10 IP from SDF-1-activated HeLa cell lysates

Syndecan-4 SDF-1α Merged

A

B

Fig 3 SDF-1 colocalizes with SD-4 on HeLa cells (A) HeLa cells were double stained with fluorescently labeled biotinylated SDF-1a (green) and anti-(SD-4) mAb 5G9 (red) Confocal microscopy analysis shows the colocalization of biotinylated SDF-1a with SD-4, as assessed by the yellow (red-green) colocalization, suggesting the clustering of SDF-1 and SD-4 Data are representative of three individual experi-ments Bar ¼ 5 lm (B) HeLa cells were double-stained with biotinylated SDF-1a and with anti-(SD-4) mAb Stainings were revealed with streptavidin-15 nm colloidal gold particles or anti-mouse Ig bound to

6 nm colloidal gold particles, respectively Black arrows show colocalization of 6- and 15-nm colloidal gold particles Bar ¼ 100 nm (initial magnification · 27 500) Data are rep-resentative of three individual experiments.

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was revealed with anti-SD-4 mAb 5G9 (Fig 4B, lane 3

vs 6, 8 and data not shown); it was marginally observed

if the cells were not stimulated (Fig 4B lane 1) This

increase of the tyrosine-phosphorylation of SD-4

induced by SDF-1 on HeLa cells is time and

concentra-tion-dependent: it was marginal if the cells were

incuba-ted for 2 min or 30 min with 3, 50 or 125 nm of SDF-1,

and significant if the cells were incubated for 10 min

with 125 nm SDF-1 (Fig 4B, lanes 3 vs 2, 4 and data

not shown) These latter conditions were therefore used

for the following IPs To further demonstrate the

occur-rence of tyrosine-phosphorylated SD-4, the

SDF-1-unactivated- and SDF-1-activated HeLa cell lysates

were precipitated with anti-SD-4 mAb 5G9 and

devel-oped with anti-Ptyr mAb 4G10 (Fig 5A, lanes 1 and 2)

To confirm equal loading of the samples, the 5G9 IPs

were stripped and reprobed with anti-SD-4 mAb 5G9 (Fig 5A, lanes 5 and 6) The phosphorylated 110–

200 kDa smear was revealed with anti-Ptyr mAb 4G10

in the electroblotted IP of the SDF-1-stimulated cell lysates (Fig 5A, lane 2) This smear was marginally revealed in the unstimulated cells (Fig 5A, lane 1) These data strongly indicate that SDF-1 induces a rapid and significant increase in the tyrosine phosphorylation

of SD-4 on HeLa cells and that a physical association of tyrosine phosphorylated CXCR4 with tyrosine phos-phorylated SD-4 occurs

The protein core of tyrosine phosphorylated SD-4 was examined in parallel after digestion of the GAGs chains (Fig 5B) For this purpose, the anti-Ptyr 4G10 IPs and the anti-SD-4 5G9 IPs of the SDF-1-unstimu-lated and stimuSDF-1-unstimu-lated HeLa cells were treated with a

D C

Fig 4 SDF-1 induces the tyrosine-phosphorylation of SD-4 on HeLa cells Confluent serum-starved HeLa cells were either stimulated (+) or not (–) with SDF-1a Equal amounts of proteins from whole cell extracts were immunoprecipitated with the indicated antibodies and equival-ent amounts of IP samples were separated on 12% SDS ⁄ PAGE and immunoblotted using the indicated mAb or polyclonal antibodies (A) HeLa cells were stimulated (+) (lanes 2,4) or not (–) (lanes 1,3) for 10 min with 125 n M SDF-1a Cell lysates were immunoprecipitated either with anti-CXCR4 Igs G19 (lanes 1,2) or anti-Ptyr mAb 4G10 (lanes 3,4) Western blots were developed, respectively, with anti-Ptyr mAb 4G10 (lanes 1,2) or anti-CXCR4 mAb 12G5 (lanes 3,4) (B) HeLa cells were stimulated (+) (lanes 2,3,4,6,8) or not (–) (lanes 1,5,7) with

125 n M SDF-1a for the indicated time Cell lysates were immunoprecipitated with anti-Ptyr mAb 4G10 (lanes 1–8) Western blots were developed with anti-(SD-4) mAb 5G9 (lanes 1–4), anti-b-glycan Abs (lanes 5,6) or anti-(SD-2) Igs (lanes 7,8) (C,D) The intensities of the phos-phorylated bands shown in A and B (lanes 1–4) were quantified in absorbance units by densitometric scanning and analyzed with SCION

IMAG-ER They were expressed as ratios of the data observed for the SDF-1 stimulated cells relative to the untreated control cells Each bar represents the mean ± SE of triplicate determinations of an individual experiment The significance of the differences as compared with untreated control cells was assessed using Student’s t-test: **P < 0.05 The position of immunoglobulin chains is indicated by a star Pro-tein bands with changes in tyrosine phosphorylation state are indicated by arrows.

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A

C

Fig 5 Heparan sulfate is involved in the tyrosine phosphorylation of SD-4 induced by SDF-1 on HeLa cells (A) Upper panel: HeLa cells were either stimulated (+) (lanes 2 and 4) or not (–) (lanes 1 and 3) for 10 min with 125 n M SDF-1a In some experiments, cells were pretreated in parallel with heparitinases I and III mixture (lanes 3 and 4) Lysates were then immunoprecipitated with anti-(SD-4) mAb 5G9 Western blots were developed with anti-Ptyr mAb 4G10 (lanes 1–4) Lanes 5 and 6 confirm the equal loading of samples by reprobing the polyvinylidene difluoride membrane with anti-SD-4 5G9 mAb The position of the immunoglobulin chains is indicated by a star (B) HeLa cells were stimula-ted (+) (lanes 2, 4, 6 and 8) or not (–) (lanes 1, 3, 5 and 7) for 10 min with 125 n M SDF-1a Cells lysates were immunoprecipitated with anti-Ptyr 4G10 mAb (lanes 1–4) or with anti-SD-4 5G9 mAbs (lanes 5–8) The IPs were treated with heparitinases I, III, and chondroitinase ABC Western blots were developed, respectively, with anti-SD-4 5G9 mAb (lanes 1 and 2), anti-(SD-1) DL-101 mAb (lanes 3 and 4), anti-Ptyr 4G10 mAb (lanes 5 and 6) or the isotype IgG2b (lanes 7 and 8) (C) Upper panel: HeLa cells were stimulated (+) (lanes 2 and 3) or not (–) (lane 1) for 10 min with 125 n M SDF-1a In some experiments, cells were pretreated, in parallel, with heparitinases I and III (lane 3) Lysates were then immunoprecipitated with anti-(SD-4) mAb 5G9 Western blots were developed with anti-CXCR4 mAb 12G5 Lower panels in (A) and (C): The data shown in (A) (lanes 1–4) and in (C) were quantified in absorbance units by densitometric scanning and analyzed with SCION IMAGER They were expressed as the ratios of the data observed for the SDF-1 stimulated cells relative to those observed for the correspond-ing unstimulated, control cells Each bar represents the mean ± SE of triplicate determinations of an individual experiment The significance

of the differences as compared either with controls or with heparitinase-treated cells was assessed using a t-test **P < 0.05.

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mixture of heparitinases I and III, and chondroitinase

ABC, and then eluted from the beads The eluates

were electroblotted and revealed, respectively, with

anti-SD-4 mAb 5G9 and anti-Ptyr mAb 4G10

Pro-teins of 50–55 kDa which increased significantly after

stimulation of the cells by SDF-1 were revealed No

immunoreactivity was detected using either the isotype

or anti-SD-1 mAb DL-101, anti-SD-2 and

anti-(beta-glycan) Igs (Fig 5B and data not shown)

We then used coimmunoprecipitation experiments to

further analyse the physical association of CXCR4 and

SD-4 The anti-SD-4 5G9 IPs of unstimulated as well

as SDF-1-stimulated HeLa cells lysates, respectively,

were characterized by the presence of 48 kDa proteins

and of several other minor proteins of apparent

molecular masses > 48 kDa, all immunoreactive with

12G5 (Fig 5C, lanes 1 and 2) Therefore, the

SDF-1-independent heteromeric complex between CXCR4 and

SD-4 (Fig 5C, lane 1) is still present if the cells are

sti-mulated by the chemokine (Fig 5C, lane 2 vs 1)

The tyrosine phosphorylation of SD-4 induced

by SDF-1 on HeLa cells depends on the HS chains

of this PG

To examine whether the tyrosine phosphorylation of

SD-4 induced by SDF-1 on HeLa cells depends on

HS, we treated these cells with mixtures of heparitinase

I and III prior to their stimulation by SDF-1 To

pre-serve cell viability, concentrations of heparitinases were

lower than those used to treat the IPs The efficiency

of the enzymes was investigated: if the cells were

incu-bated in enzyme-free medium and then stimulated with

SDF-1, the 5G9 IPs revealed with 10E4 showed, as

expected, the 110–200 kDa broad smear, described

above; however, if the cells were pretreated with

hepari-tinases I and III, this smear was no longer present

(data not shown) Moreover, this heparitinases

pre-treatment of the cells prevented in a significant manner

the tyrosine-phosphorylation of SD-4 induced by

SDF-1, as assessed by the anti-SD-4 5G9 IPs revealed

with anti-Ptyr 4G10 mAb (Fig 5A, lane 4 vs 3) In

these experiments, the apparent relative molecular

masses of most tyrosine-phosphorylated SD-4

mole-cules were also decreased, as expected [17] (Fig 5A,

lanes 3 and 4 vs 2)

The homo- or hetero-oligomerization of CXCR4

induced by SDF-1 on HeLa cells is prevented by

heparitinases I and III pretreatment of these cells

Heparitinases I and III pretreatment of the HeLa cells

also significantly prevented the homo- or hetero-

oligo-merization of CXCR4 induced by SDF-1 on HeLa cells,

as assessed by the anti-SD-4 5G9 IP of the cell lysates revealed with anti-CXCR4 mAb 12G5 (Fig 5C, lane 3

vs 2) This indicates that the HS-dependent binding of SDF-1 to SD-4 enables the chemokine to induce the homo- or hetero-oligomerization of its GPCR

The physical association of tyrosine-phosphoryl-ated SD-4 with tyrosine phosphoryltyrosine-phosphoryl-ated CXCR4 does not depend on GAGs chains

When anti-CXCR4 G19 IPs of the SDF-1 stimulated cell lysates were treated with heparitinases I and III, and chondroitinase ABC mixture, both SD-4 and CXCR4 remained on the beads, as assessed by their respective revelation with 12G5 and 5G9 (data not shown) This suggests that GAG-dependent interac-tions are not involved in these physical associainterac-tions Finally, in all the experiments described above, results of immunoprecipitation of cell lysates with iso-type-matched control antibodies (data not shown) rule out nonspecific protein association with membrane components under our experimental conditions

The activation of p44/p42 MAPK and JNK/SAP kinase by SDF-1 on HeLa cells is HS- and SD-4- dependent

To analyze some of the transduction pathways induced

by SDF-1 on HeLa cells, whole cell extracts from either unstimulated or stimulated HeLa cells were elec-troblotted and revealed using phospho-specific anti-p44⁄ p42 mitogen-activated protein kinase (MAPK) or anti-p46⁄ p54-Jun N-terminal ⁄ stress-activated protein kinase (JNK⁄ SAP kinase) Abs, respectively Parallel immunoblottings with anti-total polyclonal Abs confirmed equal loading of the samples (Fig 6) As expected [24–26], SDF-1a and phorbol 12-myristate-13-acetate (PMA) induced a rapid activation of p44⁄ 42 MAPK and JNK⁄ SAP kinase signaling in HeLa cells

by increasing phosphorylations of the respective pro-teins (Fig 6) This effect was time and concentration-dependent: It rose from 3 nm up to 125 nm SDF-1a and if the time of incubation with the chemokine was enhanced from 5 to 15 min On the contrary, these phosphorylations decreased if the time of incubation with the chemokine was enhanced up to 30 min (Fig 6A) According to these results, the cells were incubated for 15 min in the presence of 125 nm of SDF-1 in the following experiments (Fig 6B) In these conditions, pretreating these cells with heparitinases I and III significantly decreased these SDF-1-induced phosphorylations (Fig 6B) (P < 0.05)

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As expected [21,26,27], SDF-1 also stimulates

intra-cellular calcium mobilization in HeLa cells (Fig 7A)

However, enzymatic removal of HS from the surface

of these cells did not affect this increased fluorescence

intensity observed in dye-loaded cells (mean ±

SE¼ 101 ± 21, n ¼ 30) as compared to untreated

control cells (mean ± SE¼ 97 ± 16, n ¼ 32), or the

percentage of SDF-1 responding cells (Fig 7A,B and

data not shown)

Transfection of HeLa cells with SD-4 double-stran-ded RNA (SD-4 dsRNA) resulted, as expected, in a SD-4 mRNA downregulation reaching 80% reduc-tion on day 3, while the mRNAs of SD-1, SD-2 and CXCR4 were not changed (Fig 8A) Moreover, when measuring the expressions of these proteins by FACS in these transfected cells, we found a 65% downregulation

of SD-4 expression, while SD-1, SD-2, beta-glycan or CXCR4 expressions remained unchanged as expected

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A

B

Fig 6 Heparan sulfate is involved in the activation of MAPK induced by SDF-1 stimulation of HeLa cells (A) Serum-starved HeLa cells were either stimulated or not with 3 n M or 125 n M SDF-1a for 5, 15 and 30 min, and then analyzed for p44⁄ p42 MAPK and JUN ⁄ SAPK activations (B) Upper panel: Untreated (–) or heparitinases I- and III-treated (+) HeLa cells were either stimulated or not for 10 min with PMA (0.5 l M ) or SDF-1a (125 n M ).Whole cell extracts were separated on 12% SDS ⁄ PAGE and immunoblotted using either phosphospecific anti-(p44 ⁄ p42 MAPK) or phosphospecific p46 ⁄ p54-SAPK ⁄ JNK rabbit polyclonal antibodies Parallel immunoblottings with (total p44 ⁄ p42 MAPK) or anti-(total p46 ⁄ p54-SAPK ⁄ JNK) polyclonal antibodies, respectively, confirmed equal loading of samples Lower panel in (B): The results were quantified by densitometric scanning and analyzed with SCION IMAGER For each lane, data were expressed as p44 ⁄ p42 or SAPK ⁄ JNK phos-phorylated proteins over total proteins in absorbance units The amount of MAPK (p44 ⁄ p42 or SAPK ⁄ JNK) phosphorylation in the SDF-1-sti-mulated cells was calculated according to the level of phosphorylated MAPK proteins in unstiSDF-1-sti-mulated control cells, which was considered as 100% Each bar represents the mean ± SE of triplicate determination of an individual experiment The significance of the differences between the SDF-1-stimulated cells and the corresponding heparitinases treated cells was assessed using a t-test **P < 0.05.

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(Fig 8B–D and data not shown) To monitor

the sequence specificity for SD-4 RNA interference,

4 dsRNAs was used as a control The

mutSD-4 dsRNA construct caused no significant reduction of

SD-4 mRNA and protein expressions, concordant with

previous reports on RNA interference methodology

[28,29] (Fig 8A and data not shown) (P¼ 0.11) We

then observed that both p44⁄ p42 MAPK and

JNK⁄ SAP kinase activations were significantly reduced

after the knockdown of SD-4 upon SDF-1a

stimula-tion, as compared with the data observed in

mock-transfected cells and in cells mock-transfected with mutSD-4

dsRNA, respectively (Fig 8E) (P < 0.05) By contrast,

under the same conditions, no change in the Ca2+

mobilization induced by SDF-1 after the knockdown

of SD-4 on HeLa cells was observed (Fig 7C,D)

Discussion

CXCR4 and SDF-1 play pivotal roles in many diseases

[5–8,30–32] SDF-1 binding to GAGs, especially HS,

has been demonstrated [17,33,34] Moreover, SDF-1

forms complexes on CXCR4-positive cells with

CXCR4 as expected and also with SD-4, but not with

SD-1, SD-2, beta-glycan or CD44 [17] Furthermore,

an SDF-1-independent heteromeric complex between

CXCR4 and SD-4 occurs on these cells, but not with

SD-1, SD-2, beta-glycan or CD44 [17] Therefore,

SDF-1 may bind both its GPCR CXCR4 and SD-4 However, whether SDF-1 directly binds SD-4 has not been demonstrated previously We show here a direct binding of SDF-1 to electroblotted SD-4 enriched from HeLa cell lysates The fact that no binding of the chemokine to SD-1, SD-2, beta-glycan or CD44 was detected strongly argues for the selectivity of this bind-ing We then examined whether SDF-1 is associated with SD-4 at the plasma membranes of intact HeLa cells By using both confocal and electron microscopy analysis, we show strong evidence for the occurrence

of a colocalization between SDF-1 and SD-4 at the HeLa cell plasma membrane The fact that in the same conditions, no colocalization of SDF-1 with another

PG, SD-1, was observed, argues further for the selec-tivity of this association Therefore, our findings observed at the molecular level were strengthened by experiments performed at the cellular level

Thereafter, we asked whether GAGs are involved in SDF-1 binding to SD-4 By pretreating the electroblot-ted PGs from the HeLa cells with heparitinase I and III and chondroitinase ABC mixture, we demonstrate the strong GAG dependency of this binding However, our data do not rule out the additional involvement of protein–protein interactions between SDF-1 and the SD-4 core protein Indeed, while the SD core proteins share a high degree of conservation in their short cyto-plasmic and transmembrane domains, in contrast their

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heparitinases I and III treated HeLa cell untreated HeLa cell

SD-4 dsRNA HeLa cell mock-transfected

HeLa cell

Fig 7 Heparan sulfate is not involved in

int-racellular Ca 2+ mobilization induced by

SDF-1 on HeLa cells Untreated HeLa cells (A),

heparitinases I- and III-treated HeLa cells

(B), mock-transfected HeLa cells (C), or

SD-4 dsRNA transfected HeLa cells (D) were

loaded for 30 min with Fluo-3 and then

stimulated with SDF-1a (125 n M ), as

indica-ted by black arrows The plots show the

variations of the fluorescence intensity

(expressed in arbitrary units), measured

overtime within the analyzed cells Data

are representative of three individual

experiments.

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extracellular domains are divergent with the exception

of consensus sites for GAG attachment [15,35]

The participation of the SD-4 ectoplasmic domain in

SDF-1 binding raises the question whether this binding

is accompanied by intracellular modifications of SD-4

such as tyrosine phosphorylation, which plays critical

role in a variety of cellular processes We have therefore

asked whether SD-4 functions as an SDF-1 signaling

molecule For this purpose, we investigated whether

SDF-1 stimulation of HeLa cells induces an increase in

the tyrosine phosphorylation of SD-4, besides that of

CXCR4 which has already been reported [21–23] The

SD cytoplasmic domains contain four conserved

tyro-sine residues, two of which are in favorable sequences

for phosphorylation [36] Endogenous tyrosine phos-phorylation of SDs has already been detected while most cell surface SDs are phosphorylated following treatment with the tyrosine phosphatase inhibitor per-vanadate [37] Tyrosine phosphorylation of the SD cytoplasmic domain may be a common mechanism for regulating SD activity In this study, immunoprecipita-tion experiments using Ptyr, CXCR4 and anti-(SD-4) mAbs show for the first time that besides the tyrosine phosphorylation of CXCR4, tyrosine phos-phorylation of SD-4 occurs in response to SDF-1 sti-mulation of HeLa cells This tyrosine phosphorylation depends on the time of incubation of the cells with the chemokine: marginal for 2-min incubation, significant

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IgGl IgGl

(SD-4ds RNA)

(mocktransfected)

Fig 8 SD-4 is involved in SDF-1 activation of MAPK pathways HeLa cells were transfected with either SD-4 dsRNAs or MutSD-4 dsRNA or were mock-transfected (A) Left panel: HeLa cells were analyzed for SD-4, SD-1, SD-2, CXCR4 specific mRNA, by semiquantitative RT-PCR,

3 days post transfection To normalize for input of total RNA, GAPDH mRNA was also determined Right panel: SD-4 mRNA levels were quantified by densitometric scanning and analyzed with SCION IMAGER Results are depicted relative to mock-transfected control Each bar rep-resents the mean ± SE of triplicate determination of an individual experiment The significance of the differences as compared to mock-transfected control cells was assessed using a t-test **P < 0.05 (B, C, D) HeLa cells were analyzed for (B) SD-4 (C) SD-1 and (D) CXCR4 protein expressions by FACS analysis, 3 days post transfection Reactivity was compared to an isotype-matched control mAb (E) Upper panel: HeLa cells were treated for 15 min with 125 n M SDF-1a, 3 days post-transfection Whole cell extracts were separated on 12% SDS ⁄ PAGE and analyzed by immunoblot using phosphospecific anti-(p44 ⁄ p42 MAPK) or phosphospecific p46 ⁄ p54-SAPK ⁄ JNK polyclonal rab-bit antibodies, respectively Parallel immunoblotting with anti-(total p44 ⁄ p42 MAPK) or anti-(total p46 ⁄ p54-SAPK ⁄ JNK) polyclonal antibodies was performed to confirm equal loading of samples Lower panel: The results were quantified by densitometric scanning and analyzed with

SCION IMAGER For each lane, data were expressed as p44 ⁄ p42 MAPK or SAPK ⁄ JNK phosphorylated proteins over total proteins in absorbance units The amount of MAPK (p44 ⁄ p42 or SAPK ⁄ JNK) phosphorylations in the SDF-1-stimulated cells was calculated according to the level of phosphorylated MAPK proteins in untreated control cells, which was considered as 100% Each bar represents the mean ± SE of triplicate determination of an individual experiment The significance of the differences between the phosphorylation states of the SDF-1a-stimulated, SD-4dsRNA- transfected cells and those of the SDF-1a-stimulated, mock-transfected cells was assessed using a t-test **P < 0.05.

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